Critical Reviews in Analytical Chemistry

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New Trend in the Extraction of Pesticides from

the Environmental and Food Samples Applying
Microextraction Based Green Chemistry Scenario:
A Review

Muhammad Saqaf Jagirani, Ozgur Ozalp & Mustafa Soylak

To cite this article: Muhammad Saqaf Jagirani, Ozgur Ozalp & Mustafa Soylak (2021): New Trend
in the Extraction of Pesticides from the Environmental and Food Samples Applying Microextraction
Based Green Chemistry Scenario: A Review, Critical Reviews in Analytical Chemistry, DOI:
10.1080/10408347.2021.1874867

To link to this article: https://doi.org/10.1080/10408347.2021.1874867

Published online: 09 Feb 2021.

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CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY
https://doi.org/10.1080/10408347.2021.1874867

New Trend in the Extraction of Pesticides from the Environmental and Food
Samples Applying Microextraction Based Green Chemistry Scenario: A Review
Muhammad Saqaf Jagirania,b, Ozgur Ozalpa,c, and Mustafa Soylaka,c
a
Faculty of Sciences, Department of Chemistry, Erciyes University, Kayseri, Turkey; bNational Center of Excellence in Analytical Chemistry,
University of Sindh, Sindh, Pakistan; cTechnology Research and Application Center (TAUM), Erciyes University, Kayseri, Turkey

ABSTRACT KEYWORDS
This review focused on the green microextraction methods used for the extraction of pesticides Green chemistry;
from the environmental and food samples. Microextraction techniques have been explored and microextraction; solid phase
applied in various fields of analytical chemistry since its beginning, as evinced by the numerous microextraction; liquid
phase
reviews published. The success of any technique in science and technology is measured by the microextraction; pesticides
simplicity, environmentally friendly, and its applications; and the microextraction technique is
highly successive. Deliberations were attentive to studies where efforts have been made to valid-
ate the methods through the inter-laboratory comparison study to assess the analytical perform-
ance of microextraction techniques against conventional methods. Succinctly, developed
microextraction methods are shown to impart significant benefits over conventional techniques.
Provided that the analytical community continues to put forward attention and resources into the
growth and validation of the microextraction technique, a promising future for microextraction
is forecasted.

Introduction of active ingredients (22%) and dollars (33%) and.[19]The

The term pesticide is used to composites, that covers a
diverse group of chemical compounds that are employed to
kill, counteract, or control different insect pests such as mol-
luscicides (mollusks), insecticides (insects), herbicides
(weeds), fungicides (fungi), nematocides (nematodes),
rodenticides (rodents), and plant growth promoters.[1–6]
Environmental Protection Agency (EPA) has defined the
pesticides as any constituent or combination of different
substances proposed for the preventing, repelling, destroy-
ing, or mitigating the pests, or plant desiccant, regulators,
defoliant, or nitrogenous stabilizer. Pesticide contains two
main constituents: active and inert. The active constituent
performs the key role of pests, while the inert part such as
herbs, edible oils, species, cellulose are added with the active
part to make pesticide and play a key role in efficiency and
performance of pesticide.[7–14] Different types of pesticides
such as synthetic pyrethroids, organochlorine pesticides
(OCPs), and organophosphorus pesticides (OPPs).[15,16] Due
to a wide range of applications of pesticides, it increases the
consumption from time to time, according to the Ministry
of Agriculture and Rural Development in 2009 the sale of
pesticides reached up to 49,760.8 tons in Poland.[17,18] It is
assessed by the countries of the European Union (EU) con-
sume up to more than 0.3 million, tons per annum of pesti-
cides only for agriculture purposes. The world marketplace
for pesticides is expected up to 33.59 billion dollars, from
which America signifies the major part, in terms of pounds
consuming rate of pesticides in diverse countries depends
on the agricultural area and nature of yield. The World top
ten pesticide consuming (ton/year) countries are Italy
(69,796), Turkey (67,025), Colombia (53,603), India
(44,519), Japan (40,305), Bolivia (34,803), Ecuador (34,402),
Germany (30,413), Romania (29,224), and Chile (19,880).[20]
At present more than 800 pesticide active materials are
existing in a broad range of viable goods these constituents
belong to up to 100 ingredients class. Carbamates,
Benzoylureas, organophosphorus compounds, sulfonylureas,
pyrethroids, or triazines are very important groups. They are
used for different purposes such as rat and other rodent poi-
sons, insect repellents for personal use flea and tick sprays,
pet collars; powders, laundry, kitchen, and sanitizers and
bath disinfectants Products that kill mildew and mold; some
garden and lawn products, such as weed killers; some swim-
ming-pool chemicals.[21,22]But due to the large quantity of
pesticide usage the residue of agricultural commodities, pol-
lute the environment also the foodstuffs the larger part of
the human population’s effects due to the hazardous effects
of pesticides. Besides their many advantages, pesticides are
considered the most hazardous environmental pollutants
due to their capability to accrue as well as their flexibility,
and very long term dangerous effect on the human beings
and other living creatures it case a lot of despises such as
(Breast cancer,[23,24] Liver cancer,[25,26] Epithelial ovarian
cancer,[27] Uterine cervix cancer,[28] Bladder Cancer,[29]
Invasive ductal cancer,[30–32] Cardiovascular disease,[33]

CONTACT Mustafa Soylak soylak@erciyes.edu.tr Faculty of Sciences, Department of Chemistry, Erciyes University, Kayseri, 38039 Turkey
ß 2021 Taylor & Francis Group, LLC
2 M. S. JAGIRANI ET AL.
Alzheimer’s disease,[34] Autism spectrum disorders,[35] meta-
bolic syndrome (central obesity, hypertension, dysglycemia,
and dyslipidemia.),[36–39] bone structure disorders,[16]
anemia[12,14] embryologic diseases,[40] Endocrine disrup-
tion,[41] congenital disabilities.[31] The existence of pesticides
in the ecosystem is predominantly dangerous and their out-
come and utility are still indefinite.[42] They also play a part
in different biological, physical, and chemical processes, as a
consequence of which even more noxious substances may
form; by accruing in the living things, these can lead to irre-
versible, harmful changes. The unsafe use of pesticides has
adverse effects on humans and the environment, increasing
exposure to poisoning and diseases. Pesticides are an inclu-
sive risk because they move with the wind, sea, and also in
rain tides from one region to another place where they have
not ever been used before. To protect the people’s health
different regulations and guidelines have been employed to
provide safe and healthy food by reducing the maximum
residue limits (MRLs) in different commodities.[10,43–46]
Such monitoring limits are mostly accomplished through the
risk assessment procedure that needs thorough monitoring
of pesticides in the environment and foodstuffs. The hazard-
ous classification has revealed that several pesticides can
cause serious health issues at very low concentrations. Such
studies have focused on fixing the very low concentration
limit of MRLs. The US Environmental Protection Agency
has recognized the MRL of acetochlor in the groundwater at
0.1 mg/L.[47]Therefore, different countries have recognized
plans and legal protocols to monitor and control the con-
centration of pesticides in the environmental and food sam-
ples. Such approaches are aimed to confirm that pesticide
remains in environmental and food samples accomplish
with the maximum permissible limit recognized by the
national and international government organizations. The
chromatographic techniques are such nice techniques for the
monitoring of pesticide contaminations such as gas chroma-
tography (GC),[3,31,48,49] high-performance liquid chroma-
tography,[50–52] micellar electrokinetic
chromatography,[32,53–55] and supercritical liquid chromatog-
raphy.[56–59] However. The level of pesticide pollutants too
low to directly quantify using such chromatographic techni-
ques. Due to the public and scientific concern about envir-
onmental contamination, greener and environmentally
friendly procedures have been introduced in numerous areas
of research and society. From an analytical fact, food and
environmental samples are highly complex and diverse: the
factors affecting the site of sample and the nature of the
sample, types of different matrix and the presence of coex-
isting materials, and very low concentration of targeted ana-
lytes. The sampling quality and sample pretreatment
essentially determine the accomplishment of the study from
the complex matrix. Ideally, the preparation of the sample
should be as easy as promising, because it not only time-
saving time but also reduces the chance of introducing con-
tamination. Therefore, different analytical methods must be
able to monitor the residue from different foodstuffs at a
very low level with an acceptable level of accuracy and pre-
cision. Despite the improvement in analytical techniques, a
very low level of limit of detection (LOD) is still a major
task for the innovative sample preparation approaches,[60]
mostly these procedures containing enrichment of analytes,
may be significantly contributing to a decrease in LOD with
acceptable technique performance and characteristics.
Various sample preparation approaches have been reported
for the separation and pre-concentration of analytes includ-
ing liquid-liquid extraction (LLE) and, solid-phase extraction
SPE.[61–72] One of the eldest and most common removal
approaches, in tedious sample preparation, is a liquid-liquid
extraction (LLE). Different organic solvents have been used
in the LLE such as dichloromethane and mixtures of petrol-
eum ether[73] dichloromethane or hexane.[74–77] LLE is
known as a smart approach for the screening test of new
pesticides[78,79] Because of its easiness, efficacy, nominal
operator training. Due to its easiness, it is widely recognition
in various standard methods. Though, this method has some
limitations: it needs a large amount of toxic organic solvents
and multistage procedure, there is a risk of suspension
forming during the contact, and the problem of dumping of
post-extraction solvent. To obtain the expected pre-concen-
tration coefficient, the excess solvent generally has to be
evaporated. And also extract and clean-up are often neces-
sary. To overcome these limitations several developments
have been reported for this method, most of them have
involved and miniaturizing the method to decrease the
amount of solvent consumed. The SPE associating the use
of a number of different adsorbents (e.g., PSA, amine, C18)
has been used.[80,81] Other elimination methods such as
matrix solid-phase dispersion[82,83] accelerated solvent
extraction,[17] and QuEChERS with dispersive solid-phase
extraction (d-SPE) technique using a different type of
adsorbents such as C18, PSA, silica gel, florisil graphitized
carbon black, and amine-functionalized graphene.[84–86] The
adverse impact of analytical methods has been reduced from
the environment mostly in three different ways: decrease the
number of solvents required for the sample pre-concentra-
tion; decrease the number of toxic reagents and solvents
that used during the analysis step, particularly by miniatur-
ization and automatization; growth of alternative direct ana-
lytical approaches that not need reagents or solvents.[87] The
analytical procedures contain different key steps such as col-
lections of samples, preparation, separation and pre-concen-
tration and data assessment make different influence to the
environment effluence and there are some potential techni-
ques to make them economical beneficial and greener and
to closer to the green chemistry principles.
Green chemistry scenario
Green characteristics in analytical approaches currently, the
development is to improve the analytical methodologies
assisting a wide range of analytes to be recognized in an
only one analytical run (multi-residue methods (MRM)); but
the difficulty is that the compounds to be detected simultan-
eously, often existing at a very low level, have different phys-
ical and chemical properties depends on their chemical
characteristics.[88] New methodologies have been established

Figure 1. Schematic representation of microextraction techniques.[117]
which remove many problems and also surge the precision,
reproducibility, throughput, and economically beneficial. In
numerous cases, the capacity for a smaller initial size of the
sample, even at the trace level analysis is also crucial.[89] The
new trend in a sample preparation procedure that minimizes
the quantity of solvents and reagents that contribute to
improving environmental quality. However, the use of
reagents and organic solvents is unavoidable and their alter-
native is not a good substitute is a reducing of their ingest-
ing. At this stage, automation of analytical methods by
means of flow-injection (FI) approaches plays major charac-
ter in the Green Chemistry framework.[90,91] Green
Analytical chemistry is the use of chemical protocols, meth-
odologies, and techniques that eliminate or decrease the use
or manufacturing of products, feedstocks, by-products,
reagents, organic solvents, etc., that are very dangerous to
the environment as well as for human health.[92]
Miniaturization is the best way to minimize the side effects
of unwanted solvents. In this respect, the combination of
up-to-date analytical procedures with breakthroughs in
miniaturization and microelectronics allows the advance-
ment of an efficient analytical tool for control the pollution
and processes. Combination and monetarization in analyt-
ical procedures with developments in chemometrics are
essential. Of-course, improvement and development of new
modules for the instrumentation are critical in green analyt-
ical chemistry. For example, we have elucidated the potential
and the adaptability of new analytical ordering and their
potential for decreasing the use of harmful materials and the
extents of waste produced during analysis.[93,94] To highlight
green chemistry problems the research pays more attention
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 3
to develop a new method with good qualities such as the
easy, fast selective, and sensitive minimum quantity of solv-
ent that has been used or solvent-free method. The microex-
traction technique is the best candidate, that to fulfill the
criteria of green analytical chemistry.
Microextraction technique
The microextraction methods have been established by dif-
ferent researchers, to substantiate the recent improvements
in the advancement of highly efficient and modern analytical
techniques such as liquid chromatography,[3,48,49] gas chro-
matography[53] coupled to different detectors (diode array
detector, mass spectrometry, ultraviolet detector, etc), capil-
lary electrophoresis which is hyphenated with the microex-
traction technique,[66]These hyphenated microextraction
based methods gave been applied for the qualitative and
quantitative study of pesticide residues from foods. Before
the sample preparation, it is essential to extract, isolate, and
pretreatment the target analyte from the complex matrices
such as vegetables, fruits, and other environmental samples.
The hyphenation of modern techniques with microextrac-
tion techniques reduces the cost, time, technical errors. The
developed sensitivity and selectivity make it a promising
technique to electron the quantity of sample required in the
analysis. All these methods are hyphenated with modern
analytical techniques, on-line or off-line either sometimes
on-line.[95] The off-line process is a good substitute when
the quantity of samples is small because there is normally
no need for an automatic procedure and time-consuming.
Conventional techniques will need extra protocols setting up
4 M. S. JAGIRANI ET AL.
Figure 2. Different types of SPME.[144,145]
an automatic method, on-line, or either at-line becomes
meaningful when a large number of analyzed samples. The
automation usually advances in the data quality, increases
the analyte throughput, cost-effective, and develop the prod-
uctivity of instruments and operators. When the targeted
analytes are unstable and the limited volume of sample is
present and high sensitivity is needed in this regard the on-
line systems are convenient. The selection elimination
method is through on the different basic factors. Obviously,
the preparation of sample must be tailored to the final ana-
lysis. The media of sample and the nature and quantity of
analytes in the sample are important. Also essential are
extraction speed, complexity, flexibility, and simplicity of the
process development, and sharpness of the technique.
Different microextraction approaches have been developed
for the extraction of toxic pollutants such as pesticides, met-
als, pharmaceuticals, etc. from the food and environmental
samples. Microextraction techniques contain different types
such as liquid-phase microextraction (LPME)[96] solid-phase
microextraction (SPME),[97–103] liquid-liquid microextraction
(LLM), single-drop microextraction (SDME),[104–107] disper-
sive liquid-liquid microextraction (DLLME),[108–111] hollow
fiber liquid-phase microextraction (DF-LPME),[55,112,113]
stir-bar sorptive extraction (SBSE), and on-line solid-phase
extraction (SPE), have numerous benefits over the trad-
itional methods of conventional SPE[114–116] and liquid-
liquid extraction (LLE). The key advantages are negligible
use of harmful organic solvents, and characteristically, the
high enrichment factor Figure 1 shows the schematic repre-
sentation of microextraction used for the extraction of pesti-
cides from food and environmental samples using
different materials.
Solid-phase microextraction
SPME was presented by Belardi and Pawliszyn in 1989.[97]
According to the Green Analytical Chemistry (GAC) strat-
egies, the SPME is considered as a green analytical proced-
ure for the extraction of analytes from the complex metrics
without the use of toxic organic solvents. The analytes could
be efficiently eliminated by the SPME from any kind of
matrices such as liquid and gas samples by the adsorption
and desorption on to the fibrous materials such as polymeric
thin layer sheets, nanomaterials attached to the solid surface
of fiber that fixed inside the injection needle or capil-
lary.[118–120] Imprinted polymeric materials also used as
adsorbent material[121–132] The analytes partition between
SPME fiber coating and sample matrices. It gains more
attention from the analytical scientists in different scientific
disciplines.[118,133–135] It is a very easy time saving, sensitive
technique.[120,136–139] The SPME contains two modes of
extraction such as headspace mode (HS-SPME) and one is
the direct immersion mode (DI-SPME) to extract the analy-
tes from different types of a matrix such as gas and liquid.
Usually, the HS-SPME mode has been used for the study of
unstable substances. The DI-SPME was used for the analysis
of lower volatile compounds.[140–143] Presently a new
approach combination of extraction mode and temperature
in the single-elimination method. Figure 2 shows the differ-
ent types of SPME.
Types of SPME
The DI-HS SPME was developed by Karasek et al.[146] for
the real-time analysis of compounds with different volatil-
ities (PAH and BTEX). This developed method was with
associated conventional SPME technique based on the single
extraction temperature and mode and showed to be smart
characteristic, simultaneously it removes a higher quantity of
both low volatile and volatile compounds as compared to
conventional methods. In the DI-SPME technique, the fabric
material is in direct interaction with the sample which
adsorbs the analyte directly. The fabric materials have good
efficiency to separate the targeted analyte from the sample
metrics in the presence of coexistence materials. DI-HS-
SPME mode has been widely used in used for the analysis
of volatile compounds as well as semi-volatile compounds
such as organochlorine pesticides (e.g., acephate, dimethoate,
omethoate, and pyrethroids from the food
samples.[142,143,147–149]
Headspace solid-phase microextraction
HS-SPME is an excellent technique used to eliminate and
pretreatment semi-volatile or volatile analytes and can

Figure 3. Graphical illustration of SPME process and its applications.[155]
minimize some limitation of the conventional pre-concen-
tration method.[150] This method is recognized on the distri-
bution equilibrium of analytes between the sample media,
water, headspace, and the fabric coating with an adsorbent
polar or nonpolar polymer.[149,151] As compared with other
conventional solvent extraction methods the HS-SPME does
not allow to absorb nonvolatile compounds onto the fabric
material to avoid them to introduce into the instrument it
can help to save the inlet column reduce the instrumental
maintenance charges. Moreover, this technique is easy to
operate and minimizes the sample handling process; HS-
SPME can achieve high sample output and reduce subjective
errors. Afterward, HS-SPME coupled with GC combining
with different types of detectors has been widely used in the
present decade to eliminate the different types of pesticides
carbamate pesticides SPME/GC/FID[101] organochlorine pes-
ticides SPME/GC/ECD[152] pyrethroid pesticides SPME/GC-
TOF/MS,[147] 13 pesticides SPME/GC/MSD[153] and pyreth-
roid pesticides SPME/GC/lECD.[154] Figure 3 represents the
schematic diagram of SPME process and its applications.
Applications of SMPE for the elimination
of pesticides
Different researchers reported SMPE based approaches for
the extraction of pesticides such as wine[156–158]
water.[156,159–164] Caiet al., prepared a polyphenylmethylsi-
loxane (PPMS) based new coating material for the SPME
association with the micro-wave-assisted extraction (MAE)
applied for the determination of OCPs from the Chinese
tea. The developed method was hyphenated with the GC-
ECD and obtained good LOD 0.081 ng/l.[165] Yao et al. used
commercially available five different kinds (PDMS, 85 m PA,
and 65 m
7, 30 and 100 m) of fibers used for the solid-phase
microextraction based detection of organophosphorus pesti-
cides (OPPs) from the water samples. The different param-
eter has been optimized such as time, pH, temperature, and
volume of sodium chloride to achieve the maximum adsorp-
tion capacity. The LODs have been found 0.049 g/l for the
parathion and 0.301 g/l for carbophenothion. These materi-
als contain have good repeatability and this proposed
method was used for the analysis of real water samples with
good percentage recovery was found up to 75.3 to
102.6%.[166] Dimitra et al., used Polydimethylsiloxane-coated
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 5
fiber (100 mm) for the SPME of pesticides such as trifluralin,
S-ethyl-N,N-di-n-propylthiolcarbamate (EPTC), deethylatra-
zine, atrazine, alachlor, and terbuthylazine and insecticides,
such as diazinon, carbofuran, parathion methyl, disulfoton,
parathion ethyl, fenthion, and ethionfrom the surface water.
After the pre-concentration, the samples have been analyzed
by the GC-MS and GC-FID.[167] Xin-Yue et al.proposed
SPME basednew method for the selective and sensitive
extraction of five carbamate pesticides in the apples by using
the carbon nanotubes-reinforced hollows (CNTs-HF-SPME)
as a fabric material hyphenated with HPLC-DAD. After the
optimized different parameters, the achieved enrichment fac-
tors were in the range of 49–308 with good reproducibility.
The LOD was obtained from the proposed method in the
range of 0.09–6.00 ng/g. According to the results, the pro-
posed method was efficient enrichment pre-concentration
procedures for the determination of carbamate pesticides in
apples.[168] Doong & Liao proposed HS-SPME for the elim-
ination of OCPs from the soil samples. Different parameters
have been optimized such as type of fiber
(Polydimethylsiloxane [PDMS] 100 mm size anddivinylben-
zene (PDMS–) 65-mm), adsorption time, temperature effect,
matrix effects to achieve maximum extraction capacity.
Developed method obtained good extraction capability with
linearity range of OCPs 0.2–4 ng/g and also the limit of
detection and limit was achieved up to 0.06–0.65 ng/g.[169]
Dong et al., prepared a new sol–gel calix[4]arene/hydroxy-
terminated silicone oil coating fibers was used HS-SPME
coupled with GC-ECD to determination of 12 organochlor-
ine pesticides (OCPs) from the radish sample. The LOD was
found up to174 ng/kg for the proposed method.[170] Luiz
et al., have been used 50/30 DVB/CAR/PDMS fiber coatings
for the DI-SMPE combine with GC-ECD (DI-SPME-GC-
ECD) for the determination of 18 organochlorine pesticides
from the groundwater. Under the optimal condition the
SPME-GC/ECD technique shows good linearity and repro-
ducibility and found LOD was from 4.5  10
3 to 1.5 ng/L
with good percentage recovery[171] Fernandez et al., was
proposed a SPME based method for the extraction of 18
organophosphorus pesticide from the honeybee samples
used poly(dimethylsiloxane) and polyacrylateas a fibers
under the optimized conditions the LOD was found up to
below than 10 mg/kg. The proposed method was successfully
applied for the analysis of environmental samples.[172] Yu
et al. has been used bisbenzo crown ether/
6 M. S. JAGIRANI ET AL.
hydroxylterminated silicone oil (OH-TSO) based fabric
material for the SPME of organophosphorus pesticides
(OPs) from the food samples juice, honey, pakchoi, and
orange). The OH-TSO-SPME-GC-FPD shows good extrac-
tion efficiency and higher sensitivity toward the organphos-
phorous pesticides (OPs). The obtained LOD value was
0.003–1.0 ng/g. proposed method was successful applied for
the analysis of real samples for the determination of selected
pesticides.[173] Li et al., developed SPME- GC–ECD method
for the extraction of the group of organochlorine pesticides
(OCPs) including aldrin, OCPs, p,p9-DDE, o,p9-DDE, o,p9-
DDT,dieldrin,p,p9-DDT, b-endosulfan, a-endosulfan, endrin,
d-HCH, endosulfan sulfate, g-HCH, heptachlor, methoxy-
chlor, heptachlor epoxide, trifluralin, and methoxychlor used
16 different types of SPME fibers. The developed method
have good LOD value from 0.002 to 0.070 mg/l.[174] Dias
et al., proposed new SPME method for the determination of
seven different organochlorine pesticides using gold nano-
particles as a coating material. The limit of detection was
obtained up to 0.13 mg/L.[146] Kin &Huat, were reported Hs-
SPME-GC-ECD based method for the determination of
organophosphorus such as malathion, diazinon, quinalphos,
profenofos, andchlorpyrifos and organochlorine including a-
endosulfan, b-endosulfan and chlorothalonil pesticides from
the vegetables and fruits.[86] Wang et al., proposed SPME
based method for the determination of OCPs from the vege-
table samples using hyper-crosslinked polymer benzenedi-
methanol (HCP-BDM) as a fiber. The HCP-BDM-SME-GC-
ECD method was successfully applied from the real sample
analysis with acceptable LOD value of 50 ng/g.[175] Ebrahimi
et al., developed hallow fiber (HF) SPME for the extraction
of pesticides such as fenitrothion, diazinon, malathion, phos-
alone, tridemorph, and fenvalerate from the human hair and
water samples. The HF-SPME–HPLC-PDA proposed
method was successfully used for the analysis of pesticides
from the environmental biological. The LOD was found
between 0.004 and 0.095 ng/mL with a good percentage
recovery from 82 to 94 for the pesticides.[176] Jabbari et al.,
propose new ceramic–magnetic graphene (C–G/Fe3O4)
nanoparticles based SPME of organophosphorus pesticides
(OPPs) from the water samples, due to the 3 D structure of
the C–G/Fe 3O4 nanoparticles that making it suitable for the
SPME applications. Under the optimal conditions proposed
method obtained good linearity 0.05–400 mg/L and good
LOD value between 5 and 60 ng/L. The C–G/Fe3O4-SPME
materials were successfully used for the elimination of OPPs
in the spiked sample before analysis by the HPLC–UV[177]
Liu et al., developed new Mesoporous TiO2 nanoparticles
based SPME method for the extraction of six different
organochlorine pesticides (OCPs). The synthesized fabric
material possesses a homogeneous surface and good repro-
ducibility. The proposed method contains good linearity
5–5000 ng/L with acceptable LOD value 0.08–0.60 ng/L. The
developed method was successfully applied for the sensitive
determination of OCPs in the real water samples.[178] Zhang
et al., reported copper-based metal-organic framework
(MOF-199) with graphite oxide based new SPME based new
method for the extraction of organochlorine pesticides
(OCPs) from the real environmental samples. The LOD
value was obtained up to 2.3–6.9 ng/L with good percentage
recoveries 82.7%–96.8%, 90.6%–104.4%,
72.2%–82.8%–94.3%, and 107.7% respectively.[179] Heidari
and Razmi, reported carbon coated magnetic Fe3O4 (Fe3O4/
C) nanoparticles as a fabric material for the SPME apply for
the detoxification of organophosphorus pesticides (OPPs)
from the environmental samples coupling with the HPLC-
UV. Under the optimized condition the developed method
was applied for the determination of OPPs in the aqueous
system with low LOD value up to 4.3–47.4 pg/mL and
obtained high enrichment factors value in the ranging from
330–1200.[63] Also, Table 1 shows the different SPME based
reported methods for the extraction of pesticides using dif-
ferent materials.
Dispersive solid-phase microextraction
The dispersive solid-phase microextraction method is known
to be suitable for the proper extraction of analytes but is
mainly used as a cleaning step to minimize matrix environ-
ments.[84,203,204] Dispersive SPME (DSPME) is fast, cheap,
and efficient due to the fact that the method time, the
amount of adsorbent, and the desorption solution volume
are less than the DSPE method. For these reasons, it is more
preferred recently.[205] The DSPME method, based on the
device used to dispense the sorbent into the sample solution,
can be divided into three classes: (a) Traditional DSPME,
(b) Vortex supported DSPME and (c) Ultrasonically assisted
DSMPE Each of these methods can be divided into two
groups, depending on the type of sorbent. As a sorbent,
composite can also be classified into two subgroups (with
magnetic adsorbent and non-magnetic adsorbent). When
the studies in the literature are examined, it is determined
that the application areas of the DSPME method have been
developed over the years. The application area of ultrasonic-
ally assisted DSPME is more than the other two methods.
At the same time, there are many application areas of vortex
supported DSPME, which is more frequently preferred than
the conventional DSMPE method. When the adsorbent types
in which these three methods were applied were investi-
gated, it was determined by these investigations that non-
magnetic adsorbents were preferred more than magnetic
adsorbents and they had more application areas.[206]
Liquid-phase microextraction
LPME is a simple, fast, cheaper, selective, and sensitive tech-
nique as associated with other traditional removal techni-
ques. It was firstly introduced in the 1990s. Furthermore, it
widely uses for the analysis of environmental pollutants
including pesticides. LPME is hyphenated with the modern
chromatographic techniques to improve the extraction effi-
ciency and pretreatment.[41,207–209] LPME approach seems to
be a promising technique for the improvement of highly
sensitive standard processes since the related LOD of the
chromatographic technique can be at the ng/L. LPME is a
fast technique with a very less amount of solvent volume
Table 1. SPME used for the elimination of pesticides.
Analytes Microextraction Method Nanomaterials Real Samples Instrument PF/EF LOD (mg/L) Ref.
[180]
Hexachlorobenzene, In vivo SPME MWCNTs/PANI-PPy@PDMS Garlic samples GC-MS 2659, 1234, 438, 1764 0.76 1.90, 2.49, 0.39,
Chlorothalonil, Fipronil,
Chlorfenapyr
[181]
Prometon, Trietazine, SPME PDMS Surface water samples GC-MS — 0.002, 0.004, 0.007, 0.011,
Propazine, 0.006, 0.010, 0.014,
Terbutylazine, Atrazine, 0.013, 0.010, 0.017
Prometryn, Terbutryn,
Simazine,
Ametryn, Simetryn
[182]
Diazinon, SPME PDMS–2OHMe18C6 Strawberry, green apple GC-ECD — 0.0048, 0.0045, 0.0047
Chlorpyrifos, Profenofos, and red grape
[183]
Triazolone, Penconazole, MSPE Fe3O4@SiO2 Cucumber and GC-FID 845, 866, 903, 878, 895 0.12, 0.15, 0.14, 0.19, 0.18
Hexaconazole, cabbage samples
Diniconazole,
Tebuconazole
[184]
Tetramethrin, DLME-D-m-SPE Fe3O4@APTS Field water samples, HPLC-UV 108, 66, 51, 93 0.05, 0.5, 0.5, 2
Fenpropathrin, cucumber and cabbage
Deltamethrin,
Permethrin,
[185]
Chlorpyrifos, MSPE Fe3O4@TGA@TMU-6 Water and rice HPLC-UV 502, 394, 401 1.0, 0.5, 0.5
Profenofos, Phosalone,
[186]
Aldrin, DDD, DDE, DDT, SPME DVB/PDMS Plant sample GC-ECD — 0.102–1.693
Dieldrin, Endosulfan
[187]
23 multiclass pesticides SPME DVB/Car/PDMS fiber Drinking water samples GC-MS — 0.006–5.4545
[188]
Chlorpyrifos, Malathion, MD-lSPE amino-functionalized Coffee bean samples GC-ECD — 1.42, 1.43, 1.35, 1.33
Hexaconazole, Atrazine hollow silica-titania
microsphere
[189]
Malathion, Fenitrothion MDSPME chitosan–iron oxide Cucumber and GC-FID 17.1, 17.0 1.0, 0.3
magnetic orange samples
nanocomposite
[190]
Bifenthrin, Fenpropathrin, MSPE- DLLME-SFO Fe3O4/MIL-101(Cr) Water and tea samples GC-ECD — 0.009, 0.015, 0.012, 0.008
Permethrin,
Deltamethrin
[191]
Benzophenone, TF-SPME diatomaceous earth Real river water samples HPLC-DAD — 1, 1, 8, 8
triclocarban, 4-
methylbenzylidene
camphor, 2-ethylhexyl-
p-methoxycinnamate
[192]
Carbofuran, Molinate, RDSE-SPME divinylbenzene/carboxen/ Rice samples GC-MS — 2.5, 3.7, 0.57, 0.46, 5.90
Atrazine, Simazine, polydimethylsiloxane
Tebuconazole
[193]
Ametryn, Chlorpyrifos, AF-DSPE-DLLME polycarbonate Different fruit GC-FID 241, 310, 247, 256, 220, 0.61, 0.67, 0.57, 034, 0.46,
Penconazole, Oxadiazon, juice samples 443, 356 1.20, 100
Diniconazole,
Clodinafop–propargyl,
Tebuconazole
[194]
24 pesticides SPME Carbon nanomaterial Water samples GC-MS — 0.0002–1.1309
[195]
Methomyl, carbaryl, SPME Conjugated Water sample UPLC-MS/MS 65–100 0.0020, 0.010, 0.0025,
aldicarb-sulfoxide, microporous polymers 0.010, 0.0090, 0.0070,
propoxur, aldicarb, 0.0090, 0.010,
carbofuran, aldicarb- 0.050, 0.025
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY

sulfone, methiocarb,
(continued)
7
Table 1. Continued. 8
Analytes Microextraction Method Nanomaterials Real Samples Instrument PF/EF LOD (mg/L) Ref.
carbofuran-3–hydroxyl,
ox-amyl
[196]
Ethoprophos, Sulfotep, SPME Hydroxyl- Water samples GC-FPD — 0.50, 0.08, 0.18, 1.01, 0.66,
Cadusafos, Phorate, functionalized graphene 0.04, 0.03, 0.21
Terbufos, Fonofos,
Chlorpyrifos, Parathion
[187]
10 OCP, Carbofuran, DI-SPME DVB/Car/PDMS Water samples GC-ECD — 0.006, 0.212, 0.181, 0.606,
Molinate, Trifluralin, fiber coating 0.06, 0.036, 0.272, 0.606,
M. S. JAGIRANI ET AL.

Atrazine, Terbufos, 0.303, 0.909, 0.606,

Parathion methyl, 0.006, 1.8, 5.45, 0.606
Alachlor, Metolachlor,
Chlorpyriphos,
Pendimethalin,
Chlordane, Profenofos,
Tebuconazole,
Permethrin
[197]
Malathion, Diazinon, SPME GG/GO/PANI Grape, apple juice and HPLC-UV — 0.003, 0.03, 0.03, 0.03
Phosalone, Chlorpyrifos fresh tomato samples
[198]
14 OPPs DI-SPME C-(C3N4@MOF) Fruit and GC-MS — 0.23–0.75
vegetable samples
[198]
Diazinon, Parathion-methyl, Multifiber SPME SPME fiber Chinese cabbage and GC-NPD — 0.0052, 0.098, 0.014,
Pirimiphos-methyl, cherry tomato samples 0.23, 0.082
Isocarbophos,
Quinalphos
[199]
Diazinon, Chlorpyrifos DI-SPME (PDMS/DVB) fiber Juice samples GC-NPD — 0.18, 0.20
[200]
Diazinon, Chlorpyrifos, SPE– DLLME Magnetic graphene oxide Fruit samples GC-FID 399, 384, 340, 369 1.8, 1.0, 6.0, 1.5
Phosalone, Ametryn
[201]
20 UASE-HS-SPME PDMS fiber Marine water samples GC-MS/MS — 0.01–0.27
organochlorine
pesticides
[202]
Carbamate pesticides SPME VPED-MMF Water and Fruit HPLC-UV 0.038–0.39
juice samples

Figure 4. Different types of LPME.[214]
used during the extraction process. Normally the LPME pro-
ceed among the less amount of water-immiscible solvents
and the water contain the targeted analyte. The acceptor
phase could be in the form of suspension for the headspace
extraction or directly absorbed.[10,210–212] It contains a high
enrichment factor. Currently, LPME had been working
under the different three extraction modes including
SDME,[105] DLLME, and hollow-fiber LPME (HF-
LPME).[213] Figure 4 represents the different types of LPME.
Single-drop microextraction
The SDME was first reported by Cantwell et al. in 1996 they
used a single organic drop as the acceptor phase that is dir-
ectly combined with the GC analysis.[215]The objects of
designing this approach comprise to achieve high enrich-
ment factor the wish to ease interferences from the sample
matrices. SDME mode is based on the distribution of the
analytes among a micro-drop of organic solvent at the tip of
a micro-syringe injection and aqueous solution of the sam-
ple. This technique combines elimination, pretreatment, and
sample inserting into a single step.[106,107,216] Now the
SDME has different modes which are categorized into two
or three phases it depends on the number of phases co-
existing at the equilibrium. In the two-phase mode direct
immersion, constant flow, droplet to droplet, and directly
suspended droplets while the three-phase mode comprises
liquid–liquid-liquid microextraction and headspace SDME is
a simple, sensitive cheaper, and greener method for the
extraction of pollutants.[105,106]
Dispersive liquid-liquid microextraction
In present years easy and highly efficient method of sample
preparation, DLLME method have been widespread, in this
method a very small volume (microliters) of elimination sol-
vents and conforms the accomplishment of high coefficients
of analytes pretreatment. The qualities of this method very
small volume of a mixture of solvent and dispersive are
quickly injected into an aqueous solution of a sample using
the needle. As a consequence, the extractant is completely
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 9
dispersed into the aqueous sample as smaller drops with a
high surface area that favors significant upsurges in the rate
transfer and efficient extraction of analyte in the droplets of
extraction solvent. DLLME was firstly reported in 2006.
DLLME is new sample preparation and pretreatment tech-
nique, it proposing a high enrichment factor and a smaller
volume of water samples. It is widely applied due to its
returns such as time-saving, simplicity, cost-effectiveness,
and ease to method development, which make it existing to
virtually analytical laboratories.[17,109,209,217–220]
Hollow-fiber LPME
HF-LPME firstly introduced Pedersen-Bjergaard and
Rasmussen in 1999[221,222] to escape the drop instability in
SDME and fabricated on the basis of liquid membrane elim-
ination Last 5 years this technique widely used in different
analytical fields for the analysis of different matrices such as
soil, food, water and environment to extract different analy-
tes such as polybrominateddiphenyl ethers,[223,224] polycyclic
aromatic hydrocarbons,[225,226] chlorophenols[227] and poly-
chlorinated biphenyls,[226] and also pesticides including 12
organochlorine pesticides (OCPs), a group of seven and
eight multiclass pesticides,[228] vinclozin[229] and OCPs, six
organosulfur pesticides.[230] Figure 5 shows the extraction
process of LPME.
Application of LPME
Maria Asensio-Ramos et al., a novel simple has been devel-
oped for the extraction of benzimidazole pesticides such as
carbendazim/benomyl, fuberidazole, and thiabendazole a
carbamate and organophosphate (triazophos) from the soil
using two-phase HF-LPME using 1-octanol as extraction
solvent. At the optimal condition, HF-LPME-HPLC-FD
obtained good linearity, accuracy, and precision. The LODs
were found in the range of 0.001–6.94 ng/g (S/N ¼ 3). The
proposed method was applied to different matrices.[231]
Bolanos et al. reported HF-LPME based method for the
extraction of different kinds of 50 pesticides from alcoholic
beverages after extraction the samples were determined by
10 M. S. JAGIRANI ET AL.
Figure 5. Schematic view of extraction of process LPME.
the UHPLC–MS/MS. Under the optimized condition, this
method HF-LPME- UHPLC–MS/MS achieves good linear-
ity with a low value of LOD 0.01–5.61 g/L. Finally, the pro-
posed method was applied for the real samples,[232] Zhang
et al., proposed a method for the LPME of five different
carbamate pesticides using Trimethylphenyl- ammonium
hydroxide (TMPAH) and trimethylsulfonium hydroxide
(TMSH) before using the GC–MS, the LOD of the devel-
oped method was found up 0.2 and 0.8 g/L, it provided
good enrichment factor up to 224. The proposed method
was successfully applied for the extraction of carbamate
pesticides from the real water samples.[233] Huang et al.,
developed a new method for the extraction of organochlor-
ine pesticides applying a solvent cooling assisted dynamic
hollow-fiber-supported- HS-LPME, before using the
GC–MS analysis. The proposed method was achieved good
enrichment was 65–211 with an acceptable value of LOD
0.209 g/l.[234] Basheeret al. proposed a new efficient method
for the extraction of OPPs thionazin, triethyl-phosphoro-
thioate, phorate, sulfate, methyl parathion, disulfoton, and
ethyl parathion from the water samples using binary solv-
ent-based two-phase hollow fiber membrane (HFM)- pro-
tected with (BN-LPME) before the using the GC/MS. The
LOD was found up to 0.3–11.4 ng L
1. The proposed pro-
cedure was applied for the real water to extract the pesti-
cides.[235] Liu & Quan, proposed this work for the
extraction of OPPs such as fenitrothion, phoxim, and etho-
prophos using ionic liquids (1-benzyl-3-methylimidazolium
bis[(trifluoromethyl)sulfonyl]imide ([BeMIM][Tf2N])) based
DLLME prior HPLC-UV analysis. Under the optimized
condition, we obtained a good enrichment factor with
good LOD 0.1 lg/kg.[110] Lu et al. developed ionic liquids
(3-methyl-1-(ethoxy carbonyl methyl) imidazoliumbis(tri-
fluoromethylsulfonyl)-imide [MimCH2COOCH3][NTf2])
based DLLME of Ops from the water with good enrich-
ment factor 400, good percentage recovery, and reproduci-
bility. Table 2 shows the application of LPME used for the
elimination of different pesticides from food and environ-
mental samples.[295]
Conclusion
Green methods play a significant role during the analysis of
pesticides because they follow the protocols of green chemis-
try. During the analysis of pesticides lot of secondary pollu-
tants contaminant, the environment, the green methods
used to avoid these secondary pollutants. The microextrac-
tion is fulfilled the requirement of green chemistry during
the sample preparation contains less amount of solvent or
without the solvent. Microextraction techniques are simple,
cheaper, greener highly selective and sensitive, and environ-
mentally friendly. The SPME is a simple called solvent-free
technique. This technique work on the principles of adsorp-
tion and desorption it is a very simple technique. The
LPME contains a very low amount of organic solvent during
the extraction of pesticides from the environment. The
microextraction techniques obtained high percentage recov-
eries and high enrichment factor In Microextraction techni-
ques different materials have been used such as
nanomaterials, nanocomposites, imprinted polymers, ionic
liquids, switchable solvents, deep eutectic solvents. These
materials are used to enhance the selectivity and sensitivity
toward the pesticides.
Table 2. LPME based green techniques for the extraction of pesticides.
Analytes Microextraction Method Real Samples Instrument PF/EF LOD (mg/L) Ref.
[236]
2,4-D, MCPA, Dicroprop, SUPRAS-LPME Water, rice HPLC-DAD 37, 52, 59, 59, 119, 149 2.0, 1.0, 2.0, 2.0, 1.0, 1.0, 1.0
Mecoprop,2,4-DB, MCPB
[237]
Propham, Chlorpropham, BID Water GC-MS 952, 985, 807, 926, 574, 0.02, 0.04, 0.03, 0.02, 0.02, 0.02,
Promecarb, Carbofuran, 751, 1038, 1025 0.022, 0.03
Aminocarb, Pirimicarb,
Carbaryl, Methlocarb
[238]
Penconazole, Hexaconazale, TAT-DLLME Packed grape juice GC-FID 9970, 9800, 9940, 0.08, 0.09, 0.10, 0.10, 0.13
Diniconazole, Tebuconazole Fresh cucumber 9715, 9889
Difenoconazole Tomato
[239]
Dichlobenil, a-HCH, HLLE–DLLME Cacao powder GC–ECD 89, 50, 65, 74 0.024, 0.041, 0.0320, 038
b-HCH, Aldrin
[240]
Carbofuran, Carbaryl, MSA-DLLME Tea samples HPLC-DAD 130, 177, 185 0.41, 0.13, 0.61
Isocarbophos
[241]
SAC, KTP, NAX, DIC, IBU mLPME Urine, saliva, river and HPLC-UV 29, 25, 34, 45, 75 0.1, 0.1, 0.1, 0.1, 0.5
lake samples
[242]
Heptachlor, Aldrin, a-Endosulfan, DHFP-LPME Tea leaves sample GC-ECD 221, 34, 297, 46, 254, 92 0.031, 0.059, 0.053, 0.054,
p,p’-DDE, Dieldrin, o,p’-DDT 0.043, 0.164
[243]
Penconazole, Hexaconazole, AALLME Surface water, packed grape GC-FID 483, 449, 504, 456, 479 0.20, 0.30, 0.40, 0.70, 1.10
Diniconazole, juice, fresh grape juice,
Tebuconazole, Triticona cucumber and tomato
[244]
Penconazole, Hexaconazole, DLLME Surface water, packed grape GC-FID 79, 80, 101, 143, 142 1.90, 3.20, 4.00, 3.90, 5.90
Diniconazole, juice, fresh grape juice,
Tebuconazole, Triticona cucumber and tomato
[244]
18 organophosphorus FA-DSDME Human blood samples LC-MS/MS 30–132 0.0009–0.122
pesticides (OPPs)
[245]
Diazinon, Ametryn, Chlorpyrifos, LLE-DLLME Honey samples GC-FID 353, 289, 400, 350, 428, 0.0011, 0.0011, 0.00069, 0.00057,
Penconazole, Oxadiazon, 374, 279 0.0032, 0.0071, 0.012
Diniconazole, Fenazaquin
[246]
Myclobutanil, Triadimefon, UAATPE- VADLLME Longan sample HPLC-DAD 48.80, 45.90, 48.80, 47.80, 11.06, 17.40, 9.57, 13.97, 8.07,
Tebuconazole, Hexaconazole, 45.80, 49.80, 44.30, 5.58, 7.74, 7.18, 7.49
Diniconazole, Fenpropathrin, 45.40, 52.90
Deltamethrin,
Permethrin, Bifenthrin
[247]
Penconazole, Hexaconazole, AALME Surface water, grape juice, GC-FID 775, 753, 713, 782, 808 0.55, 0.53, 0.56, 0.59, 1.13
Diniconazole, Tebuconazole, cucumber juice and
Triticonazole, tomato juice
[248]
Tetramethrin, Fenpropathrin, DLLME Fruit juices samples HPLC-UV 62–84 2–5
Cypermethrin,
Deltamethrin, Permethrin
[249]
Esbiothrin, Prallethrin, Bifenthrin, HF-LPME Water samples GC-MS 139–255 0.002–0.012
Tetramethrin, Phenothrin,
Permethrin, Cyfluthrin,
Cypermethrin, Deltamethrin
[250]
Bifenthrin, Phenothrin, SPI-SFO–HLLME grape, sour cherry, mango, GC-MS 370, 460, 365, 415, 440, 0.029, 0.006, 0.038, 0.009, 0.013,
Tetramethrin, Fenpropathrin, apricot, peach, and 405, 410, 375, 425, 395 0.026, 0.012, 0.034,
Cyhalothrin, Permethrin, orange juices 0.015, 0.033
Cypermethrin, Cyfluthrin,
Flucythrinate, Deltamethrin
[251]
Dichlorvos, Diazinon. SB-DLLME apple juice, grape juice, orange GC-FID 466, 473, 509, 564, 616 1.4, 0.5, 0.2, 1.0, 0.9
Chlorpyrifos, juice, and mango juice
Profenofos, Phosalone
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY

[252]
o,o,o-Triethylphosphorothioate, SFE-DLLME Marine sediment samples GC-FID 138, 82, 144, 125, 140, 3, 6, 2, 1, 9, 5, 9
Thionazin, Sulfotepp, 121, 67
(continued)
11
Table 2. Continued. 12
Analytes Microextraction Method Real Samples Instrument PF/EF LOD (mg/L) Ref.
Disulfoton, Methyl Parathion,
Parathion, Famphur
[253]
Penconazole, Hexaconazole, SPE-DLLME Grape juice samples GC-FID 4101, 10556, 9594, 0.053, 0.061, 0.128, 0.139, 0.890
Diniconazole, Tebuconazaole, 8499, 5380
Triticonazole
[254]
Chlorpyrifos DLLME-SFO Groundwater and soil sample GC-FPD 232.42 2.81
[255]
Diazinon, Malathion, Phosalone, IL-DLLME HPLC-MS — 0.07, 0.19, 0.06, 0.08, 0.03, 0.06
Imidacloprid, Biphenthrin,
M. S. JAGIRANI ET AL.

Cypermethrin
[256]
Prometon, Simetryn, Propazine, DLLME Water samples 1750–2100 0.05, 0.10, 0.10, 0.10, 0.10
Atrazine, Simazine
[257]
Bixafen, Fipronil, Bixafen, Fipronil BDLLME domestic and industrial GC-MS, B-DLLME 7.8, 119 56, 725, 7.3, 6.1
wastewater, soil and
mint samples
[258]
Atrazine, Ametryn, Propazine DLLME sunflower oil, corn oil, soybean GC-NPD 78, 74, 96 0.02, 0.06, 0.09
oil, and grapeseed oil
[259]
Penconazole, Hexaconazole, SEV-DLLME Waste water, well water, grape GC-FID 2738, 1580, 482, 974, 0.11, 0.09, 0.14, 0.78, 0.69, 1.04
Tebuconazole, Triticonazole, juice, apple juice 1048, 1142
Difenconazole (1),
Difenconazole (2)
[260]
Diazinon, Ametryn, Chlorpyrifos, Salt–induced HLLME Apple, sour cherry, peach, grape, GC-FID 455, 410, 420, 480, 465, 0.22, 0.37, 0.35, 0.27, 0.29,
Penconazole, Oxadiazon, orange juice samples 425, 435 0.48, 0.46
Diniconazole, Fenazaquin
[261]
Transfluthrin, Fenpropathrin, DLLME Water samples HPLC-UV 49, 55, 58, 57 0.56, 0.45, 0.41, 0.65
Cyhalothrin, Permethrin
[262]
o,o,o-Triethyl phosphorothioate, LPME Water samples GC-FPD 807, 699, 1302, 745, 997, 0.01, 0.01, 0.01, 0.02, 0.01, 0.03,
Thionazin, Sulphotepp, 1110, 891, 976, 621 0.02, 0.02, 0.04
Phorate, Dimethoate,
Disulphoton, Methyl
parathion, Parathion, Famphur
[263]
Chlortoluron, prometon, IL-DLLME Honey sample HPLC 34–65 6.92, 5.84, 8.55, 8.59, 5.31,
propazine, linuron, prebane,
[109]
Metalaxyl, Chlorpyrifos, DES-DLLME Green tea, rose water and herbal GC-FID 1760, 2042, 2487, 2447, 0.22, 0.23, 0.16, 0.12, 0.12, 0.16,
Penconazole, Haloxyfop-R- distillates 2197, 2073, 2520, 2321, 0.16, 0.15, 0.11
methyl, Oxadiazon, 2444, 2853, 0.20
Diniconazole, Clodinafop-
propargyl, Fenpropathrin,
Fenazaquin, Fenoxaprop-
P-ethyl
[111]
Diazinon, Isazofos, Chlorthiophos, DLLME Honey sample GC-MS 94, 89, 84, 97, 98, 82, 86, 0.10, 0.05, 0.08, 0.06, 0.07, 0.09,
Chloropyrifos, Fenthion, 93, 91 0.08, 0.09, 0.10
Malathion, Fenthionsulfoxide,
Piperophos, Anilofos
[264]
Malathion, Heptachlor, epoxide, MSPE/DLLME Fruit juice samples GC-ECD 332, 349, 285, 210, 320, 0.006, 0.013, 0.01, 0.022, 0.008,
Endrin, 2,4-DDT, Azinphos 540, 340 0.038, 0.023
ethyl, Cypermethrin,
Deltamethrin
[265]
Transfluthrin, Allethrin, UA-DLLME Domestic waste watersamples GC-FID 1725, 1605, 1509, 1214, 0.4, 0.3, 0.2, 0.3, 0.6, 0.4, 0.6,
Prallethrin, Imiprothrin, 768, 739, 803, 728, 748 0.5, 0.7
Tetramethrin, Phenothrin,
Cypermethrin,
Cyphenothrin, Permethrin
[266]
DLLME Milk and water samples GC-FID and GC-MS 156–400 2–58
Penconazole, Hexaconazole,
Tebuconazole, Triticonazole,
Difenconazole (1),
Difenconazole (2)
[267]
Prophos, Diazinon, Chlorpyrifos DLLME Water samples GC-MS 319, 259, 257, 382, 5.1, 3.9, 1.5, 9.1, 1.9, 2.5
methyl, Methyl parathion, 249, 235
Fenchlorphos, Chlorpyrifos
[268]
2,4-D, MCPA RM-DLLME Water samples HPLC-UV 148, 157 0.8, 0.5
[269]
Dichlobenil, a-HCH, DLLME Various cocoa powder and GC-ECD 85, 92, 76, 74 0.017, 0.011, 0.022, 0.031
b-HCH, Aldrin bean samples
[270]
Fenpropathrin, cyhalothrin, DLLME-SFO Water samples GC-ECD 475–790 0.0015, 0.0014, 0.0029, 0.0014
permethrin, tau-fluvalinate
[271]
Permethrin, deltamethrin, USA-MNF-LPME Soil, water, and milk GC-MS 413.1 0.00281
cypermethrin
[272]
Diazinon, Malathion, SS-LPME Tomato samples GC-MS 155, 152, 152 6.3, 7.1, 4.8,
Chloropyrifos
[273]
Chlorimuron ethyl, bensulfuron DSPE-DLLME Soil samples MEKC 3000–5000 1.0, 1.0, 0.5, 0.5, 0.5
methyl, tribenuron methyl,
chlorsulfuron,
metsulfuron methyl
[274]
Carbofuran, carbaryl, pirimicarb SPE-DLLME Fruits and vegetables HPLC-UV 5400–7650 0.005–0.06
[275]
Pirimicarb, Carbaryl, Methiocarb, LLE-IL-DLLME Fruit juice HPLC-DAD 160, 205, 217, 147, 197 2.3, 0.64, 0.45, 3.9, 3.3
Aldicarb, Carbofuran
[276]
Dichlorovos, Mevinphose, HLLME Water samples GC-FPD 317, 274, 327, 325, 260, 0.02, 0.02, 0.005, 0.01, 0.01, 0.01,
Phorate, Diazinon, Disolfotane, 665, 369, 344, 455, 324, 0.01, 0.01, 0.01, 0.01, 0.005,
Methylparathion, Sumithion, 658, 315, 478, 562, 394 0.01, 0.02, 0.04
Chloropyrifose, Malathion,
Fenthion, Profenphose, Ethion,
Phosalone, Azinphose methyl,
Co-Ral
[277]
Permethrin, Bifenthrin, MA-HLLME Fruit and vegetable samples GC-MS 371, 365, 315, 415, 335 6.3, 9.3, 9.4, 4.3, 5.5
Deltamethrin, Cyhalothrin,
Cypermethrin
[278]
Metalaxyl, Chlorpyrifos, LTI–HLLE–DES–DLLME Various cucumber samples GC-FID 290, 365, 310, 305, 335, 0.88, 0.61, 0.81, 0.83, 0.68, 0.48,
Penconazole, 365, 300, 380, 405, 315 0.79, 0.49, 0.42, 0.76
Haloxyfop–R–methyl,
Oxadiazon, Diniconazole,
Clodinafop–propargyl,
Fenpropathrin, Fenazaquin,
Fenoxaprop–P–ethyl
[279]
Chlorpyrifos, Diazinon, QuEChERS–DLLME Fruit and vegetables GC-FID 265, 240, 340, 375, 340 0.48, 0.38, 0.39, 0.27, 0.30
Diniconazole, Oxadiazon,
Penconazole
[280]
Chlorpyrifos, Penconazole, HLLE-DLLME-SFO Fruit juices and fruits GC-FID 3659, 3265, 3490, 3416, 0.56, 0.47, 0.20, 0.45, 0.34, 0.51,
Haloxyfop-R-methyl, 3271, 3473, 3517, 0.25, 0.37, 0.60
Oxadiazon, Diniconazole, 3443, 3728
Clodinafop-propargyl,
Fenpropathrin, Fenazaquin,
Fenaxaprop-P-ethyl
[281]
Bifenthrin, Fenpropathrin, DLLME-SFO Real liquid milk GC-ECD — 0.09, 0.08, 0.16, 0.22, 0.44,
Cyhalothrin, Permethrin, 0.38, 0.29
Flucythrinate, Fenvalerate,
Deltamethrin,
[282]
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY

Diazinon, Malathion, Chlorpyrifos MFEM Water samples GC-FID 306, 329, 342 4, 8, 6
[283]
Chlorpyrifos, Penconazole, PCL–g–GQDs–based Fruit juices GC-FID 714, 691, 732, 754, 792, 4.8, 5.5, 5.1, 5.4, 4.76, 5.3, 6.2,
Haloxyfop–R–methyl, DSPE–DLLME 815, 840, 803, 680 6.7, 4.9
(continued)
13
Table 2. Continued. 14
Analytes Microextraction Method Real Samples Instrument PF/EF LOD (mg/L) Ref.
Oxadiazon, Diniconazole,
Clodinafop–propargyl,
Fenpropathrin, Fenazaquin,
Fenoxaprop–P–ethyl
[284]
Carbaryl UAMSPE water UV-Vis — 33
[285]
Carbaryl, Hexythiazox, In matrix-DES-SFO-DLLME Cow milk GC-FID 390, 425, 430, 390, 365, 1.6, 2.1, 1.8, 2.4, 1.3, 3.9, 0.9
Pretilachlor, Iprodione, 320, 445,
Famoxadone,
M. S. JAGIRANI ET AL.

Sethoxydim, Fenazaquin
[286]
Diazinon, Malathion, Chlorpyrifos MWA–DLLME Aqueous sample GC-FID 1340, 1900, 1880 0.65, 1.30, 0.74
[287]
Multi-residue pesticides (19 units) SPE-DLLME Water, fruit, honey, and milk GC-MS/SIM 2362–10,593 0.5–1.0
[288]
Deltamethrin, Fenvalerate, DES-UA-DLLME Water samples HPLC-UVD 129, 131, 136, 129, 127 0.60, 0.30, 0.60, 0.30, 0.60
Permethrin,
Etofenprox, Bifenthrin
[289]
Etrimfos, Fenthion, Diazinon, DSPE–DES–SFOD–DLLME Sunflower, olive, corn, canola, GC-NPD 170, 183, 192, 175 0.24, 0.11, 0.06, 0.19
Chloropyrifos and sesame oils
[290]
Flucythrinate, Beta-cypermethrin, VA-EME Mushroom HPLC-DAD — 0.10–0.19
Fenvalerate
[245]
Diazinon, Ametryn, Chlorpyrifos, LLE-DLLME Honey samples GC-FID 353, 289, 400, 350, 428, 11, 1.1, 0.69, 0.57, 0.32,
Penconazole, Oxadiazon, 374, 279 0.71, 1.20
Diniconazole, Fenazaquin
[291]
a-HCH, HCB, 4,4-DDT, BDE-28, VALLME Oil samples GC-MS/MS — 0.5, 0.4, 0.4, 0.2, 0.3, 0.5, 0.5, 0.7
BDE-47, BDE-99, BDE-153,
BDE-154
[292]
Triadimenol, Fipronil, UA-ELPME Different herbal HPLC-DAD — 0.2, 0.02, 0.2, 0.2, 0.2
Tebuconazole, Hexaconazole, medicine samples
Diniconazole
[293]
Myclobutanil, Tebuconazole, DCF-EME Water sample GC-MS 409, 342, 473, 372 0.14, 0.24, 0.17, 1.04
Epoxiconazole, Difenoconazole
[294]
Nimesulide, Indomethacin, LD-DLLME Water samples HPLC-DAD 35, 42, 64, 66 0.81, 0.11, 1.14, 0.26
phenylbutazone,
flufenamic acid
[294]
a –Endosulfan, b –Endosulfan BAlE Tea samples GC-MS — 8.0, 4.0
 CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 15

Acknowledgments GC-NFD gas chromatography–nitrogen phos-

phorous detector
Dr. Muhammad Saqaf Jagirani would like to thank the TUBITAK 2221 GC-NPD gas chromatography–nitrogen phos-
Postdoctoral fellowship/visiting researchers. The authors are also grate- phorus detection
ful for the financial support of the Unit of the Scientific Research GG/GO/PANI graphenized graphite/graphene oxide/
Projects of Erciyes University (FBG-2020-10013) (Kayseri, Turkey). polyanilinenanocomposite
HF-LPME hollow fiber-based liquid-phase
microextraction
Abbreviations HLLE homogenous liquid–liquid extraction
HLLE-DLLME-SFO homogeneous liquid-liquid extraction-
a-HCH a-Hexachlorocyclohexane dispersive liquid-liquid microextraction
b-HCH b-Hexachlorocyclohexane solidification of floating organic drop
mLPME microfluidic based liquid-phase HLLME homogeneous liquid–liquid
microextraction microextraction
2,4-D 2,4-dichlorophenoxyacetic acid IBU ibuprofen
2,4-D2 4-dichlorophenoxyacetic acid IL ionic liquid
2,4-DB 4-(2,4-dichlorophenoxy) butanoic acid KTP ketoprofen
AALLME air-agitated liquid–liquid LC–MS/MS liquid chromatography tandem mass
microextraction spectrometry
AALLME air-assisted liquid–liquid LD-DLLME low denstity-dispersive liquid liquid
microextraction microextraction
APTS 3-aminopropyl triethoxysilane LLE-DLLME liquid–liquid extraction–dispersive
BAlE bar adsorptive microextraction liquid–liquid microextraction
BDLLEME binary dispersive liquid-liquid microex- LLLME on-line hollow fiber liquid–liquid–liquid
traction method
microextraction
BID bubble-in-drop microextraction
LPME liquid phase microextraction
D-m-SPE dispersive m-solid phase extraction
LTI-HLLE-DES-DLLME low temperature–induced homogenous
DCF-EME carbon dioxide flotation after emulsifi-
liquid–liquid extraction–deep eutectic
cation microextraction
solvent–based dispersive liquid–liquid
DDD 1,1-dichloro-2,4-
bis[chlorophenyl]ethane microextraction
DDE 1,1-dichloro-2,2-bis[p- MA-HLLME microwave assisted homogeneous
chlorophenyl]ethylene liquid–liquid microextraction
DDE dichlorodiphenyldichloroethylene MCPA 4-chloro-2-methylphenoxyacetic acid
DDT 1,1,1-trichloro-2,2-bis[p- MCPA2 methyl-4-chlorophenoxyacetic acid
chlorophenyl]ethane MCPB 4-(4-Chloro-2-methylphenoxy) buta-
DDT dichlorodiphenyltrichloroethane noic acid
DES deep eutectic solvents MDSPME magnetic dispersive solid-phase
DES-FF-DSDME deep eutectic solvent based ferrofluid- microextraction
directly suspended droplet Mecoprop 2-(4-Chloro-2-methylphenoxy) propa-
microextraction. noic acid
DHFP-LPME dynamic hollow fiber protected liquid MEKC micellarelectrokinetic chromatography
phase microextraction MFEM microfunnel-filter-based emulsification
DIC diclofenac microextraction magnetic solid phase
Dichloprop 2-(2,4-dichlorophenoxy) propanoic acid extraction (MSPE) coupled
DI-SPME direct immersion mode solid phase with dispersive
microextraction MGO-SPE-DLLME magnetic graphene oxide based–solid
DLLME dispersive liquid–liquid microextraction phase extraction–dispersive liquid–li-
DLLME dispersive liquid–liquid microextraction quid microextraction
DLLME-SFO dispersive liquid–liquid microextraction MSA-DLLME stirring-assisted dispersive liquid–liquid
based on solidification of the floating microextraction
organic droplets MSPE magnetic solid phase extraction
DLLME-SFO dispersive liquid–liquid microextraction MWCNTs/PANI-PPy@PDMS multiwalled carbon nanotubes/polyani-
with solidification of a floating line-polypyrrole@polydimethylsiloxane
organic drop NAX naproxen
DLLME-SFO liquid–liquid microextraction based on PCL-g-GQDs-based
the solidification of floating DSPE-DLLME poly (e–caprolactone) grafted graphene
organic drop quantum dots–based dispersive solid
DLME/D-m-SPE dispersive liquid microextraction com- phase extraction– dispersive liquid–li-
bined with dispersive m-solid quid microextraction
phase extraction PDMS polydimethylsiloxane
DVB/PDMS divinylbenzene/polydimethylsiloxane PDMS–2OHMe18C6 polydimethylsiloxane–2-hydroxymethyl-
FA-DSDME fast agitated directly suspended droplet 18-crown-6
microextraction QuEChERS quick easy cheap effective rugged and
GC-ECD gas chromatography combined-electron safe method
capture detection RM-DLLME reverse micelle-mediated dispersive
GC-FPD gas chromatography with flame pho- liquid–liquid microextraction
tometry detection SAC salicylic acid
GC-MS gas chromatography-mass spectrometry SB-DLLME solid-based disperser liquid–liquid
microextraction
16 M. S. JAGIRANI ET AL.

SBSE-DLLME stir bar sorptive extraction combined Physiol. 2019, 156, 129–137. DOI: 10.1016/j.pestbp.2019.02.
with dispersive liquid–liquid 014.
microextraction [7] Machado, I.; Gerez, N.; Pist
on, M.; Heinzen, H.; Cesio, M. V.
SEV-DLLME silylated extraction vessel-dispersive Determination of Pesticide Residues in Globe Artichoke
liquid–liquid microextraction Leaves and Fruits by GC-MS and LC-MS/MS Using the Same
SFE-DLLME supercritical fluid extraction dispersive QuEChERS Procedure. Food Chem. 2017, 227, 227–236. DOI:
liquid–liquid microextraction 10.1016/j.foodchem.2017.01.025.
SFO-LPME solidification of floating organic drop- [8] Suganthi, A.; Bhuvaneswari, K.; Ramya, M. Determination of
lets microextraction Neonicotinoid Insecticide Residues in Sugarcane Juice Using
SIM selective ion monitoring LCMSMS. Food Chem. 2018, 241, 275–280. DOI: 10.1016/j.
SS-LPME in syringe dispersive liquid–phase foodchem.2017.08.098.
microextraction method couple [9] Atwood, D.; Paisley Jones, C. Pesticides Industry Sales and
SUPRAs supramolecular solvents Usage (Rep.) from U.S. Environmental Protection Agency.
TAT-DLLME temperature-assisted tandem dispersive http://www.epa.gov/sites/production/files/2017-01/documents/
liquid–liquid microextraction pesticides-industry-sales-usage-2016_0.pdf. January 13, 2018.
TF-SPME thin-film solid-phase microextraction [10] Lawal, A.; Wong, R. C. S.; Tan, G. H.; Abdulra’uf, L. B.;
TGA thioglycolic acid Alsharif, A. M. A. Multi-Pesticide Residues Determination in
UAATPE-VADLLME ultrasonic-assisted aqueous two-phase Samples of Fruits and Vegetables Using Chemometrics
extraction coupled to vortex-assisted Approach to QuEChERS-dSPE Coupled with Ionic Liquid-
dispersive liquid-liquid microextraction Based DLLME and LC–MS/MS. Chromatographia 2018, 81,
UA-DLLME ultrasound-assisted dispersive liquid–li- 759–768. DOI: 10.1007/s10337-018-3511-7.
quid microextraction [11] Tong, Z.; Dong, X.; Yang, S.; Sun, M.; Gao, T.; Duan, J.; Cao,
UA-DLLME-DES ultrasound-assisted dispersive liquid- H. Enantioselective Effects of the Chiral Fungicide
liquid microextraction method based on Tetraconazole in Wheat: Fungicidal Activity and Degradation
hydrophobic deep eutectic solvent Behavior. Environ. Pollut. 2019, 247, 1–8. DOI: 10.1016/j.env-
UA-ELPME ultrasound-assisted emulsification liquid pol.2019.01.013.
phase microextraction [12] Lin, X.-Y.; Mou, R.-X.; Cao, Z.-Y.; Cao, Z.-Z.; Chen, M.-X.
UAMSPE ultrasound-assisted dispersive solid Analysis of Pyrethroid Pesticides in Chinese Vegetables and
phase microextraction Fruits by GC–MS/MS. Chem. Pap. 2018, 72, 1953–1962. DOI:
UASE-HS-SPME ultrasound-assisted solvent extraction 10.1007/s11696-018-0447-1.
combined headspace solidphase [13] Pirsaheb, M.; Fattahi, N.; Karami, M.; Ghaffari, H. R.
microextraction Simultaneous Determination of Deltamethrin, Permethrin and
USA-MNF-LPME ultrasound assisted magnetic nanofluid Malathion in Stored Wheat Samples Using Continuous Sample
based liquid phase microextraction Drop Flow Microextraction Followed by HPLC–UV. Food
VA-EME vortex-assisted emulsification Measure. 2018, 12, 118–127. DOI: 10.1007/s11694-017-9622-2.
microextraction [14] Kabir, E. R.; Rahman, M. S.; Rahman, I. A Review on
VALLME vortex assisted liquid-liquid Endocrine Disruptors and Their Possible Impacts on Human
microextraction Health. Environ. Toxicol. Pharmacol. 2015, 40, 241–258. DOI:
VPED-MMF new monolithic adsorbent-multiple 10.1016/j.etap.2015.06.009.
monolithic fiber (poly(vinylboronic [15] Aguilera-Luiz, M. M.; Plaza-Bolanos, P.; Romero-Gonzalez, R.;
anhydride pyridine complex-co- Vidal, J. L.; Frenich, A. G. Comparison of the Efficiency of
ethylenedimethacrylate) Different Extraction Methods for the Simultaneous
Determination of Mycotoxins and Pesticides in Milk Samples
by Ultra High-Performance Liquid Chromatography-Tandem
References Mass Spectrometry. Anal. Bioanal. Chem. 2011, 399,
2863–2875. DOI: 10.1007/s00216-011-4670-7.
[1] Kalia, A.; Gosal, S. Effect of Pesticide Application on Soil [16] Mohammadi, M.; Tavakoli, H.; Abdollahzadeh, Y.; Khosravi,
Microorganisms. Arch. Agron. Soil Sci. 2011, 57, 569–596. A.; Torkaman, R.; Mashayekhi, A. Ultra-Preconcentration and
DOI: 10.1080/03650341003787582. Determination of Organophosphorus Pesticides in Soil
[2] Kim, K.-H.; Kabir, E.; Jahan, S. A. Exposure to Pesticides and Samples by a Combination of Ultrasound Assisted Leaching-
the Associated Human Health Effects. Sci. Total Environ. Solid Phase Extraction and Low-Density Solvent Based
2017, 575, 525–535. DOI: 10.1016/j.scitotenv.2016.09.009. Dispersive Liquid–Liquid Microextraction. RSC Adv. 2015, 5,
[3] Buerge, I. J.; B€achli, A.; Kasteel, R.; Portmann, R.; Lopez- 75174–75181. DOI: 10.1039/C5RA11959F.
Cabeza, R.; Schwab, L. F.; Poiger, T. Behavior of the Chiral [17] Bidari, A.; Ganjali, M. R.; Norouzi, P.; Hosseini, M. R. M.;
Herbicide Imazamox in Soils: pH-Dependent, Enantioselective Assadi, Y. Sample Preparation Method for the Analysis of
Degradation, Formation and Degradation of Several Chiral Some Organophosphorus Pesticides Residues in Tomato by
Metabolites. Environ. Sci. Technol. 2019, 53, 5725–5732. DOI: Ultrasound-Assisted Solvent Extraction Followed by Dispersive
10.1021/acs.est.8b07209. Liquid-Liquid Microextraction. Food Chem. 2011, 126,
[4] Xie, J.; Zhao, L.; Liu, K.; Guo, F.; Gao, L.; Liu, W. Activity, 1840–1844. DOI: 10.1016/j.foodchem.2010.11.142.
Toxicity, Molecular Docking, and Environmental Effects of [18] Samsidar, A.; Siddiquee, S.; Shaarani, S. M. A Review of
Three Imidazolinone Herbicides Enantiomers. Sci. Total Extraction, Analytical and Advanced Methods for
Environ. 2018, 622-623, 594–602. DOI: 10.1016/j.scitotenv. Determination of Pesticides in Environment and Foodstuffs.
2017.11.333. Trends Food Sci. Technol. 2018, 71, 188–201. DOI: 10.1016/j.
[5] Rani, M.; Shanker, U.; Jassal, V. Recent Strategies for Removal tifs.2017.11.011.
and Degradation of Persistent & Toxic Organochlorine [19] Ware, G. W.; Whitacre, D. M. An Introduction to Insecticides.
Pesticides Using Nanoparticles: A Review. J. Environ. Manage. In The Pesticide Book, 6 th ed. Published by InTech 2012.
2017, 190, 208–222. DOI: 10.1016/j.jenvman.2016.12.068. ISBN: 978-953-51-0007-2.
[6] Birolli, W. G.; Arai, M. S.; Nitschke, M.; Porto, A. L. The [20] Verma, N.; Bhardwaj, A. Biosensor Technology for Pesticides -
Pyrethroid (±)-Lambda-Cyhalothrin Enantioselective A Review. Appl. Biochem. Biotechnol. 2015, 175, 3093–3119.
Biodegradation by a Bacterial Consortium. Pestic. Biochem. DOI: 10.1007/s12010-015-1489-2.

[21] Bunch, M. J.; Suresh, V. M.; Kumaran, T. V. S. Environment
and health aspects of pesticides use in Indian agriculture.
International Conference on Environment and Health.
Citeseer; 2003, p. 17.
[22] Helou, K.; Harmouche-Karaki, M.; Karake, S.; Narbonne, J.-F.
A Review of Organochlorine Pesticides and Polychlorinated
Biphenyls in Lebanon: Environmental and Human
Contaminants. Chemosphere 2019, 231, 357–368. DOI: 10.
1016/j.chemosphere.2019.05.109.
[23] Thomas, K. V.; Bijlsma, L.; Castiglioni, S.; Covaci, A.; Emke,
E.; Grabic, R.; Hernandez, F.; Karolak, S.; Kasprzyk-Hordern,
B.; Lindberg, R. H.; et al. Comparing Illicit Drug Use in 19
European Cities through Sewage Analysis. Sci. Total Environ.
2012, 432, 432–439. DOI: 10.1016/j.scitotenv.2012.06.069.
[24] Parada, H., Jr; Wolff, M. S.; Engel, L. S.; White, A. J.; Eng,
S. M.; Cleveland, R. J.; Khankari, N. K.; Teitelbaum, S. L.;
Neugut, A. I.; Gammon, M. D. Organochlorine Insecticides
DDT and Chlordane in Relation to Survival following Breast
Cancer. Int. J. Cancer. 2016, 138, 565–575. DOI: 10.1002/ijc.
29806.
[25] McGlynn, K. A.; Abnet, C. C.; Zhang, M.; Sun, X.-D.; Fan, J.-
H.; O’Brien, T. R.; Wei, W.-Q.; Ortiz-Conde, B. A.; Dawsey,
S. M.; Weber, J.-P.; et al. Serum Concentrations of 1,1,1-
Trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) and 1,1-
Dichloro-2,2-bis(p-chlorophenyl)ethylene (DDE) and Risk of
Primary Liver Cancer. J. Natl. Cancer Inst. 2006, 98,
1005–1010., DOI: 10.1093/jnci/djj266.
[26] Li, J.; Jiang, S.; Chang, Y.; Guo, Z.; Yao, S.; Yuan, J.; Li, G.
Association among Serum Organochlorine Pesticide Residues,
Glutathione S-Transferase M1 Genetic Polymorphism and
Female Breast Cancer. Scientific Research 2013, 5. DOI:10.
4236/abcr.2013.22005.
[27] Sharma, T.; Banerjee, B. D.; Mazumdar, D.; Tyagi, V.; Thakur,
G.; Guleria, K.; Ahmed, R. S.; Tripathi, A. K. Association of
Organochlorine Pesticides and Risk of Epithelial Ovarian
Cancer: A Case Control Study. J. Reprod. Health Med. 2015, 1,
76–82. DOI: 10.1016/j.jrhm.2015.01.006.
 G. P.; L  D.; Le
[28] Rodrıguez, A. opez, M. I. R.; Casillas, T. A. on,
J. A. A.; Mahjoub, O.; Prusty, A. K. Monitoring of
Organochlorine Pesticides in Blood of Women with Uterine
Cervix Cancer. Environ. Pollut. 2017, 220, 853–862. DOI: 10.
1016/j.envpol.2016.10.068.
[29] Boada, L.; Henrıquez-Hernandez, L.; Zumbado, M.; Almeida-
Gonzalez, M.; Alvarez-Leon, E.; Navarro, P.; Luzardo, O.
Organochlorine Pesticides Exposure and Bladder Cancer:
Evaluation from a Gene-Environment Perspective in a
Hospital-Based Case-Control Study in the Canary Islands
(Spain). J. Agromed. 2016, 21, 34–42. DOI: 10.1080/1059924X.
2015.1106374.
[30] Yang, J.-Z.; Wang, Z.-X.; Ma, L.-H.; Shen, X.-B.; Sun, Y.; Hu,
D.-W.; Sun, L.-X. The Organochlorine Pesticides Residues in
the Invasive Ductal Breast Cancer Patients. Environ. Toxicol.
Pharmacol. 2015, 40, 698–703. DOI: 10.1016/j.etap.2015.07.
007.
[31] Xiang, D.; Zhong, L.; Shen, S.; Song, Z.; Zhu, G.; Wang, M.;
Wang, Q.; Zhou, B. Chronic Exposure to Environmental
Levels of Cis-Bifenthrin: Enantioselectivity and Reproductive
Effects on Zebrafish (Danio rerio). Environ. Pollut. 2019, 251,
175–184. DOI: 10.1016/j.envpol.2019.04.089.
[32] Yue, M.-E.; Lin, Q.; Xu, J.; Jiang, T.-F. Headspace in-Tube
Microextraction Combined with Reverse-Flow Micellar
Electrokinetic Capillary Chromatography for Detection of
Pyrethroid Herbicides in Fruits. Acta Chromatogr. 2019, 31,
189–193. DOI: 10.1556/1326.2018.00436.
[33] Kim, S.-A.; Kim, K.-S.; Lee, Y.-M.; Jacobs, D. R.; Lee, D.-H.
Associations of Organochlorine Pesticides and Polychlorinated
Biphenyls with Total, Cardiovascular, and Cancer Mortality in
Elders with Differing Fat Mass. Environ. Res. 2015, 138, 1–7.
DOI: 10.1016/j.envres.2015.01.021.
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 17
[34] Medehouenou, T. C. M.; Ayotte, P.; Carmichael, P.-H.;
Kr€  Tyas, S. L.;
oger, E.; Verreault, R.; Lindsay, J.; Dewailly, E.;
Bureau, A.; Laurin, D. Plasma Polychlorinated Biphenyl and
Organochlorine Pesticide Concentrations in Dementia: The
Canadian Study of Health and Aging. Environ. Int. 2014, 69,
141–147. DOI: 10.1016/j.envint.2014.04.016.
[35] Ornoy, A.; Weinstein-Fudim, L.; Ergaz, Z. Prenatal Factors
Associated with Autism Spectrum Disorder (ASD). Reprod.
Toxicol. 2015, 56, 155–169. DOI: 10.1016/j.reprotox.2015.05.
007.
[36] Carr~ao, D. B.; dos Reis Gomes, I. C.; Junior, F. B.; de Oliveira,
A. R. M. Evaluation of the Enantioselective in Vitro
Metabolism of the Chiral Pesticide Fipronil Employing a
Human Model: Risk Assessment through in Vitro-in Vivo
Correlation and Prediction of Toxicokinetic Parameters. Food
Chem. Toxicol. 2019, 123, 225–232. DOI: 10.1016/j.fct.2018.10.
060.
[37] Habenschus, M. D.; Nardini, V.; Dias, L. G.; Rocha, B. A.;
Barbosa, F.; Jr.; de Oliveira, A. R. M. In Vitro Enantioselective
Study of the Toxicokinetic Effects of Chiral Fungicide
Tebuconazole in Human Liver Microsomes. Ecotoxicol.
Environ. Saf. 2019, 181, 96–105. DOI: 10.1016/j.ecoenv.2019.
05.071.
[38] Qian, Y.; Ji, C.; Yue, S.; Zhao, M. Exposure of Low-Dose
Fipronil Enantioselectively Induced Anxiety-like Behavior
Associated with DNA Methylation Changes in Embryonic and
Larval Zebrafish. Environ. Pollut. 2019, 249, 362–371. DOI: 10.
1016/j.envpol.2019.03.038.
[39] Xu, X.; Xu, X.; Han, M.; Qiu, S.; Hou, X. Development of a
Modified QuEChERS Method Based on Magnetic Multiwalled
Carbon Nanotubes for the Simultaneous Determination of
Veterinary Drugs, Pesticides and Mycotoxins in Eggs by
UPLC-MS/MS. Food Chem. 2019, 276, 419–426. DOI: 10.1016/
j.foodchem.2018.10.051.
[40] Xu, C.; Sun, X.; Niu, L.; Yang, W.; Tu, W.; Lu, L.; Song, S.;
Liu, W. Enantioselective Thyroid Disruption in Zebrafish
Embryo-Larvae via Exposure to Environmental Concentrations
of the Chloroacetamide Herbicide Acetochlor. Sci. Total
Environ. 2019, 653, 1140–1148. DOI: 10.1016/j.scitotenv.2018.
11.037.
[41] Zhang, X.; Wang, X.; Luo, F.; Sheng, H.; Zhou, L.; Zhong, Q.;
Lou, Z.; Sun, H.; Yang, M.; Cui, X.; Chen, Z. Application and
Enantioselective Residue Determination of Chiral Pesticide
Penconazole in Grape, Tea, Aquatic Vegetables and Soil by
Ultra Performance Liquid Chromatography-Tandem Mass
Spectrometry. Ecotoxicol. Environ. Saf. 2019, 172, 530–537.
DOI: 10.1016/j.ecoenv.2019.01.103.
[42] Tankiewicz, M.; Fenik, J.; Biziuk, M. Determination of
Organophosphorus and Organonitrogen Pesticides in Water
Samples. TrAC Trends Anal. Chem. 2010, 29, 1050–1063. DOI:
10.1016/j.trac.2010.05.008.
[43] Zhao, E.; Han, L.; Jiang, S.; Wang, Q.; Zhou, Z. Application of
a Single-Drop Microextraction for the Analysis of
Organophosphorus Pesticides in Juice. J. Chromatogr. A. 2006,
1114, 269–273. DOI: 10.1016/j.chroma.2006.03.011.
[44] Abbas, M. S.; Soliman, A. S.; El-Gammal, H. A.; Amer, M. E.;
Attallah, E. R. Development and Validation of a Multiresidue
Method for the Determination of 323 Pesticide Residues in
Dry Herbs Using QuEChERS Method and LC-ESI-MS/MS.
Int. J. Environ. Anal. Chem. 2017, 97, 1003–1023. DOI: 10.
1080/03067319.2017.1381954.
[45] Kim, Y.-A.; Abd El-Aty, A.; Rahman, M. M.; Jeong, J. H.;
Shin, H.-C.; Wang, J.; Shin, S.; Shim, J.-H. Method
Development, Matrix Effect, and Risk Assessment of 49
Multiclass Pesticides in Kiwifruit Using Liquid
Chromatography Coupled to Tandem Mass Spectrometry. J.
Chromatogr. B. 2018, 1076, 130–138. DOI: 10.1016/j.jchromb.
2018.01.015.
[46] Rong, L.; Wu, X.; Xu, J.; Dong, F.; Liu, X.; Pan, X.; Du, P.;
Wei, D.; Zheng, Y. Simultaneous Determination of Three
18 M. S. JAGIRANI ET AL.
Pesticides and Their Metabolites in Unprocessed Foods Using
Ultraperformance Liquid Chromatography-Tandem Mass
Spectrometry. Food Addit. Contam. Part A Chem. Anal.
Control Expo. Risk. Assess. 2018, 35, 273–281. DOI: 10.1080/
19440049.2017.1398419.
[47] Lu, M.; Ding, C.-C. Determination of Acetamide-Group
Herbicides by High Performance Liquid Chromatography.
Admin. Tech. Environ. Monitor. 2007, 3. 3.
[48] Buerge, I. J.; Krauss, J.; L
opez-Cabeza, R.; Siegfried, W.; St€
ussi,
M.; Wettstein, F. E.; Poiger, T. Stereoselective Metabolism of
the Sterol Biosynthesis Inhibitor Fungicides Fenpropidin,
Fenpropimorph, and Spiroxamine in Grapes, Sugar Beets, and
Wheat. J. Agric. Food Chem. 2016, 64, 5301–5309. DOI: 10.
1021/acs.jafc.6b00919.
[49] Dallegrave, A.; Pizzolato, T. M.; Barreto, F.; Eljarrat, E.;
Barcelo, D. Methodology for Trace Analysis of 17 Pyrethroids
and Chlorpyrifos in Foodstuff by Gas Chromatography-
Tandem Mass Spectrometry. Anal. Bioanal. Chem. 2016, 408,
7689–7697. DOI: 10.1007/s00216-016-9865-5.
[50] He, R.; Fan, J.; Tan, Q.; Lai, Y.; Chen, X.; Wang, T.; Jiang, Y.;
Zhang, Y.; Zhang, W. Enantioselective Determination of
Metconazole in Multi Matrices by High-Performance Liquid
Chromatography. Talanta 2018, 178, 980–986. DOI: 10.1016/j.
talanta.2017.09.045.
[51] Wang, J.; Duan, H.-L.; Ma, S.-Y.; Zhang, J.; Zhang, Z.-Q.
Solidification of a Switchable Solvent-Based QuEChERS
Method for Detection of 16 Pesticides in Some Fruits and
Vegetables. J. Agric. Food Chem. 2019, 67, 8045–8052. DOI:
10.1021/acs.jafc.9b00686.
[52] Zhang, P.; Yu, Q.; He, X.; Qian, K.; Xiao, W.; Xu, Z.; Li, T.;
He, L. Enantiomeric Separation of Type I and Type II
Pyrethroid Insecticides with Different Chiral Stationary Phases
by Reversed-Phase High-Performance Liquid Chromatography.
Chirality 2018, 30, 420–431. DOI: 10.1002/chir.22801.
[53] Cao, X.; Hogan, A.; Moore, E. Rapid Separation of
Organophosphate Pesticides Using Micellar Electrokinetic
Chromatography and Short-end Injection. J. Forensic. Sci.
2019, 64, 1213–1220. DOI: 10.1111/1556-4029.13963.
[54]  Menendez-Lopez, N.; Boltes, K.; Castro-Puyana,
Garcıa, M. A.;
M.; Marina, M. L. A Capillary Micellar Electrokinetic
Chromatography Method for the Stereoselective Quantitation
of Bioallethrin in Biotic and Abiotic Samples. J. Chromatogr.
A. 2017, 1510, 108–116. DOI: 10.1016/j.chroma.2017.06.056.
[55] Yang, Q.; Chen, B.; He, M.; Hu, B. Sensitive Determination of
Seven Triazine Herbicide in Honey, Tomato and
Environmental Water Samples by Hollow Fiber Based Liquid-
Liquid-Liquid Microextraction Combined with Sweeping
Micellar Electrokinetic Capillary Chromatography. Talanta
2018, 186, 88–96. DOI: 10.1016/j.talanta.2018.04.012.
[56] Cheng, Y.; Zheng, Y.; Dong, F.; Li, J.; Zhang, Y.; Sun, S.; Li,
N.; Cui, X.; Wang, Y.; Pan, X.; Zhang, W. Stereoselective
Analysis and Dissipation of Propiconazole in Wheat, Grapes,
and Soil by Supercritical Fluid Chromatography-Tandem Mass
Spectrometry. J. Agric. Food Chem. 2017, 65, 234–243. DOI:
10.1021/acs.jafc.6b04623.
[57] Jiang, Y.; Fan, J.; He, R.; Guo, D.; Wang, T.; Zhang, H.;
Zhang, W. High-Fast Enantioselective Determination of
Prothioconazole in Different Matrices by Supercritical Fluid
Chromatography and Vibrational Circular Dichroism
Spectroscopic Study. Talanta 2018, 187, 40–46. DOI: 10.1016/
j.talanta.2018.04.097.
[58] Tan, Q.; Fan, J.; Gao, R.; He, R.; Wang, T.; Zhang, Y.; Zhang,
W. Stereoselective Quantification of Triticonazole in
Vegetables by Supercritical Fluid Chromatography. Talanta
2017, 164, 362–367. DOI: 10.1016/j.talanta.2016.08.077.
[59] Tao, Y.; Zheng, Z.; Yu, Y.; Xu, J.; Liu, X.; Wu, X.; Dong, F.;
Zheng, Y. Supercritical Fluid Chromatography-Tandem Mass
Spectrometry-Assisted Methodology for Rapid Enantiomeric
Analysis of Fenbuconazole and Its Chiral Metabolites in
Fruits, Vegetables, Cereals, and Soil. Food Chem. 2018, 241,
32–39. DOI: 10.1016/j.foodchem.2017.08.038.
[60] Johnson, W. E.; Fendinger, N. J.; Plimmer, J. R. Solid-Phase
Extraction of Pesticides from Water: Possible Interferences
from Dissolved Organic Material. Anal. Chem. 1991, 63,
1510–1513. DOI: 10.1021/ac00015a003.
[61] Wang, H.; Yuan, X.; Wu, Y.; Chen, X.; Leng, L.; Wang, H.; Li,
H.; Zeng, G. Facile Synthesis of Polypyrrole Decorated
Reduced Graphene Oxide–Fe3O4 Magnetic Composites and
Its Application for the Cr (VI) Removal. Chem. Eng. J. 2015,
262, 597–606. DOI: 10.1016/j.cej.2014.10.020.
[62] Xu, X.; Yang, H.; Wang, L.; Han, B.; Wang, X.; Lee, F. S.-C.
Analysis of Chloroacetanilide Herbicides in Water Samples by
Solid-Phase Microextraction Coupled with Gas
Chromatography-Mass Spectrometry. Anal. Chim. Acta. 2007,
591, 87–96. DOI: 10.1016/j.aca.2007.03.044.
[63] Heidari, H.; Razmi, H. Multi-Response Optimization of
Magnetic Solid Phase Extraction Based on Carbon Coated
Fe3O4 Nanoparticles Using Desirability Function Approach
for the Determination of the Organophosphorus Pesticides in
Aquatic Samples by HPLC-UV. Talanta 2012, 99, 13–21. DOI:
10.1016/j.talanta.2012.04.023.
[64] Amiri, A.; Baghayeri, M.; Vahdati-Nasab, N. Effective
Extraction of Organophosphorus Pesticides Using Sol–Gel
Based Coated Stainless Steel Mesh as Novel Solid-Phase
Extraction Sorbent. J. Chromatogr. A. 2020, 1620, 461020.
DOI: 10.1016/j.chroma.2020.461020.
[65] Kunene, P.; Mahlambi, P. Optimization and Application of
Ultrasonic Extraction and Soxhlet Extraction Followed by
Solid Phase Extraction for the Determination of Triazine
Pesticides in Soil and Sediment. J. Environ. Chem. Eng. 2020,
8, 103665. DOI: 10.1016/j.jece.2020.103665.
[66] €
Ozer, E. T.; Osman, B.; Parlak, B. An Experimental Design
Approach for the Solid Phase Extraction of Some
Organophosphorus Pesticides from Water Samples with
Polymeric Microbeads. Microchem. J. 2020, 154, 104537. DOI:
10.1016/j.microc.2019.104537.
[67] Zhao, J.; Meng, Z.; Zhao, Z.; Zhao, L. Ultrasound-Assisted
Deep Eutectic Solvent as Green and Efficient Media Combined
with Functionalized Magnetic Multi-Walled Carbon
Nanotubes as Solid-Phase Extraction to Determine Pesticide
Residues in Food Products. Food Chem. 2020, 310, 125863.
DOI: 10.1016/j.foodchem.2019.125863.
[68] Soylak, M.; Ozalp, O.; Uzcan, F. Magnetic Nanomaterials for
the Removal, Separation and Preconcentration of Organic and
Inorganic Pollutants at Trace Levels and Their Practical
Applications: A Review. Trends Environ. Anal. Chem. 2021,
29, e00109. DOI: 10.1016/j.teac.2020.e00109.
[69] Soylak, M.; Agirbas, M.; Yilmaz, E. A New Strategy for the
Combination of Supramolecular Liquid Phase Microextraction
and UV-Vis Spectrophotometric Determination for Traces of
Maneb in Food and Water Samples. Food Chem. 2021, 338,
128068 DOI: 10.1016/j.foodchem.2020.128068.
[70] Habila, M.; Alhenaki, B.; El-Marghany, A.; Sheikh, M.; Ghfar,
A.; ALOthman, Z.; Soylak, M. Metal Organic Frameworks
Enhanced Dispersive Solid Phase Microextraction of
Malathion before Detection by Ultra-Performance Liquid
Chromatography-Tandem Mass Spectrometry. J. Sep. Sci.
2020, 43, 3103–3109. DOI: 10.1002/jssc.202000033.
[71] Soylak, M.; Gorucu, H. H.; Yilmaz, E. Micelle-Based Restricted
Access Ion-Pair Microextraction of Phosphate at Trace Levels
in Water Samples for Separation, Preconcentration and
Determination. EuroBiotech J. 2020, 4, 89–96. DOI: 10.2478/
ebtj-2020-0010.
[72] ALOthman, Z. A.; Yilmaz, E.; Habila, M.; Ghfar, A. A.;
Alhenaki, B.; Soylak, M.; Ahmed, A.; Hadj, B. Supramolecular
Solvent Microextraction and Ultra-Performance Liquid
Chromatography-Tandem Mass Spectrometry Combination
for the Preconcentration and Determination of Malathion in

Environmental Samples. Desalin. Water Treat. 2019, 144,
166–171. DOI: 10.5004/dwt.2019.23574.
[73] Tahboub, Y. R.; Zaater, M. F.; Al-Talla, Z. A. Determination
of the Limits of Identification and Quantitation of Selected
Organochlorine and Organophosphorous Pesticide Residues in
Surface Water by Full-Scan Gas Chromatography/Mass
Spectrometry. J. Chromatogr. A. 2005, 1098, 150–155. DOI:
10.1016/j.chroma.2005.08.064.
[74] Sankararamakrishnan, N.; Sharma, A. K.; Sanghi, R.
Organochlorine and Organophosphorous Pesticide Residues in
Ground Water and Surface Waters of Kanpur, Uttar Pradesh,
India. Environ. Int. 2005, 31, 113–120. DOI: 10.1016/j.envint.
2004.08.001.
[75] Pirard, C.; Widart, J.; Nguyen, B. K.; Deleuze, C.; Heudt, L.;
Haubruge, E.; De Pauw, E.; Focant, J.-F. Development and
Validation of a Multi-Residue Method for Pesticide
Determination in Honey Using On-Column Liquid-Liquid
Extraction and Liquid Chromatography-Tandem Mass
Spectrometry. J. Chromatogr. A. 2007, 1152, 116–123. DOI:
10.1016/j.chroma.2007.03.035.
[76] Tse, H.; Comba, M.; Alaee, M. Method for the Determination
of Organophosphate Insecticides in Water, Sediment and
Biota. Chemosphere 2004, 54, 41–47. DOI: 10.1016/S0045-
6535(03)00659-3.
[77] Sabik, H.; Jeannot, R. Determination of Organonitrogen
Pesticides in Large Volumes of Surface Water by
Liquid–Liquid and Solid-Phase Extraction Using Gas
Chromatography with Nitrogen–Phosphorus Detection and
Liquid Chromatography with Atmospheric Pressure Chemical
Ionization Mass Spectrometry. J. Chromatogr. A. 1998, 818,
197–207. DOI: 10.1016/S0021-9673(98)00555-X.
[78] Fatoki, O.; Awofolu, R. Methods for Selective Determination
of Persistent Organochlorine Pesticide Residues in Water and
Sediments by Capillary Gas Chromatography and Electron-
Capture Detection. J. Chromatogr. A. 2003, 983, 225–236.
DOI: 10.1016/S0021-9673(02)01730-2.
[79] Mahara, B. M.; Borossay, J.; Torkos, K. Liquid–Liquid
Extraction for Sample Preparation Prior to Gas
Chromatography and Gas Chromatography–Mass
Spectrometry Determination of Herbicide and Pesticide
Compounds. Microchem. J. 1998, 58, 31–38. DOI: 10.1006/
mchj.1997.1517.
[80] Lopez-Blanco, M.; Blanco-Cid, S.; Cancho-Grande, B.; Simal-
Gandara, J. Application of Single-Drop Microextraction and
Comparison with Solid-Phase Microextraction and Solid-Phase
Extraction for the Determination of a-and b-Endosulfan in
Water Samples by Gas Chromatography–Electron-Capture
Detection. J. Chromatogr. A. 2003, 984, 245–252. DOI: 10.
1016/S0021-9673(02)01873-3.
[81] Albero, B.; Sanchez-Brunete, C.; Tadeo, J. L. Multiresidue
Determination of Pesticides in Juice by Solid-Phase Extraction
and Gas Chromatography-Mass Spectrometry. Talanta 2005,
66, 917–924. DOI: 10.1016/j.talanta.2004.12.046.
[82] Navarro, S.; Barba, A.; Navarro, G.; Vela, N.; Oliva, J.
Multiresidue Method for the Rapid Determination–in Grape,
Must and Wine–of Fungicides Frequently Used on Vineyards.
J. Chromatogr. A. 2000, 882, 221–229. DOI: 10.1016/S0021-
9673(00)00337-X.
[83] Torres, C.; Pico, Y.; Manes, J. Determination of Pesticide
Residues in Fruit and Vegetables. J. Chromatogr. A. 1996, 754,
301–331. DOI: 10.1016/S0021-9673(96)00407-4.
[84] Anastassiades, M.; Lehotay, S. J.; Stajnbaher, D.; Schenck, F. J.
Fast and Easy Multiresidue Method Employing Acetonitrile
Extraction/Partitioning and “Dispersive Solid-Phase
Extraction” for the Determination of Pesticide Residues in
Produce. J. AOAC Int. 2003, 86, 412–431. DOI: 10.1093/jaoac/
86.2.412.
[85] Walorczyk, S.; Gnusowski, B. Development and Validation of
a Multi-Residue Method for the Determination of Pesticides in
Honeybees Using Acetonitrile-Based Extraction and Gas
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 19
Chromatography–Tandem Quadrupole Mass Spectrometry. J.
Chromatogr. A. 2009, 1216, 6522–6531. DOI: 10.1016/j.
chroma.2009.07.045.
[86] Kin, C. M.; Huat, T. G. Headspace Solid-Phase
Microextraction for the Evaluation of Pesticide Residue
Contents in Cucumber and Strawberry after Washing
Treatment. Food Chem. 2010, 123, 760–764.
[87] Armenta, S.; Garrigues, S.; De la Guardia, M. Green Analytical
Chemistry. TrAC Trends Anal. Chem. 2008, 27, 497–511. DOI:
10.1016/j.trac.2008.05.003.
[88] Greulich, K.; Alder, L. Fast Multiresidue Screening of 300
Pesticides in Water for Human Consumption by LC-MS/MS.
Anal. Bioanal. Chem. 2008, 391, 183–197. DOI: 10.1007/
s00216-008-1935-x.
[89] Escuderos-Morenas, M.; Santos-Delgado, M.; Rubio-Barroso,
S.; Polo-Dı ez, L. Direct Determination of Monolinuron,
Linuron and Chlorbromuron Residues in Potato Samples by
Gas Chromatography with Nitrogen–Phosphorus Detection. J.
Chromatogr. A. 2003, 1011, 143–153. DOI: 10.1016/S0021-
9673(03)01139-7.
[90] Molina-Dıaz, A.; Garcıa-Reyes, J. F.; Gilbert-Lopez, B. Solid-
Phase Spectroscopy from the Point of View of Green
Analytical Chemistry. TrAC Trends Anal. Chem. 2010, 29,
654–666. DOI: 10.1016/j.trac.2010.03.010.
[91] Kurowska-Susdorf, A.; Zwier_zd_zy nski, M.; Bevanda, A. M.;
Talic, S.; Ivankovic, A.; Płotka-Wasylka, J. Green Analytical
Chemistry: Social Dimension and Teaching. TrAC Trends
Anal. Chem. 2019, 111, 185–196. DOI: 10.1016/j.trac.2018.10.
022.
[92] Tobiszewski, M.; Mechli nska, A.; Zygmunt, B.; Namiesnik, J.
Green Analytical Chemistry in Sample Preparation for
Determination of Trace Organic Pollutants. TrAC Trends
Anal. Chem. 2009, 28, 943–951. DOI: 10.1016/j.trac.2009.06.
001.
[93] Zuin, V. G.; Segatto, M. L.; Zandonai, D. P.; Grosseli, G. M.;
Stahl, A.; Zanotti, K.; Andrade, R. S. Integrating Green and
Sustainable Chemistry into Undergraduate Teaching
Laboratories: Closing and Assessing the Loop on the Basis of a
Citrus Biorefinery Approach for the Biocircular Economy in
Brazil. J. Chem. Educ. 2019, 96, 2975–2983. DOI: 10.1021/acs.
jchemed.9b00286.
[94] Castro, J. R.; Garcıa-Hernandez, L.; Ortega, P. A. R.; Islas,
D. A. Green Synthesis of Gold Nanoparticles (AuNPs) by
Cupressus Goveniana Extract. ECS Trans. 2018, 84, 207–215.
DOI: 10.1149/08401.0207ecst.
[95] Quintana, J. B.; Rodrıguez, I. Strategies for the
Microextraction of Polar Organic Contaminants in Water
Samples. Anal. Bioanal. Chem. 2006, 384, 1447–1461. DOI: 10.
1007/s00216-005-0242-z.
[96] Kokosa, J. M. Advances in Solvent-Microextraction
Techniques. TrAC Trends Anal. Chem. 2013, 43, 2–13. DOI:
10.1016/j.trac.2012.09.020.
[97] Arthur, C. L.; Pawliszyn, J. Solid Phase Microextraction with
Thermal Desorption Using Fused Silica Optical Fibers. Anal.
Chem. 1990, 62, 2145–2148. DOI: 10.1021/ac00218a019.
[98] Gionfriddo, E.; Souza-Silva, E. A.; Ho, T. D.; Anderson, J. L.;
Pawliszyn, J. Exploiting the Tunable Selectivity Features of
Polymeric Ionic Liquid-Based SPME Sorbents in Food
Analysis. Talanta 2018, 188, 522–530. DOI: 10.1016/j.talanta.
2018.06.011.
[99] Pang, L.; Yang, P.; Pang, R.; Yuan, Y.; Ge, L.; Zhang, H.
Polymeric Ionic Liquid Based Fused Silica Fiber by Chemical
Binding for Headspace Solid-Phase Microextraction of
Organophosphate Esters in Water Samples. Int. J. Environ.
Anal. Chem. 2017, 97, 1094–1106. DOI: 10.1080/03067319.
2017.1381955.
[100] Sapahin, H. A.; Makahleh, A.; Saad, B. Determination of
Organophosphorus Pesticide Residues in Vegetables Using
Solid Phase Micro-Extraction Coupled with Gas
20 M. S. JAGIRANI ET AL.
Chromatography–Flame Photometric Detector. Arabian J.
Chem. 2019, 12, 1934–1944. DOI: 10.1016/j.arabjc.2014.12.001.
[101] Wu, M.; Chen, G.; Liu, P.; Zhou, W.; Jia, Q. Polydopamine-
Based Immobilization of a Hydrazone Covalent Organic
Framework for Headspace Solid-Phase Microextraction of
Pyrethroids in Vegetables and Fruits. J. Chromatogr. A. 2016,
1456, 34–41. DOI: 10.1016/j.chroma.2016.05.100.
[102] Habila, M. A.; ALOthman, Z. A.; Al-Tamrah, S. A.; Ghafar,
A. A.; Soylak, M. Activated Carbon from Waste as an Efficient
Adsorbent for Malathion for Detection and Removal Purposes.
J. Ind. Eng. Chem. 2015, 32, 336–344. DOI: 10.1016/j.jiec.2015.
09.009.
[103] Shahid, R.; Kazi, T. G.; Afridi, H. I.; Talpur, F. N.; Akhtar, A.;
Baig, J. A. Deep-Eutectic-Solvent-Based Dispersive and
Emulsification Liquid-Liquid Microextraction Methods for the
Speciation of Selenium in Water and Determining Its Total
Content Levels in Milk Formula and Cereals. Anal. Methods
2020, 12, 5186–5194. DOI: 10.1039/d0ay01517b.
[104] Liu, H.; Dasgupta, P. K. Analytical Chemistry in a Drop.
Solvent Extraction in a Microdrop. Anal. Chem. 1996, 68,
1817–1821. DOI: 10.1021/ac960145h.
[105] Jeannot, M. A.; Przyjazny, A.; Kokosa, J. M. Single Drop
Microextraction-Development, Applications and Future
Trends. J. Chromatogr. A. 2010, 1217, 2326–2336. DOI: 10.
1016/j.chroma.2009.10.089.
[106] Kokosa, J. M. Recent Trends in Using Single-Drop
Microextraction and Related Techniques in Green Analytical
Methods. TrAC Trends Anal. Chem. 2015, 71, 194–204. DOI:
10.1016/j.trac.2015.04.019.
[107] Xu, L.; Basheer, C.; Lee, H. K. Developments in Single-Drop
Microextraction. J. Chromatogr. A. 2007, 1152, 184–192. DOI:
10.1016/j.chroma.2006.10.073.
[108] Deng, W.; Yu, L.; Li, X.; Chen, J.; Wang, X.; Deng, Z.; Xiao,
Y. Hexafluoroisopropanol-Based Hydrophobic Deep Eutectic
Solvents for Dispersive Liquid-Liquid Microextraction of
Pyrethroids in Tea Beverages and Fruit Juices. Food Chem.
2019, 274, 891–899. DOI: 10.1016/j.foodchem.2018.09.048.
[109] Farajzadeh, M. A.; Abbaspour, M.; Kazemian, R.; Afshar
Mogaddam, M. R. Preparation of a New Three-Component
Deep Eutectic Solvent and Its Use as an Extraction Solvent in
Dispersive Liquid-Liquid Microextraction of Pesticides in
Green Tea and Herbal Distillates. J. Sci. Food. Agric. 2020,
100, 1904–1912. DOI: 10.1002/jsfa.10200.
[110] Liu, W.; Quan, J. A Novel Ionic Liquid of [BeMIM][Tf 2 N]
for Extracting Pesticides Residues in Tea Sample by Dispersive
Liquid–Liquid Microextraction. Chromatographia 2020, 83,
41–51. DOI: 10.1007/s10337-019-03819-5.
[111] Mokhtari, N.; Torbati, M.; Farajzadeh, M. A.; Afshar
Mogaddam, M. R. Synthesis and Characterization of
Phosphocholine Chloride-Based Three-Component Deep
Eutectic Solvent: Application in Dispersive Liquid-Liquid
Microextraction for Determination of Organothiophosphate
Pesticides. J. Sci. Food Agric. 2020, 100, 2364–2371. DOI: 10.
1002/jsfa.10203.
[112] Bedendo, G. C.; Jardim, I. C. S. F.; Carasek, E. Multiresidue
Determination of Pesticides in Industrial and Fresh Orange
Juice by Hollow Fiber Microporous Membrane Liquid-Liquid
Extraction and Detection by Liquid Chromatography-
Electrospray-Tandem Mass Spectrometry. Talanta 2012, 88,
573–580. DOI: 10.1016/j.talanta.2011.11.037.
[113] Ma, X.; Wang, J.; Wu, Q.; Wang, C.; Wang, Z. Extraction of
Carbamate Pesticides in Fruit Samples by Graphene
Reinforced Hollow Fibre Liquid Microextraction Followed by
High Performance Liquid Chromatographic Detection. Food
Chem. 2014, 157, 119–124. DOI: 10.1016/j.foodchem.2014.02.
007.
[114] Ridgway, K.; Lalljie, S. P.; Smith, R. M. Sample Preparation
Techniques for the Determination of Trace Residues and
Contaminants in Foods. J. Chromatogr. A. 2007, 1153, 36–53.
DOI: 10.1016/j.chroma.2007.01.134.
[115] David, F.; Sandra, P. Stir Bar Sorptive Extraction for Trace
Analysis. J. Chromatogr. A. 2007, 1152, 54–69. DOI: 10.1016/j.
chroma.2007.01.032.
[116] Giordano, A.; Fernandez-Franz on, M.; Ruiz, M.; Font, G.;
Pico, Y. Pesticide Residue Determination in Surface Waters by
Stir Bar Sorptive Extraction and Liquid Chromatography/
Tandem Mass Spectrometry. Anal. Bioanal. Chem. 2009, 393,
1733–1743. DOI: 10.1007/s00216-009-2627-x.
[117] Murtada, K. Trends in Nanomaterial-Based Solid-Phase
Microextraction with a Focus on Environmental Applications-
A Review. Trends Environ. Anal. Chem. 2020, 25, e00077.
DOI: 10.1016/j.teac.2019.e00077.
[118] Płotka-Wasylka, J.; Owczarek, K.; Namiesnik, J. Modern
Solutions in the Field of Microextraction Using Liquid as a
Medium of Extraction. TrAC - Trends Anal. Chem. 2016, 85,
46–64. DOI: 10.1016/j.trac.2016.08.010.
[119] Rutkowska, M.; Płotka-Wasylka, J.; Sajid, M.; Andruch, V.
Liquid–Phase Microextraction: A Review of Reviews.
Microchem. J. 2019, 149, 103989. DOI: 10.1016/j.microc.2019.
103989.
[120] Aydin, F.; Yilmaz, E.; Soylak, M. A Simple and Novel Deep
Eutectic Solvent Based Ultrasound-Assisted Emulsification
Liquid Phase Microextraction Method for Malachite Green in
Farmed and Ornamental Aquarium Fish Water Samples.
Microchem. J. 2017, 132, 280–285. DOI: 10.1016/j.microc.2017.
02.014.
[121] Alveroglu, E.; Balouch, A.; Talpur, F. N.; Shah, M. T.; Kumar,
A.; Mahar, A. M.; Jagirani, M. S. Ultrasonic Mediated
Synthesis of Arsenic Imprinted Polymer and Their Analytical
Practicality as a Selective Sorbent for Removal of Toxic as 3þ
Ion from Real Samples. J. Polym. Res. 2020, 27, 1–11. DOI: 10.
1007/s10965-020-02196-0.
[122] Jagirani, M. S.; Balouch, A.; Abdullah; Mahar, A. M.; Mustafai,
F. A.; Rajar, K.; Tunio, A.; Sabir, S.; Samoon, M. K. Arsenic
Remediation by Synthetic and Natural Adsorbents. Pak. J.
Anal. Environ. Chem. 2017, 18, 18–36.
[123] Jagirani, M. S.; Balouch, A.; Mahesar, S. A.; Kumar, A.;
Abdullah; Mustafai, F. A.; Bhanger, M. I. Preparation of Novel
Arsenic-Imprinted Polymer for the Selective Extraction and
Enhanced Adsorption of Toxic As3þ Ions from the Aqueous
Environment. Polym. Bull. 2019, 77, 5261–5279. DOI: 10.1007/
s00289-019-03008-2.
[124] Jagirani, M. S.; Balouch, A.; Mahesar, S. A.; Kumar, A.;
Baloch, A. R.; Abdullah; Bhanger, M. I. Fabrication of
Cadmium Tagged Novel Ion Imprinted Polymer for
Detoxification of the Toxic Cd2 þ Ion from Aqueous
Environment. Microchem. J. 2020, 158, 105247. DOI: 10.1016/
j.microc.2020.105247.
[125] Jagirani, M. S.; Soylak, M. A Review: Recent Advances in Solid
Phase Microextraction of Toxic Pollutants Using
Nanotechnology Scenario. Microchem. J. 2020, 159, 105436.
DOI: 10.1016/j.microc.2020.105436.
[126] Jagirani, M. S.; Uzcan, F.; Soylak, M. A Selective and Sensitive
Procedure for Magnetic Solid-Phase Microextraction of Lead
(II) on Magnetic Cellulose Nanoparticles from Environmental
Samples Prior to Its Flame Atomic Absorption Spectrometric
Detection. J. Iran. Chem. Soc. 2020, 1–9. DOI: 10.1007/s13738-
02085-9.
[127] Kori, A. H.; Jakhrani, M. A.; Mahesar, S. A.; Shar, G. Q.;
Jagirani, M. S.; Shar, A. R.; Sahito, O. M. Risk Assessment of
Arsenic in Ground Water of Larkana City. Geol. Ecol. Landsc.
2018, 2, 8–14. DOI: 10.1080/24749508.2018.1438742.
[128] Kori, A. H.; Mahesar, S. A.; Jagirani, M. S.; Laghari, Z. H.;
Panhwar, T.; Jagirani, M. D.; Sahito, O. M.; Lanjwani, M. F.
Human Exposure and Risk Assessment Due to Toxic Heavy
Metals in Groundwater of Larkana City. Water Air Soil Pollut.
2020, 231, 1–10.
[129] Kumar, A.; Balouch, A.; Pathan, A. A.; A.; Jagirani, M. S.;
Mahar, A. M.; Rajput, M.-U.-H. Novel Chromium Imprinted
Polymer: Synthesis, Characterization and Analytical

Applicability for the Selective Remediation of Cr(VI) from an
Aqueous System. Int. J. Environ. Anal. Chem. 2019, 99,
454–473. DOI: 10.1080/03067319.2019.1599876.
[130] Kumar, A.; Balouch, A.; Pathan, A. A.; Jagirani, M. S.; Mahar,
A. M.; Zubair, M.; Laghari, B, Abdullah Remediation of Nickel
Ion from Wastewater by Applying Various Techniques: A
Review. Acta Chem. Malaysia 2019, 3, 1–15. DOI: 10.2478/
acmy-2019-0001.
[131] Kumar, A.; Balouch, A. A.; Pathan, A. M.; Mahar, Abdullah,
M. S.; Jagirani, F. A.; Mustafai, M.; Zubair, B.; Laghari, P.
Panah, Remediation Techniques Applied for Aqueous System
Contaminated by Toxic Chromium and Nickel Ion. Geol. Ecol.
Landsc. 2017, 1, 143–153. DOI: 10.1080/24749508.2017.
1332860.
[132] Kumar, S.; Alveroglu, E.; Balouch, A.; Talpur, F. N.; Jagirani,
M. S.; Mahar, A. M.; Pato, A. H.; Mal, D.; Lal, S. Fabrication
of Chromium Imprinted Polymer: A Real Magneto Selective
Sorbent for Chromium Cr (VI) Removal in a Real Water
Sample. N. J. Chem. 2020, DOI: 10.1039/D0NJ04054A.
[133] Kataoka, H.; Lord, H. L.; Pawliszyn, J. Applications of Solid-
Phase Microextraction in Food Analysis. J. Chromatogr. A.
2000, 880, 35–62. DOI: 10.1016/S0021-9673(00)00309-5.
[134] Ozdemir, S.; Mohamedsaid, S. A.; Kilinc, E.; Yı ldı rı m, A.;
Soylak, M. Application of Magnetized Fungal Solid Phase
Extractor with Fe2O3 Nanoparticle for Determination and
Preconcentration of Co (II) and Hg (II) from Natural Water
Samples. Microchem. J. 2018, 143, 198–204. DOI: 10.1016/j.
microc.2018.07.032.
[135] Ozdemir, S.; Serkan Yalcin, M.; Kilinc, E.; Soylak, M. Boletus
Edulis Loaded with ^I3-Fe 2 O 3 Nanoparticles as a Magnetic
Sorbent for Preconcentration of Co (II) and Sn (II) Prior to
Their Determination by ICP-OES. Microchim Acta 2017, 185,
73–73.
[136] Beltran, J.; Lopez, F. J.; Hernandez, F. Solid-Phase
Microextraction in Pesticide Residue Analysis. J. Chromatogr.
A. 2000, 885, 389–404. DOI: 10.1016/S0021-9673(00)00142-4.
[137] Buldini, P. L.; Ricci, L.; Sharma, J. L. Recent Applications of
Sample Preparation Techniques in Food Analysis. J.
Chromatogr. A. 2002, 975, 47–70. DOI: 10.1016/S0021-
9673(02)01335-3.
[138] €
Aydin, F.; Yilmaz, E.; Olmez, E.; Soylak, M. Cu2O-CuO Ball
like/Multiwalled Carbon Nanotube Hybrid for Fast and
Effective Ultrasound-Assisted Solid Phase Extraction of
Uranium at Ultra-Trace Level Prior to ICP-MS Detection.
Talanta 2020, 207, 120295. DOI: 10.1016/j.talanta.2019.120295.
[139] Erbas, Z.; Soylak, M.; Ozdemir, S.; Kilinc, E. Fe3O4@ SiO2@
Bacillus Pumilis: Magnetised Solid Phase Bio-Extractor for
Preconcentration of Pb (II) and Cu (II) from Water Samples.
Int. J. Environ. Anal. Chem. 2019, 99, 1112–1122. DOI: 10.
1080/03067319.2019.1616710.
[140] Ozdemir, S.; Yalcin, M. S.; Kilinc, E.; Soylak, M. Boletus
Edulis Loaded with c-Fe2O3 Nanoparticles as a Magnetic
Sorbent for Preconcentration of Co(II) and Sn(II) Prior to
their Determination by ICP-OES. Mikrochim. Acta. 2017, 185,
73. DOI: 10.1007/s00604-017-2605-5.
[141] Ozdemir, S.; Yalcin, M. S.; Kilinc, E.; Soylak, M. Magnetic
Solid-Phase Extraction Based on Coriolus Versicolor-
Immobilized gamma-Fe2O3 Nanoparticles for
Preconcentration and Determination of Al (III) in Water and
Food Samples. Turk. J. Chem. 2019, 43, 1217–1228. DOI: 10.
3906/kim-1904-18.
[142] Ozkantar, N.; Yilmaz, E.; Soylak, M.; Tuzen, M. Pyrocatechol
Violet Impregnated Magnetic Graphene Oxide for Magnetic
Solid Phase Microextraction of Copper in Water, Black Tea
and Diet Supplements. Food Chem. 2020, 321, 126737. DOI:
10.1016/j.foodchem.2020.126737.
[143] Kanberoglu, G. S.; Yilmaz, E.; Soylak, M. Fabrication and
Characterization of SiO2@ Fe3O4@ Nanodiamonds for
Vortex-Assisted Magnetic Solid-Phase Extraction of Lead in
Cigarette Samples Prior to FAAS Detection. Journal of the
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 21
Iranian Chemical Society. 2020, 17, 1627–1634. DOI:10.1007/
s13738-020-01882-6.
[144] Jain, R.; Singh, R. Microextraction Techniques for Analysis of
Cannabinoids. TrAC Trends Anal. Chem. 2016, 80, 156–166.
DOI: 10.1016/j.trac.2016.03.012.
[145] Spietelun, A.; Marcinkowski, Ł.; de la Guardia, M.; Namiesnik,
J. Green Aspects, Developments and Perspectives of Liquid
Phase Microextraction Techniques. Talanta 2014, 119, 34–45.
DOI: 10.1016/j.talanta.2013.10.050.
[146] Dias, A. N.; Sim~ao, V.; Merib, J.; Carasek, E. Use of Green
Coating (Cork) in Solid-Phase Microextraction for the
Determination of Organochlorine Pesticides in Water by Gas
Chromatography-Electron Capture Detection. Talanta 2015,
134, 409–414. DOI: 10.1016/j.talanta.2014.11.045.
[147] Souza-Silva, E. A.; Lopez-Avila, V.; Pawliszyn, J. Fast and
Robust Direct Immersion Solid Phase Microextraction
Coupled with Gas Chromatography-Time-of-Flight Mass
Spectrometry Method Employing a Matrix Compatible Fiber
for Determination of Triazole Fungicides in Fruits. J.
Chromatogr. A. 2013, 1313, 139–146. DOI: 10.1016/j.chroma.
2013.07.071.
[148] Tuzen, M.; Saygi, K. O.; Soylak, M. Solid Phase Extraction of
Heavy Metal Ions in Environmental Samples on Multiwalled
Carbon Nanotubes. J. Hazard Mater. 2008, 152, 632–639.
DOI: 10.1016/j.jhazmat.2007.07.026.
[149] Tuzen, M.; Saygi, K. O.; Usta, C.; Soylak, M. Pseudomonas
aeruginosa Immobilized Multiwalled Carbon Nanotubes as
Biosorbent for Heavy Metal Ions. Bioresour. Technol. 2008, 99,
1563–1570. DOI: 10.1016/j.biortech.2007.04.013.
[150] Li, J.; Zhang, Z.; Sun, M.; Zhang, B.; Fan, C. Use of a
Headspace Solid-Phase Microextraction-Based Methodology
Followed by Gas Chromatography–Tandem Mass
Spectrometry for Pesticide Multiresidue Determination in
Teas. Chromatographia 2018, 81, 809–821. DOI: 10.1007/
s10337-018-3499-z.
[151] Du, L.; Li, J.; Li, W.; Li, Y.; Li, T.; Xiao, D. Characterization of
Volatile Compounds of pu-Erh Tea Using Solid-Phase
Microextraction and Simultaneous Distillation–Extraction
Coupled with Gas Chromatography–Mass Spectrometry. Food
Res. Int. 2014, 57, 61–70. DOI: 10.1016/j.foodres.2014.01.008.
[152] Gutierrez-Serpa, A.; Rocıo-Bautista, P.; Pino, V.; Jimenez-
Moreno, F.; Jimenez-Abizanda, A. I. Gold Nanoparticles Based
Solid-Phase Microextraction Coatings for Determining
Organochlorine Pesticides in Aqueous Environmental Samples.
J. Sep. Sci 2017, 40, 2009–2021.
[153] Wu, F.; Lu, W.; Chen, J.; Liu, W.; Zhang, L. Single-Walled
Carbon Nanotubes Coated Fibers for Solid-Phase
Microextraction and Gas Chromatography-Mass Spectrometric
Determination of Pesticides in Tea Samples. Talanta 2010, 82,
1038–1043. DOI: 10.1016/j.talanta.2010.06.016.
[154] Zhang, S.; Yang, Q.; Yang, X.; Wang, W.; Li, Z.; Zhang, L.;
Wang, C.; Wang, Z. A Zeolitic Imidazolate Framework Based
Nanoporous Carbon as a Novel Fiber Coating for Solid-Phase
Microextraction of Pyrethroid Pesticides. Talanta 2017, 166,
46–53. DOI: 10.1016/j.talanta.2017.01.042.
[155] Wang, Q.; Li, G.; Wang, C.; Wu, Q.; Wang, Z. Layered Porous
Organic Frameworks as a Novel Adsorbent for the Solid Phase
Extraction of Chlorophenols Prior to Their Determination by
HPLC-DAD. Microchim. Acta 2020, 187, 1–11. DOI: 10.1007/
s00604-020-4195-x.
[156] Boyd-Boland, A. A.; Pawliszyn, J. B. Solid-Phase Microextraction
of Nitrogen-Containing Herbicides. J. Chromatogr. A. 1995, 704,
163–172. DOI: 10.1016/0021-9673(95)00151-C.
[157] Falqui-Cao, C.; Wang, Z.; Urruty, L.; Pommier, J.-J.; Montury,
M. Focused Microwave Assistance for Extracting Some
Pesticide Residues from Strawberries into Water before Their
Determination by SPME/HPLC/DAD. J. Agric. Food Chem.
2001, 49, 5092–5097. DOI: 10.1021/jf010519u.
[158] Ulusoy, H. I.;_ Yı lmaz, E.; Soylak, M. Magnetic Solid Phase
Extraction of Trace Paracetamol and Caffeine in Synthetic
22 M. S. JAGIRANI ET AL.
Urine and Wastewater Samples by a Using Core Shell Hybrid
Material Consisting of Graphene Oxide/Multiwalled Carbon
Nanotube/Fe3O4/SiO2. Microchem. J. 2019, 145, 843–851.
DOI: 10.1016/j.microc.2018.11.056.
[159] Wennrich, L.; Popp, P.; K€ oller, G.; Breuste, J. Determination
of Organochlorine Pesticides and Chlorobenzenes in
Strawberries by Using Accelerated Solvent Extraction
Combined with Sorptive Enrichment and Gas
Chromatography/Mass Spectrometry. J. AOAC Int. 2001, 84,
1194–1201. DOI: 10.1093/jaoac/84.4.1194.
[160] Barnabas, I.; Dean, J.; Fowlis, I.; Owen, S. Automated
Determination of s-Triazine Herbicides Using Solid-Phase
Microextraction. J. Chromatogr. A. 1995, 705, 305–312. DOI:
10.1016/0021-9673(95)00279-V.
[161] Eisert, R.; Levsen, K. Determination of Pesticides in Aqueous
Samples by Solid-Phase Microextraction in-Line Coupled to
Gas Chromatography—Mass Spectrometry. J. Am. Soc. Mass
Spectrom. 1995, 6, 1119–1130. DOI: 10.1016/1044-
0305(95)00527-7.
[162] Tuzen, M.; Soylak, M.; Citak, D.; Ferreira, H. S.; Korn, M. G.;
Bezerra, M. A. A Preconcentration System for Determination
of Copper and Nickel in Water and Food Samples Employing
Flame Atomic Absorption Spectrometry. J. Hazard. Mater.
2009, 162, 1041–1045. DOI: 10.1016/j.jhazmat.2008.05.154.
[163] Ulusoy, H. I.; _ G€ ulle, S.; Yilmaz, E.; Soylak, M. Trace
Determination of Vitamin B12 in Food Samples by Using
Fe3O4 Magnetic Particles Including Multi-Walled Carbon
Nanotubes and Nanodiamonds. Anal. Methods 2019, 11,
5108–5117. DOI: 10.1039/C9AY01504C.
[164] Yilmaz, E.; Soylak, M. Ultrasound Assisted-Deep Eutectic
Solvent Based on Emulsification Liquid Phase Microextraction
Combined with Microsample Injection Flame Atomic
Absorption Spectrometry for Valence Speciation of
Chromium(III/VI) in Environmental Samples. Talanta 2016,
160, 680–685. DOI: 10.1016/j.talanta.2016.08.001.
[165] Cai, L.; Xing, J.; Dong, L.; Wu, C. Application of
Polyphenylmethylsiloxane Coated Fiber for Solid-Phase
Microextraction Combined with Microwave-Assisted
Extraction for the Determination of Organochlorine Pesticides
in Chinese Teas. J. Chromatogr. A. 2003, 1015, 11–21. DOI:
10.1016/S0021-9673(03)01328-1.
[166] Yao, Z-w.; Jiang, G-b.; Liu, J-m.; Cheng, W. Application of
Solid-Phase Microextraction for the Determination of
Organophosphorous Pesticides in Aqueous Samples by Gas
Chromatography with Flame Photometric Detector. Talanta
2001, 55, 807–814. DOI: 10.1016/S0039-9140(01)00504-5.
[167] Lambropoulou, D. A.; Sakkas, V. A.; Hela, D. G.; Albanis,
T. A. Application of Solid-Phase Microextraction in the
Monitoring of Priority Pesticides in the Kalamas River (NW
Greece). J. Chromatogr. A 2002, 963, 107–116. DOI: 10.1016/
S0021-9673(02)00173-5.
[168] Song, X.-Y.; Shi, Y.-P.; Chen, J. Carbon Nanotubes-Reinforced
Hollow Fibre Solid-Phase Microextraction Coupled with High
Performance Liquid Chromatography for the Determination of
Carbamate Pesticides in Apples. Food Chem. 2013, 139,
246–252. DOI: 10.1016/j.foodchem.2013.01.112.
[169] Doong, R.-A.; Liao, P.-L. Determination of Organochlorine
Pesticides and Their Metabolites in Soil Samples Using
Headspace Solid-Phase Microextraction. J. Chromatogr. A.
2001, 918, 177–188. DOI: 10.1016/S0021-9673(01)00740-3.
[170] Dong, C.; Zeng, Z.; Li, X. Determination of Organochlorine
Pesticides and Their Metabolites in Radish after Headspace
Solid-Phase Microextraction Using Calix[4]Arene Fiber.
Talanta 2005, 66, 721–727. DOI: 10.1016/j.talanta.2004.12.020.
[171] J
unior, J. L. R. N. Re-Poppi, Determination of Organochlorine
Pesticides in Ground Water Samples Using Solid-Phase
Microextraction by Gas Chromatography-Electron Capture
Detection. Talanta 2007, 72, 1833–1841.
[172] Fernandez, M.; Padron, C.; Marconi, L.; Ghini, S.; Colombo,
R.; Sabatini, A.; Girotti, S. Determination of
Organophosphorus Pesticides in Honeybees after Solid-Phase
Microextraction. J. Chromatogr. A. 2001, 922, 257–265. DOI:
10.1016/S0021-9673(01)00880-9.
[173] Yu, J.; Wu, C.; Xing, J. Development of New Solid-Phase
Microextraction Fibers by Sol-Gel Technology for the
Determination of Organophosphorus Pesticide Multiresidues
in Food. J. Chromatogr. A. 2004, 1036, 101–111. DOI: 10.
1016/j.chroma.2004.02.081.
[174] Li, H.-P.; Li, G.-C.; Jen, J.-F. Determination of Organochlorine
Pesticides in Water Using Microwave Assisted Headspace
Solid-Phase Microextraction and Gas Chromatography. J.
Chromatogr. A 2003, 1012, 129–137. DOI: 10.1016/S0021-
9673(03)00916-6.
[175] Wang, W.; Wang, W.; Zhang, S.; Li, Z.; Wang, C.; Wang, Z.
Hyper-Crosslinked Polymer Nanoparticles as the Solid-Phase
Microextraction Fiber Coating for the Extraction of
Organochlorines. J. Chromatogr. A. 2018, 1556, 47–54. DOI:
10.1016/j.chroma.2018.05.001.
[176] Ebrahimi, M.; Es‘Haghi, Z.; Samadi, F.; Hosseini, M.-S. Ionic
Liquid Mediated Sol-Gel Sorbents for Hollow Fiber Solid-
Phase Microextraction of Pesticide Residues in Water and
Hair Samples. J. Chromatogr. A. 2011, 1218, 8313–8321. DOI:
10.1016/j.chroma.2011.09.058.
[177] Jabbari, M.; Razmi, H.; Farrokhzadeh, S. Application of
Magnetic Graphene Nanoparticles for Determination of
Organophosphorus Pesticides Using Solid-Phase
Microextraction. Chromatographia 2016, 79, 985–993. DOI:
10.1007/s10337-016-3117-x.
[178] Liu, S.; Xie, L.; Zheng, J.; Jiang, R.; Zhu, F.; Luan, T.; Ouyang,
G. Mesoporous TiO2 Nanoparticles for Highly Sensitive Solid-
Phase Microextraction of Organochlorine Pesticides. Anal.
Chim. Acta. 2015, 878, 109–117. DOI: 10.1016/j.aca.2015.03.
054.
[179] Zhang, S.; Du, Z.; Li, G. Metal-Organic Framework-199/
Graphite Oxide Hybrid Composites Coated Solid-Phase
Microextraction Fibers Coupled with Gas Chromatography for
Determination of Organochlorine Pesticides from Complicated
Samples. Talanta 2013, 115, 32–39. DOI: 10.1016/j.talanta.
2013.04.029.
[180] Chen, T.; Xu, H. In Vivo Investigation of Pesticide Residues in
Garlic Using Solid Phase Microextraction-Gas
Chromatography-Mass Spectrometry. Anal. Chim. Acta. 2019,
1090, 72–81. DOI: 10.1016/j.aca.2019.09.011.
[181] Frıas, S.; Rodrıguez, M. A.; Conde, J. E.; Perez-Trujillo, J. P. ;
Optimisation of a Solid-Phase Microextraction Procedure for
the Determination of Triazines in Water with Gas
Chromatography–Mass Spectrometry Detection. J.
Chromatogr. A. 2003, 1007, 127–135. DOI: 10.1016/S0021-
9673(03)00957-9.
[182] Ibrahim, W. A. W.; Farhani, H.; Sanagi, M. M.; Aboul-Enein,
H. Y. Solid Phase Microextraction Using New Sol-Gel Hybrid
Polydimethylsiloxane-2-Hydroxymethyl-18-Crown-6-Coated
Fiber for Determination of Organophosphorous Pesticides. J.
Chromatogr. A. 2010, 1217, 4890–4897. DOI: 10.1016/j.
chroma.2010.05.050.
[183] Li, D.; He, M.; Chen, B.; Hu, B. Magnetic Porous Organic
Polymers for Magnetic Solid-Phase Extraction of Triazole
Fungicides in Vegetables Prior to Their Determination by Gas
Chromatography-Flame Ionization Detection. J. Chromatogr.
A. 2019, 1601, 1–8. DOI: 10.1016/j.chroma.2019.04.062.
[184] Mukdasai, S.; Thomas, C.; Srijaranai, S. Two-Step
Microextraction Combined with High Performance Liquid
Chromatographic Analysis of Pyrethroids in Water and
Vegetable Samples. Talanta 2014, 120, 289–296. DOI: 10.1016/
j.talanta.2013.12.005.
[185] Shakourian, M.; Yamini, Y.; Safari, M. Facile Magnetization of
Metal–Organic Framework TMU-6 for Magnetic Solid-Phase
Extraction of Organophosphorus Pesticides in Water and Rice
Samples. Talanta 2020, 218, 121139. DOI: 10.1016/j.talanta.
2020.121139.

[186] Obuseng, V. C.; Mookantsa, B. M.; Okatch, H.; Mosepele, K.;
Torto, N. Extraction of Pesticides from Plants Using Solid
Phase Microextraction and QuEChERS. S. Afr. J. Chem. 2013,
66, 183–188.
[187] do Carmo, S. N.; Mendes, L. D.; Corazza, G.; Comelli, H.;
Merib, J.; Carasek, E. Determination of Pesticides of Different
Chemical Classes in Drinking Water of the State of Santa
Catarina (Brazil) Using Solid-Phase Microextraction Coupled
to Chromatographic Determinations. Environ. Sci. Pollut. Res.
2020, 27, 43870–43874. DOI: 10.1007/s11356-020-10287-0.
[188] Asadi, M.; Sereshti, H. Magnetic Amino-Functionalized
Hollow Silica-Titania Microsphere as an Efficient Sorbent for
Extraction of Pesticides in Green and Roasted Coffee Beans. J.
Sep. Sci. 2020, 43, 2115–2124. DOI: 10.1002/jssc.201901135.
[189] Mohammadi, P.; Masrournia, M.; Es’haghi, Z. Magnetic
Dispersive Solid-Phase Microextraction for Determination of
Two Organophosphorus Pesticides in Cucumber and Orange
Samples. J. Iran. Chem. Soc. 2020, 17, 3285–3294. DOI: 10.
1007/s13738-020-01991-2.
[190] Lu, N.; He, X.; Wang, T.; Liu, S.; Hou, X. Magnetic Solid-
Phase Extraction Using MIL-101 (Cr)-Based Composite
Combined with Dispersive Liquid-Liquid Microextraction
Based on Solidification of a Floating Organic Droplet for the
Determination of Pyrethroids in Environmental Water and
Tea Samples. Microchem. J. 2018, 137, 449–455. DOI: 10.1016/
j.microc.2017.12.009.
[191] Kirschner, N.; Dias, A. N.; Budziak, D.; da Silveira, C. B.;
Merib, J.; Carasek, E. Novel Approach to High-Throughput
Determination of Endocrine Disruptors Using Recycled
Diatomaceous Earth as a Green Sorbent Phase for Thin-Film
Solid-Phase Microextraction Combined with 96-Well Plate
System. Anal. Chim. Acta. 2017, 996, 29–37. DOI: 10.1016/j.
aca.2017.09.047.
[192] Omena, E.; Oenning, A. L.; Merib, J.; Richter, P.; Rosero-
Moreano, M.; Carasek, E. A Green and Simple Sample
Preparation Method to Determine Pesticides in Rice Using a
Combination of SPME and Rotating Disk Sorption Devices.
Anal. Chim. Acta. 2019, 1069, 57–65. DOI: 10.1016/j.aca.2019.
04.002.
[193] Farajzadeh, M. A.; Dabbagh, M. S. Development of a
Dispersive Solid Phase Extraction Method Based on in Situ
Formation of Adsorbent Followed by Dispersive Liquid-Liquid
Microextraction for Extraction of Some Pesticide Residues in
Fruit Juice Samples. J. Chromatogr. A. 2020, 1627, 461398.
DOI: 10.1016/j.chroma.2020.461398.
[194] Valenzuela, E. F.; de Paula, F. G.; Teixeira, A. P. C.; Menezes,
H. C.; Cardeal, Z. L. A New Carbon Nanomaterial Solid-Phase
Microextraction to Pre-Concentrate and Extract Pesticides in
Environmental Water. Talanta 2020, 217, 121011. DOI: 10.
1016/j.talanta.2020.121011.
[195] Wang, R.; Sun, X.; Wang, X.; Chen, J.; Wang, B.; Ji, W.
Spherical Conjugated Microporous Polymers for Solid Phase
Microextraction of Carbamate Pesticides from Water samples.
J. Chromatogr. A. 2020, 1626, 461360. DOI: 10.1016/j.chroma.
2020.461360.
[196] Hu, J.; Qian, C.; Zhang, Y.; Tian, Y.; Duan, Y. Sol-Gel
Fabrication and Performance Evaluation of Graphene-Based
Hydrophobic Solid-Phase Microextraction Fibers for Multi-
Residue Analysis of Pesticides in Water Samples. Anal.
Methods 2020, 12, 3954–3963. DOI: 10.1039/d0ay01153c.
[197] Khoshmanesh, S. M.; Hamishehkar, H.; Razmi, H. Trace
Analysis of Organophosphorus Pesticide Residues in Fruit
Juices and Vegetables by an Electrochemically Fabricated
Solid-Phase Microextraction Fiber Coated with a Layer-by-
Layer Graphenized Graphite/Graphene Oxide/Polyaniline
Nanocomposite. Anal. Methods 2020, 12, 3268–3276. DOI: 10.
1039/d0ay00626b.
[198] Pang, Y.; Zang, X.; Li, H.; Liu, J.; Chang, Q.; Zhang, S.; Wang,
C.; Wang, Z. Solid-Phase Microextraction of
Organophosphorous Pesticides from Food Samples with a
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 23
Nitrogen-Doped Porous Carbon Derived from g-C3N4
Templated MOF as the Fiber Coating. J. Hazard. Mater. 2020,
384, 121430. DOI: 10.1016/j.jhazmat.2019.121430.
[199] Xiang, X.; Wang, Y.; Zhang, X.; Huang, M.; Li, X.; Pan, S.
Multifiber Solid-Phase Microextraction using Different
Molecularly Imprinted Coatings for Simultaneous Selective
Extraction and Sensitive Determination of Organophosphorus
Pesticides. J. Sep. Sci. 2020, 43, 756–765. DOI: 10.1002/jssc.
201900994.
[200] Feriduni, B.; Mohebbi, A.; Farajzadeh, M. A.; Namvar, M.
Magnetic Graphene Oxide–Based Solid-Phase Extraction
Combined with Dispersive Liquid–Liquid Microextraction for
the Simultaneous Preconcentration of Four Typical Pesticide
Residues in Fruit Juice and Pulp. Food Anal. Methods 2019,
12, 2742–2752. DOI: 10.1007/s12161-019-01635-z.
[201] Li, C.; Begum, A.; Xue, J. Analytical Methods to Analyze
Pesticides and Herbicides. Water Environ. Res. 2020, 92,
1770–1785.
[202] Wu, J.; Mei, M.; Huang, X. Fabrication of Boron-Rich
Multiple Monolithic Fibers for the Solid-Phase
Microextraction of Carbamate Pesticide Residues in Complex
Samples. J. Sep. Sci. 2019, 42, 878–887. DOI: 10.1002/jssc.
201800996.
[203] Hercegova, A.; D€ om€ot€
orova, M.; Kruzlicova, D.; Matisova, E.
Comparison of Sample Preparation Methods Combined with
Fast Gas Chromatography–Mass Spectrometry for Ultratrace
Analysis of Pesticide Residues in Baby Food. J. Sep. Sci. 2006,
29, 1102–1109. DOI: 10.1002/jssc.200500422.
[204] Leandro, C. C.; Fussell, R. J.; Keely, B. J. Determination of
Priority Pesticides in Baby Foods by Gas Chromatography
Tandem Quadrupole Mass Spectrometry. J. Chromatogr. A.
2005, 1085, 207–212. DOI: 10.1016/j.chroma.2005.06.054.
[205] Jimenez Soto, J. M.; Aranzana, M. S. C. Conical Carbon
Nanoparticles in Analytical Chemistry. In Encyclopedia of
Analytical Chemistry: Applications, Theory and
Instrumentation; Wiley: Hoboken, 2006. doi.org/10.1002/
9780470027318.a9283.
[206] Ghorbani, M.; Aghamohammadhassan, M.; Chamsaz, M.;
Akhlaghi, H.; Pedramrad, T. Dispersive Solid Phase
Microextraction. TrAC Trends Anal. Chem. 2019, 118,
793–809. DOI: 10.1016/j.trac.2019.07.012.
[207] Ouyang, G.; Zhao, W.; Pawliszyn, J. Automation and
Optimization of Liquid-Phase Microextraction by Gas
Chromatography. J. Chromatogr. A. 2007, 1138, 47–54. DOI:
10.1016/j.chroma.2006.10.093.
[208] Bedendo, G. C.; Jardim, I. C. S. F.; Carasek, E. A Simple
Hollow Fiber Renewal Liquid Membrane Extraction Method
for Analysis of Sulfonamides in Honey Samples with
Determination by Liquid Chromatography-Tandem Mass
Spectrometry. J. Chromatogr. A. 2010, 1217, 6449–6454. DOI:
10.1016/j.chroma.2010.08.030.
[209] Rezaee, M.; Assadi, Y.; Hosseini, M.-R. M.; Aghaee, E.;
Ahmadi, F.; Berijani, S. Determination of Organic Compounds
in Water Using Dispersive Liquid-Liquid Microextraction. J.
Chromatogr. A. 2006, 1116, 1–9. DOI: 10.1016/j.chroma.2006.
03.007.
[210] Ccanccapa-Cartagena, A.; Masia, A.; Pico, Y. Simultaneous
Determination of Pyrethroids and Pyrethrins by Dispersive
Liquid-Liquid Microextraction and Liquid Chromatography
Triple Quadrupole Mass Spectrometry in Environmental
Samples. Anal. Bioanal. Chem. 2017, 409, 4787–4799. DOI: 10.
1007/s00216-017-0422-7.
[211] Noori, A. H.; Rezaee, M.; Kazemipour, M.; Mashayekhi, H. A.
Simultaneous Determination of Permethrin and Deltamethrin
in Water Samples by Magnetic Solid-Phase Extraction
Coupled with Dispersive Liquid-Liquid Microextraction
Combined with Gas Chromatography. S. Afr. J. Chem. 2017,
70, 200–208.
[212] Farajzadeh, M. A.; Yadeghari, A.; Khoshmaram, L.
Combination of Dispersive Solid Phase Extraction and
24 M. S. JAGIRANI ET AL.
Dispersive Liquid–Liquid Microextraction for Extraction of
Some Aryloxy Pesticides Prior to Their Determination by Gas
Chromatography. Microchem. J. 2017, 131, 182–191. DOI: 10.
1016/j.microc.2016.12.013.
[213] Jahan, K.; Ord on~ez, R.; Ramachandran, R.; Balzer, S.; Stern,
M. Modeling Biodegradation of Nonylphenol. Water Air Soil
Pollut. Focus 2008, 8, 395–404. DOI: 10.1007/s11267-007-
9148-4.
[214] Yan, Y.; Chen, X.; Hu, S.; Bai, X. Applications of Liquid-Phase
Microextraction Techniques in Natural Product Analysis: A
Review. J. Chromatogr. A. 2014, 1368, 1–17. DOI: 10.1016/j.
chroma.2014.09.068.
[215] Jeannot, M. A.; Cantwell, F. F. Solvent Microextraction into a
Single Drop. Anal. Chem. 1996, 68, 2236–2240. DOI: 10.1021/
ac960042z.
[216] Bagheri, H.; Khalilian, F. Immersed Solvent Microextraction
and Gas Chromatography–Mass Spectrometric Detection of s-
Triazine Herbicides in Aquatic Media. Anal. Chim. Acta 2005,
537, 81–87. DOI: 10.1016/j.aca.2005.01.036.
[217] Cacho, J.; Campillo, N.; Vi~nas, P.; Hernandez-C
ordoba, M. In
Situ Ionic Liquid Dispersive Liquid-Liquid Microextraction
Coupled to Gas Chromatography-Mass Spectrometry for the
Determination of Organophosphorus Pesticides. J.
Chromatogr. A. 2018, 1559, 95–101. DOI: 10.1016/j.chroma.
2017.12.059.
[218] Hamid, Y.; Fat’hi, M. R. A Fast and Green Preconcentration
Method Based on Surfactant Ion Pair-Switchable Solvent
Dispersive Liquid–Liquid Microextraction for Determination
of Phenazopyridine in Pharmaceutical and Biological Samples.
J. Iran. Chem. Soc. 2018, 15, 1813–1820. DOI: 10.1007/s13738-
018-1378-z.
[219] Rykowska, I.; Ziembli nska, J.; Nowak, I. Modern Approaches
in Dispersive Liquid-Liquid Microextraction (DLLME) Based
on Ionic Liquids: A Review. J. Mol. Liq. 2018, 259, 319–339.
DOI: 10.1016/j.molliq.2018.03.043.
[220] Wang, H.; Hu, L.; Li, W.; Yang, X.; Lu, R.; Zhang, S.; Zhou,
W.; Gao, H.; Li, J. In-Syringe Dispersive Liquid-Liquid
Microextraction Based on the Solidification of Ionic Liquids
for the Determination of Benzoylurea Insecticides in Water
and Tea Beverage Samples. Talanta 2017, 162, 625–633. DOI:
10.1016/j.talanta.2016.10.035.
[221] Pedersen-Bjergaard, S.; Rasmussen, K. E. Liquid-Liquid-Liquid
Microextraction for Sample Preparation of Biological Fluids
Prior to Capillary Electrophoresis. Anal. Chem. 1999, 71,
2650–2656. DOI: 10.1021/ac990055n.
[222] Alsharif, A. M. A.; Tan, G.-H.; Choo, Y.-M.; Lawal, A.
Efficiency of Hollow Fiber Liquid-Phase Microextraction
Chromatography Methods in the Separation of Organic
Compounds: A Review. J. Chromatogr. Sci. 2017, 55, 378–391.
DOI: 10.1093/chromsci/bmw188.]
[223] Chimuka, L.; Cukrowska, E.; Michel, M.; Buszewski, B.
Advances in Sample Preparation Using Membrane-Based
Liquid-Phase Microextraction Techniques. TrAC Trends Anal.
Chem. 2011, 30, 1781–1792. DOI: 10.1016/j.trac.2011.05.008.
[224] Xiao, Q.; Hu, B.; Duan, J.; He, M.; Zu, W. Analysis of PBDEs
in Soil, Dust, Spiked Lake Water, and Human Serum Samples
by Hollow Fiber-Liquid Phase Microextraction Combined with
GC-ICP-MS. J. Am. Soc. Mass. Spectrom. 2007, 18, 1740–1748.
DOI: 10.1016/j.jasms.2007.07.006.
[225] King, S.; Meyer, J. S.; Andrews, A. R. Screening Method for
Polycyclic Aromatic Hydrocarbons in Soil Using Hollow Fiber
Membrane Solvent Microextraction. J. Chromatogr. A. 2002,
982, 201–208. DOI: 10.1016/S0021-9673(02)01594-7.
[226] Jiang, X.; Basheer, C.; Zhang, J.; Lee, H. K. Dynamic Hollow
Fiber-Supported Headspace Liquid-Phase Microextraction. J.
Chromatogr. A. 2005, 1087, 289–294. DOI: 10.1016/j.chroma.
2005.06.010.
[227] Banimuslem, H. A. Organic/Carbon Nanotubes Hybrid Thin
Films for Chemical Detection; Sheffield Hallam University:
Sheffield, UK, 2015.
[228] Hou, L.; Lee, H. K. Determination of Pesticides in Soil by
Liquid-Phase Microextraction and Gas Chromatography-Mass
Spectrometry. J. Chromatogr. A. 2004, 1038, 37–42. DOI: 10.
1016/j.chroma.2004.03.012.
[229] Lambropoulou, D. A.; Albanis, T. A. Sensitive Trace
Enrichment of Environmental Andiandrogen Vinclozolin from
Natural Waters and Sediment Samples Using Hollow-Fiber
Liquid-Phase Microextraction. J. Chromatogr. A. 2004, 1061,
11–18. DOI: 10.1016/j.chroma.2004.10.064.
[230] Xiong, J.; Hu, B. Comparison of Hollow Fiber Liquid Phase
Microextraction and Dispersive Liquid-Liquid Microextraction
for the Determination of Organosulfur Pesticides in
Environmental and Beverage Samples by Gas Chromatography
with Flame Photometric Detection. J. Chromatogr. A. 2008,
1193, 7–18. DOI: 10.1016/j.chroma.2008.03.072.
[231] Asensio-Ramos, M.; Hernandez-Borges, J.; Borges-Miquel,
T. M.; Rodrıguez-Delgado, M. A.  Ionic Liquid-Dispersive
Liquid-Liquid Microextraction for the Simultaneous
Determination of Pesticides and Metabolites in Soils Using
High-Performance Liquid Chromatography and Fluorescence
Detection. J. Chromatogr. A. 2011, 1218, 4808–4816. DOI: 10.
1016/j.chroma.2010.11.030.
[232] Vidal, J. M.; Plaza-Bolanos, P.; Romero-Gonzalez, R.; Frenich,
A. G. Determination of Pesticide Transformation Products: A
Review of Extraction and Detection Methods. J. Chromatogr.
A. 2009, 1216, 6767–6788. DOI: 10.1016/j.chroma.2009.08.013.
[233] Zhang, J.; Lee, H. K. Application of Liquid-Phase
Microextraction and On-Column Derivatization Combined
with Gas Chromatography-Mass Spectrometry to the
Determination of Carbamate Pesticides. J. Chromatogr. A.
2006, 1117, 31–37. DOI: 10.1016/j.chroma.2006.03.102.
[234] Huang, S.-P.; Huang, S.-D. Determination of Organochlorine
Pesticides in Water Using Solvent Cooling Assisted Dynamic
Hollow-Fiber-Supported Headspace Liquid-Phase
Microextraction. J. Chromatogr. A. 2007, 1176, 19–25. DOI:
10.1016/j.chroma.2007.10.073.
[235] Basheer, C.; Alnedhary, A. A.; Rao, B. M.; Lee, H. K.
Determination of Organophosphorous Pesticides in
Wastewater Samples Using Binary-Solvent Liquid-Phase
Microextraction and Solid-Phase Microextraction: A
Comparative Study. Anal. Chim. Acta 2007, 605, 147–152.
DOI: 10.1016/j.aca.2007.10.006.
[236] Seebunrueng, K.; Phosiri, P.; Apitanagotinon, R.; Srijaranai, S.
A New Environment-Friendly Supramolecular Solvent-Based
Liquid Phase Microextraction Coupled to High Performance
Liquid Chromatography for Simultaneous Determination of
Six Phenoxy Acid Herbicides in Water and Rice Samples.
Microchem. J. 2020, 152, 104418. DOI: 10.1016/j.microc.2019.
104418.
[237] Chullasat, K.; Huang, Z.; Bunkoed, O.; Kanatharana, P.; Lee,
H. K. Bubble-in-Drop Microextraction of Carbamate
Pesticides Followed by Gas Chromatography-Mass
Spectrometric Analysis. Microchem. J. 2020, 155, 104666. DOI:
10.1016/j.microc.2020.104666.
[238] Mogaddam, M. R. A.; Farajzadeh, M. A.; Mohebbi, A.
Application of Temperature-Assisted Tandem Dispersive
Liquid–Liquid Microextraction for the Extraction and High
Preconcentration of Triazole Pesticides. Int. J. Environ. Anal.
Chem. 2020, 1–17.
[239] Mardani, A.; Torbati, M.; Farajzadeh, M. A.; Mohebbi, A.;
Mogaddam, M. R. A. Combination of Homogeneous
Liquid–Liquid Extraction and Dispersive Liquid–Liquid
Microextraction for Extraction of Some Organochlorine
Pesticides from Cocoa. Int. J. Environ. Anal. Chem. 2020,
1–14.
[240] Wang, X.; Cheng, J.; Zhou, H.; Wang, X.; Cheng, M.
Development of a Simple Combining Apparatus to Perform a
Magnetic Stirring-Assisted Dispersive Liquid-Liquid
Microextraction and Its Application for the Analysis of
Carbamate and Organophosphorus Pesticides in Tea Drinks.

Anal. Chim. Acta. 2013, 787, 71–77. DOI: 10.1016/j.aca.2013.
05.033.
[241] Ramos-Payan, M.; Maspoch, S.; Llobera, A. An Effective
Microfluidic Based Liquid-Phase Microextraction Device
(lLPME) for Extraction of Non-Steroidal anti-Inflammatory
Drugs from Biological and Environmental Samples. Anal.
Chim. Acta 2016, 946, 56–63. DOI: 10.1016/j.aca.2016.09.040.
[242] Huang, S.-P.; Huang, S.-D. Dynamic Hollow Fiber Protected
Liquid Phase Microextraction and Quantification Using Gas
Chromatography Combined with Electron Capture Detection
of Organochlorine Pesticides in Green Tea Leaves and Ready-
to-Drink Tea. J. Chromatogr. A. 2006, 1135, 6–11. DOI: 10.
1016/j.chroma.2006.09.027.
[243] Farajzadeh, M. A.; Mogaddam, M. R. A.; Aghdam, A. A.
Comparison of Air-Agitated Liquid-Liquid Microextraction
Technique and Conventional Dispersive Liquid-Liquid Micro-
Extraction for Determination of Triazole Pesticides in
Aqueous Samples by Gas Chromatography with Flame
Ionization Detection. J. Chromatogr. A. 2013, 1300, 70–78.
DOI: 10.1016/j.chroma.2013.02.033.
[244] Kumari, R.; Patel, D. K.; Panchal, S.; Jha, R. R.; Satyanarayana,
G.; Asati, A.; Ansari, N. G.; Pathak, M. K.; Kesavachandran,
C.; Murthy, R. C. Fast Agitated Directly Suspended Droplet
Microextraction Technique for the Rapid Analysis of Eighteen
Organophosphorus Pesticides in Human Blood. J. Chromatogr.
A. 2015, 1377, 27–34. DOI: 10.1016/j.chroma.2014.12.006.
[245] Farajzadeh, M. A.; Abbaspour, M.; Kazemian, R. Synthesis of a
Green High Density Deep Eutectic Solvent and Its Application
in Microextraction of Seven Widely Used Pesticides from
Honey. J. Chromatogr. A. 2019, 1603, 51–60. DOI: 10.1016/j.
chroma.2019.06.051.
[246] Chen, Z.; Li, Q.; Yang, T.; Zhang, Y.; He, M.; Zeng, H.; Mai,
X.; Liu, Y.; Fan, H. Sequential Extraction and Enrichment of
Pesticide Residues in Longan Fruit by Ultrasonic-Assisted
Aqueous Two-Phase Extraction Linked to Vortex-Assisted
Dispersive Liquid-Liquid Microextraction Prior to High
Performance Liquid Chromatography Analysis. J. Chromatogr.
A. 2020, 1619, 460929. DOI: 10.1016/j.chroma.2020.460929.
[247] Farajzadeh, M. A.; Khoshmaram, L. Air-Assisted Liquid-Liquid
Microextraction-Gas Chromatography-Flame Ionisation
Detection: A Fast and Simple Method for the Assessment of
Triazole Pesticides Residues in Surface Water, Cucumber,
Tomato and Grape Juices Samples. Food Chem. 2013, 141,
1881–1887. DOI: 10.1016/j.foodchem.2013.05.088.
[248] Boonchiangma, S.; Ngeontae, W.; Srijaranai, S. Determination
of Six Pyrethroid Insecticides in Fruit Juice Samples Using
Dispersive Liquid-Liquid Microextraction Combined With
High Performance Liquid Chromatography. Talanta 2012, 88,
209–215. DOI: 10.1016/j.talanta.2011.10.033.
[249] San Roman, I.; Alonso, M.; Bartolome, L.; Alonso, R. Hollow
Fibre-Based Liquid-Phase Microextraction Technique
Combined With Gas Chromatography-Mass Spectrometry for
the Determination of Pyrethroid Insecticides in Water
Samples. Talanta 2012, 100, 246–253. DOI: 10.1016/j.talanta.
2012.04.039.
[250] Torbati, M.; Farajzadeh, M. A.; Torbati, M.; Nabil, A. A. A.;
Mohebbi, A.; Mogaddam, M. R. A. Development of Salt and
pH-Induced Solidified Floating Organic Droplets
Homogeneous Liquid-Liquid Microextraction for Extraction of
Ten Pyrethroid Insecticides in Fresh Fruits and Fruit Juices
Followed by Gas Chromatography-Mass Spectrometry. Talanta
2018, 176, 565–572. DOI: 10.1016/j.talanta.2017.08.074.
[251] Farajzadeh, M. A.; Khorram, P.; Nabil, A. A. A. Development
of a Green Liquid–Liquid Microextraction Method Using a
Solid Disperser Performed in a Narrow-Bore Tube for Trace
Analysis of Some Organophosphorus Pesticides in Fruit Juices.
J. Food Compos. Anal. 2015, 43, 96–105. DOI: 10.1016/j.jfca.
2015.04.012.
[252] Naeeni, M. H.; Yamini, Y.; Rezaee, M. Combination of
Supercritical Fluid Extraction with Dispersive Liquid–Liquid
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 25
Microextraction for Extraction of Organophosphorus
Pesticides from Soil and Marine Sediment Samples. J.
Supercrit. Fluids 2011, 57, 219–226. DOI: 10.1016/j.supflu.
2011.03.005.
[253] Mogaddam, M. R. A.; Mohebbi, A.; Farajzadeh, M. A. A
Sensitive Determination of Triazole Pesticides in Grape Juice
by Combining Solid Phase Extraction–Dispersive
Liquid–Liquid Microextraction Followed by Gas
Chromatography–Flame Ionisation Detection. Int. J. Environ.
Anal. Chem. 2020, 1–16.
[254] Xiong, J.; Guan, Z.; Zhou, G.; Tang, X.; Lv, Y.; Wang, H.
Determination of Chlorpyrifos in Environmental Water
Samples by Dispersive Liquid–Liquid Microextraction with
Solidification of a Floating Organic Drop Followed by Gas
Chromatography with Flame Photometry Detection. Anal.
Methods 2012, 4, 3246–3250. DOI: 10.1039/c2ay25451d.
[255] Bessonova, E.; Deev, V.; Kartsova, L. Dispersive Liquid–Liquid
Microextraction of Pesticides Using Ionic Liquids as
Extractants. J. Anal. Chem. 2020, 75, 991–999. DOI: 10.1134/
S1061934820080043.
[256] Li, Z.; Zhang, S.; Yin, X.; Wang, C.; Wang, Z. Micellar
Electrokinetic Chromatographic Determination of Triazine
Herbicides in Water Samples. J. Chromatogr. Sci. 2014, 52,
926–931. DOI: 10.1093/chromsci/bmt124.
[257] €
Ozcan, R.; B€uy€
ukpı nar, Ç.; Bakı rdere, S. Determination of
Fipronil and Bixafen Pesticides Residues Using Gas
Chromatography Mass Spectroscopy with Matrix Matching
Calibration Strategy after Binary Dispersive Liquid-Liquid
Microextraction. J. Environ. Sci. Health Pt. B. 2020, 55,
1041–1047. DOI: 10.1080/03601234.2020.1808417.
[258] Farajzadeh, M. A.; Feriduni, B.; Afshar Mogaddam, M. R.
Extraction and Preconcentration of Triazine Pesticides Using
Rapid, Simple, and Disperser Solventless Microextraction
Technique Followed by Gas Chromatography–Nitrogen
Phosphorous Detection. Eur. J. Lipid Sci. Technol. 2017, 119,
1600208. DOI: 10.1002/ejlt.201600208.
[259] Farajzadeh, M. A.; Bahram, M.; Jafary, F.; Bamorowat, M.
Combination of Extraction by Silylated Vessel-Dispersive
Liquid–Liquid Microextraction as a High-Enrichment Factor
Technique: Optimization and Application in Preconcentration
of Some Triazole Pesticides from Aqueous Samples Followed
by GC-FID Determination. Chromatographia 2011, 73,
393–401. DOI: 10.1007/s10337-010-1895-0.
[260] Farajzadeh, M. A.; Mohebbi, A.; Mogaddam, M. R. A.;
Davaran, M.; Norouzi, M. Development of Salt-Induced
Homogenous Liquid–Liquid Microextraction Based on Iso-
Propanol/Sodium Sulfate System for Extraction of Some
Pesticides in Fruit Juices. Food Anal. Methods 2018, 11,
2497–2507. DOI: 10.1007/s12161-018-1238-6.
[261] Li, S.; Han, W.; Zhao, W.; Luo, Y. Flexible Dispersive
Liquid–Liquid Microextraction for on-Site Sample Pre-
Concentration. Int. J. Environ. Anal. Chem. 2021, 101,
281–299. DOI: 10.1080/03067319.2019.1665654.
[262] Khalili-Zanjani, M. R.; Yamini, Y.; Yazdanfar, N.; Shariati, S.
Extraction and Determination of Organophosphorus Pesticides
in Water Samples by a New Liquid Phase
Microextraction–Gas Chromatography–Flame Photometric
Detection. Anal. Chim. Acta 2008, 606, 202–208. DOI: 10.
1016/j.aca.2007.11.032.
[263] Zheng, Y.-Z.; Wang, K.; Liang, Q.; Xue, X.-F.; Zhao, L.-W.;
Chen, D.-F.; Wu, L.-M.; Guo, R.; Xiong, C.-L. Ionic Liquid
Dispersive Liquid–Liquid Microextraction for Pesticide
Residue Analysis in Honey. J. Apic. Res. 2020, 59, 458–467.
DOI: 10.1080/00218839.2019.1656701.
[264] Sereshti, H.; Jamshidi, F.; Nouri, N.; Nodeh, H. R. Hyphenated
Dispersive Solid- and Liquid-Phase Microextraction Technique
Based on a Hydrophobic Deep Eutectic Solvent: Application
for Trace Analysis of Pesticides in Fruit Juices. J. Sci. Food
Agric. 2020, 100, 2534–2543. DOI: 10.1002/jsfa.10279.
26 M. S. JAGIRANI ET AL.
[265] Yan, H.; Du, J.; Zhang, X.; Yang, G.; Row, K. H.; Lv, Y.
Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction
Coupled With Capillary Gas Chromatography for
Simultaneous Analysis of Nine Pyrethroids in Domestic
Wastewaters. J. Sep. Sci. 2010, 33, 1829–1835. DOI: 10.1002/
jssc.200900716.
[266] Farajzadeh, M. A.; Djozan, D.; Mogaddam, M. A.; Bamorowat,
M. Extraction and Preconcentration Technique for Triazole
Pesticides from Cow Milk Using Dispersive Liquid–Liquid
Microextraction Followed by GC-FID and GC-MS
Determinations. J. Sep. Sci. 2011, 34, 1309–1316. DOI: 10.
1002/jssc.201000928.
[267] Alves, A. C. H.; Gonçalves, M. M. P. B.; Bernardo, M. M. S.;
Mendes, B. S. Validated Dispersive Liquid-Liquid
Microextraction for Analysis of Organophosphorous Pesticides
in Water. J. Sep. Sci. 2011, 34, 1326–1332. DOI: 10.1002/jssc.
201100111.
[268] Tayyebi, M.; Yamini, Y.; Moradi, M. Reverse Micelle-Mediated
Dispersive Liquid-Liquid Microextraction of 2,4-
Dichlorophenoxyacetic Acid and 4-Chloro-2-
Methylphenoxyacetic Acid. J. Sep. Sci. 2012, 35, 2491–2498.
DOI: 10.1002/jssc.201200150.
[269] Mardani, A.; Afshar Mogaddam, M. R.; Farajzadeh, M. A.;
Mohebbi, A.; Nemati, M.; Torbati, M. A Three-Phase Solvent
Extraction System Combined With Deep Eutectic Solvent-
Based Dispersive Liquid-Liquid Microextraction for Extraction
of Some Organochlorine Pesticides in Cocoa Samples Prior to
Gas Chromatography With Electron Capture Detection. J. Sep.
Sci. 2020, 43, 3674–3682. DOI: 10.1002/jssc.202000507.
[270] Liu, L.; Cheng, J.; Matsadiq, G.; Zhou, H.; Li, J. Application of
DLLME to the Determination of Pyrethroids in Aqueous
Samples. Chroma 2010, 72, 1017–1020. DOI: 10.1365/s10337-
010-1732-5.
[271] Shirani, M.; Akbari-Adergani, B.; Jazi, M. B.; Akbari, A. Green
Ultrasound Assisted Magnetic Nanofluid-Based Liquid Phase
Microextraction Coupled with Gas Chromatography-Mass
Spectrometry for Determination of Permethrin, Deltamethrin,
and Cypermethrin Residues. Mikrochim Acta 2019, 186, 674.
DOI: 10.1007/s00604-019-3763-4.
[272] Amri, F.; Niazi, A.; Yazdanipour, A. Three-Pesticide Residue
Analysis in Tomato Using a Fast Pressure Variation in-Syringe
Dispersive Liquid-Phase Microextraction Technique Coupled
with Gas Chromatography-Mass Spectrometry by Assisting
Experimental Design. Int. J. Environ. Anal. Chem. 2020, 99,
1–18. DOI: 10.1080/03067319.2020.1724988.
[273] Zhang, S.; Yin, X.; Yang, Q.; Wang, C.; Wang, Z.
Determination of Some Sulfonylurea Herbicides in Soil by a
Novel Liquid-Phase Microextraction Combined With
Sweeping Micellar Electrokinetic Chromatography. Anal.
Bioanal. Chem. 2011, 401, 1071–1081. DOI: 10.1007/s00216-
011-5138-5.
[274] Zhou, S.; Chen, H.; Wu, B.; Ma, C.; Ye, Y. Sensitive
Determination of Carbamates in Fruit and Vegetables by a
Combination of Solid-Phase Extraction and Dispersive Liquid-
Liquid Microextraction Prior to HPLC. Microchim. Acta. 2012,
176, 419–427. DOI: 10.1007/s00604-011-0735-8.
[275] Anvar, S. A.; Torbati, M.; Farajzadeh, M. A.; Mogaddam,
M. R. A. Elevated Temperature Homogeneous Liquid Phase
Extraction Coupled to Ionic Liquid–Based Dispersive
Liquid–Liquid Microextraction Followed by High-Performance
Liquid Chromatography: application of Water-Miscible Ionic
Liquids as Extraction Solvent in Determination of Carbamate
Pesticides. Food Anal. Methods 2020, 13, 1282–1291. DOI: 10.
1007/s12161-020-01742-2.
[276] Berijani, S.; Sadigh, M.; Pournamdari, E. Homogeneous
Liquid-Liquid Microextraction for Determination of
Organophosphorus Pesticides in Environmental Water
Samples Prior to Gas Chromatography-Flame Photometric
Detection. J. Chromatogr. Sci. 2016, 54, 1061–1067. DOI: 10.
1093/chromsci/bmw020.
[277] Sheikhzadeh, F.; Mogaddam, M. R. A.; Farajzadeh, M. A.;
Khandaghi, J. Development of Microwave Radiations-Induced
Homogeneous Liquid-Liquid Microextraction Method for
Extraction of Pyrethroid Pesticides in Fruit and Vegetable
Samples. Int. J. Environ. Anal. Chem. 2020, 100, 1–12. DOI:
10.1080/03067319.2020.1758686.
[278] Musarurwa, H.; Tavengwa, N. T. Deep Eutectic Solvent-Based
Dispersive Liquid-Liquid Micro-Extraction of Pesticides in
Food Samples. Food Chem. 2020, 127943. DOI: 10.1016/j.food-
chem.2020.127943.
[279] Farajzadeh, M. A.; Sohrabi, H.; Mohebbi, A. Combination of
Modified QuEChERS Extraction Method and Dispersive
Liquid–Liquid Microextraction as an Efficient Sample
Preparation Approach for Extraction and Preconcentration of
Pesticides from Fruit and Vegetable Samples. Food Anal.
Methods 2019, 12, 534–543. DOI: 10.1007/s12161-018-1384-x.
[280] Farajzadeh, M. A.; Alavian, A. S.; Dabbagh, M. S.
Development of an Efficient Sample Preparation Method
Based on Homogeneous Liquid-Liquid Extraction Combined
with Dispersive Liquid-Liquid Microextraction Solidification of
Floating Organic Drop for Trace Analysis of Pesticide
Residues in Fruit and Fruit Juice Samples. Food Anal. Methods
2019, 12, 2730–2741. DOI: 10.1007/s12161-019-01628-y.
[281] Gao, Y.; Xu, C.; Liu, S.; Sun, P. Determination of Seven
Pyrethroid Pesticides in Liquid Milk by Dispersive
Liquid–Liquid Microextraction Based on the Solidification of a
Floating Organic Droplet Followed by GC. Chromatographia
2018, 81, 539–544. DOI: 10.1007/s10337-017-3457-1.
[282] Talaee, M.; Lorestani, B.; Ramezani, M.; Cheraghi, M.;
Jamehbozorgi, S. Microfunnel-Filter-Based Emulsification
Microextraction Followed by Gas Chromatography for Simple
Determination of Organophosphorus Pesticides in
Environmental Water Samples. J. Sep. Sci. 2019, 42,
2418–2425. DOI: 10.1002/jssc.201900132.
[283] Mohebbi, A.; Farajzadeh, M. A.; Mahmoudzadeh, A.; Etemady,
A. Combination of Poly (e–Caprolactone) Grafted Graphene
Quantum Dots–Based Dispersive Solid Phase Extraction
Followed by Dispersive Liquid–Liquid Microextraction for
Extraction of Some Pesticides from Fruit Juices Prior to Their
Quantification by Gas Chromatography. Microchem. J. 2020,
153, 104328. DOI: 10.1016/j.microc.2019.104328.
[284] Bazrafshan, A.; Ghaedi, M.; Rafiee, Z.; Hajati, S.; Ostovan, A.
Nano-Sized Molecularly Imprinted Polymer for Selective
Ultrasound-Assisted Microextraction of Pesticide Carbaryl
from Water Samples: Spectrophotometric Determination. J.
Colloid Interface Sci. 2017, 498, 313–322. DOI: 10.1016/j.jcis.
2017.03.076.
[285] Jouyban, A.; Farajzadeh, M. A.; Mogaddam, M. R. A. In
Matrix Formation of Deep Eutectic Solvent Used in Liquid
Phase Extraction Coupled with Solidification of Organic
Droplets Dispersive Liquid-Liquid Microextraction;
Application in Determination of Some Pesticides in Milk
Samples. Talanta 2020, 206, 120169 DOI: 10.1016/j.talanta.
2019.120169.
[286] Farajzadeh, M. A.; Asghari, A.; Feriduni, B. An Efficient,
Rapid and Microwave-Accelerated Dispersive Liquid–Liquid
Microextraction Method for Extraction and Pre-Concentration
of Some Organophosphorus Pesticide Residues from Aqueous
Samples. J. Food Compos. Anal. 2016, 48, 73–80. DOI: 10.
1016/j.jfca.2016.02.007.
[287] Shamsipur, M.; Yazdanfar, N.; Ghambarian, M. Combination
of Solid-Phase Extraction with Dispersive Liquid-Liquid
Microextraction Followed by GC-MS for Determination of
Pesticide Residues From Water, Milk, Honey and Fruit Juice.
Food Chem. 2016, 204, 289–297. DOI: 10.1016/j.foodchem.
2016.02.090.
[288] Liu, X.; Liu, C.; Qian, H.; Qu, Y.; Zhang, S.; Lu, R.; Gao, H.;
Zhou, W. Ultrasound-Assisted Dispersive Liquid-Liquid
Microextraction Based on a Hydrophobic Deep Eutectic
Solvent for the Preconcentration of Pyrethroid Insecticides

Prior to Determination by High-Performance Liquid
Chromatography. Microchem. J. 2019, 146, 614–621. DOI: 10.
1016/j.microc.2019.01.048.
[289] Zahiri, E.; Khandaghi, J.; Farajzadeh, M. A.; Mogaddam,
M. R. A. Combination of Dispersive Solid Phase Extraction
with Solidification Organic Drop-Dispersive Liquid-Liquid
Microextraction Based on Deep Eutectic Solvent for Extraction
of Organophosphorous Pesticides from Edible Oil Samples. J.
Chromatogr. A. 2020, 1627, 461390. DOI: 10.1016/j.chroma.
2020.461390.
[290] Zhao, W.; Jing, X.; Chang, M.; Meng, J.; Feng, C. Vortex-
Assisted Emulsification Microextraction for the Determination
of Pyrethroids in Mushroom. Bull. Korean Chem. Soc. 2019,
40, 943–950. DOI: 10.1002/bkcs.11850.
[291] Solaesa, A. G.; Fernandes, J. O.; Sanz, M. T.; Benito-Roman,
 Cunha, S. C. Green Determination of Brominated Flame
O.;
Retardants and Organochloride Pollutants in Fish Oils by
Vortex Assisted Liquid-Liquid Microextraction and Gas
Chromatography-Tandem Mass Spectrometry. Talanta 2019,
195, 251–257. DOI: 10.1016/j.talanta.2018.11.048.
CRITICAL REVIEWS IN ANALYTICAL CHEMISTRY 27
[292] Li, X.; Wang, M.; Zhao, J.; Guo, H.; Gao, X.; Xiong, Z.; Zhao,
L. Ultrasound-Assisted Emulsification Liquid Phase
Microextraction Method Based on Deep Eutectic Solvent as
Extraction Solvent for Determination of Five Pesticides in
Traditional Chinese Medicine. J. Pharm. Biomed. Anal. 2019,
166, 213–221. DOI: 10.1016/j.jpba.2019.01.018.
[293] Yao, F.; Song, Z.-Y.; Nie, J.; Li, Z.-G.; Zhu, G.-H.; Lee, M.-R.
Development of a Microextraction Method Based on
Dissolved Carbon Dioxide Flotation after Emulsification for
the Determination of Triazole Pesticides Residues in Water
Samples by Gas Chromatography-Mass Spectrometry. Anal.
Sci. 2016, 32, 1083–1088. DOI: 10.2116/analsci.32.1083.
[294] El-Deen, A. K.; Shimizu, K. Application of D-Limonene as a
Bio-based Solvent in Low Density-Dispersive Liquid-Liquid
Microextraction of Acidic Drugs from Aqueous Samples. Anal.
Sci. 2019, 35, 1385–1391. DOI: 10.2116/analsci.19P360.
[295] Lu, D.; Liu, C.; Deng, J.; Zhou, X.; Shi, G.; Zhou, T. Rational
Design of an Ionic Liquid Dispersive Liquid-Liquid Micro-
Extraction Method for the Detection of Organophosphorus
Pesticides. Analyst 2019, 144, 2166–2172. DOI: 10.1039/
c9an00123a.