Environ Monit Assess (2012) 184:5821–5828
DOI 10.1007/s10661-011-2384-0
A simple and efficient multi-residue method based
on QuEChERS for pesticides determination
in palm oil by liquid chromatography
time-of-flight mass spectrometry
Elham Sobhanzadeh & Nor Kartini Abu Bakar &
Mhd Radzi Bin Abas & Keivan Nemati
Received: 26 October 2010 / Accepted: 16 September 2011 / Published online: 12 October 2011
# Springer Science+Business Media B.V. 2011
Abstract In this study, a rapid, specific and sensitive
multi-residue method based on acetonitrile extraction
followed by dispersive solid-phase extraction (d-SPE)
clean-up was implemented and validated for multi-
class pesticide residues determination in palm oil for
the first time. Liquid–liquid extraction followed by
low-temperature precipitation procedure was evaluat-
ed in order to study the freezing-out clean-up
efficiency to obtain high recovery yield and low co-
extract fat residue in the final extract. For clean-up
step, d-SPE was carried out using a combination of
anhydrous magnesium sulphate (MgSO4), primary
secondary amine, octadecyl (C18) and graphitized
carbon black. Recovery study was performed at two
concentration levels (10 and 100 ng g−1), yielding
recovery rates between 74.52% and 97.1% with
relative standard deviation values below 10% (n=6)
except diuron. Detection and quantification limits
were lower than 5 and 9 ng g−1, respectively. In
addition, soft matrix effects (≤±20%) were observed
for most of the studied pesticides except malathion
that indicated medium (20–50%) matrix effects. The
proposed method was successfully applied to the
analysis of suspected palm oil samples.
E. Sobhanzadeh (*) : N. K. Abu Bakar : M. R. Bin Abas :
K. Nemati
Environmental Research Group, Department of Chemistry,
University of Malaya,
Kuala Lumpur 50603, Malaysia
e-mail: elham.sobhanzadeh@yahoo.com
Keywords Multi-residue pesticides . d-SPE . Palm
oil . LC-TOF-MS
Introduction
Palm is one of the most important agricultural crops in
terms of production and applications. Palm oil (Elaeis
guineensis) is a very common cooking ingredient in
Southeast Asia and the tropical belt of Africa. Its
increasing use in the commercial food industry in
other parts of the world is due to the high oxidative
stability of the refined product and its application in
various areas such as medicine. Malaysia is not only
one of the leading countries in exporting palm fruit
but also is the largest exporter of palm oil in the
world. According to the World Bank and the Asian
Development Bank, Malaysia is the world’s second
largest palm oil producer (Ong and Goh 2002).
Palm trees are attacked by a variety of pests and
unwanted plants that could reduce the quality and
quantity of the palms used to produce palm oil. In this
respect, the extensive use of pesticides has played an
important role to control or prevention of these pests
and harmful plants as well as to increase the world
palm oil production. On the other hand, the use of
pesticides in agricultural production has acute toxicity
towards human and animal bodies. Exposure to the
hazardous pesticides is a concern of the general
population, especially the agricultural population and
5822
residents living near industrial or contaminated areas
(Lambropoulou and Albanis 2007). Therefore, the
excessive use of pesticides often leads to residues
heavily going beyond the limits. Even when applied
in accordance with Good Agricultural Practices, they
can leave residues, which can be detrimental to food
safety (Lentza Rizos et al. 2001). Therefore, it is very
important to carry on the inspection and control of
pesticide residues. The Codex Alimentarius Com-
mittee on Pesticide residues and the Joint FAO/
WHO Meeting on Pesticide Residues have estab-
lished maximum pesticide residue limits for some
of the pesticides in palms destined for oil
production (Codex Alimentarius Committee on
Pesticide Residues 2009). However, it should be
noted that there are no harmonized maximum residue
limits (MRLs) established for pesticide residues in
palm oil yet. But the National Committee on
Agricultural Commodity and Food Standards (2008)
issued a notification entitled the Thai Agricultural
Standards on Pesticide Residues: Maximum Residue
Limits (TAS 9002-2008) for palm oil on 31 July 2006
which was published in the Royal Gazette (Thai
Agriculture Standard, TAS 9002-2008).
High-fat food samples such as palm oil represent a
particular analytical challenge for pesticide residue
analysis due to the inherent complexity of the matrix
that may have an adverse affect on the results of
analysis. Modern trends in analytical chemistry are
towards the simplification and miniaturization of
sample preparation methods to save time, chemicals
and analysis cost, as well as to increase the sample
throughput and improve the quality and sensitivity of
analytical methods, and if possible to hyphenate the
different steps of the analytical process. Despite gas
chromatography–mass spectrometry (GC–MS) has
been the technique of choice for pesticide residue
analysis in fruits and vegetables (including those with
high fat content) (Garrido-Frenich et al. 2007;
Guardia-Rubio et al. 2006; Agüera et al. 2002;
Esteve-Turrillas et al. 2005; Ueno et al. 2004), the
number of polar and therefore non-GC-amenable
pesticides used in olive harvesting is increasing and
even bigger than those amenable by GC (Alder et al.
2006). Many sample preparation techniques for the
extraction of pesticides from vegetable oils especially
olive oil and even soybean oil prior to chromato-
graphic separation have been developed. Among
these, the most commonly used methodology is based
Environ Monit Assess (2012) 184:5821–5828
on gas chromatography (GC) after a comprehensive
clean-up step, in most cases based on liquid–liquid
partitioning extraction with solvents of different
polarity (Lentza Rizos et al. 2001); gel permeation
chromatography (GPC) (Guardia-Rubio et al. 2006);
microwave-assisted extraction (Fuentes et al. 2008);
solid-phase extraction (SPE) (Chen et al. 2009);
matrix solid-phase dispersion (MSPD) (Qi 2010;
Sobhazadeh et al. 2011); solid-phase microextraction
(Ravelo-Pérez et al. 2008) and quick, easy, cheap,
effective, rugged and safe (QuEChERS) (Hernández-
Borges et al. 2009).
Up to now, a limited number of analytical methods
for the detection of pesticides in palm oil samples
have been published. Liquid–liquid partitioning with
acetonitrile followed by low-temperature clean-up in
order to precipitation of lipid has been reported for
determination of the herbicides fluroxypyr, and also
chlorpyrifos and organochlorine pesticides in crude
palm oil and crude palm kernel oil (Halimah et al.
2004; Yeoh et al. 2006; Muhamad et al. 2008).
Recently, quick, easy, cheap, rugged, effective and
safe (QuEChERS) sample preparation approach,
which was firstly established by Anastassiades et al.
(2003), has been grown in popularity among pesticide
residue scientists due to its inherent advantages such
as speed, low cost and wide applicability. In this
method, pesticides are extracted with acetonitrile,
water is removed by salting out and the acetonitrile
extract is cleaned up by mixing with an SPE sorbent
rather than passing it through an SPE column. This
method provides a highly streamlined sample prepa-
ration method with excellent results for a wide range
of pesticide analytes in many types of foods. Unlike
many previous methods developed for traditional
chromatographic detection systems (e.g. UV/vis
absorbance, fluorescence, element-selective detectors),
the QuEChERS approach takes advantage of the wide
analytical scope and high degree of selectivity and
sensitivity provided by gas and liquid chromatography
(GC and LC) coupled to mass spectrometry (MS) for
detection (Lehotay et al. 2010).
To the best of our knowledge, no application of the
QuEChERS method to the analysis of pesticides in
palm oil samples has been published, although it is
currently being used in analytical laboratories for their
analysis. Therefore, the aim of this study was to
validate the efficient, sensitive and interference-free
method in combination with liquid chromatography
Environ Monit Assess (2012) 184:5821–5828 5823

electrospray time-of-flight mass spectrometry for the degasser, an autosampler and a binary pump-SL;
determining pesticides in palm oil. For this purpose, Agilent Technologies 1200 Series) equipped with a
QuEChERS method was evaluated in terms of reversed phase resolution C18 analytical column of
cleanliness of the extracts, efficiency of the extraction 50×2.1 mm and 1.8 μm particle size (Zorbax Eclipse
(recoveries), analytical performance, matrix effects SB-C18). Column temperature was maintained at 40°
and sensitivity (limits of detection) for analyses of C. The injected sample volume was 5 μL in each
multi-residue pesticides in palm oil samples collected study. In electrospray positive ionization mode,
from local markets in Kuala Lumpur, Malaysia. mobile phases A and B were acetonitrile and water
with 0.1% formic acid, respectively. The optimized
chromatographic method held the initial mobile phase
Experimental procedures
composition (10% A) constant for 5 min, followed by
a linear gradient to 100% A after 30 min. The flow
Pesticide standards and reagents
rate was optimized at 0.25 mL/min. A 10-min post-
run time was used after each analysis. This HPLC
The analytical pesticide standards—simazine, terbu-
system was connected to a time-of-flight mass
thylazine, atrazin, diuron, dimethoate, malathion
spectrometer, Agilent MSD TOF (Agilent Technolo-
and carbaryl—were obtained from Fluka (Buchs,
gies, 6,530 Accurate Mass TOF), equipped with an
Switzerland, HPLC grade 99.9%). Individual
electrospray interface operated in positive ion, using
pesticide stock solutions of the above analytes at
the following operation parameters: capillary voltage,
1.0 mg mL−1 were prepared in pure methanol and
4,000 V; nebulizer pressure, 40 psig; drying gas, 9 L/
maintained in amber-coloured bottles at 4°C. They
min; gas temperature, 300°C; fragmentor voltage (n
were kept for 2 h at ambient temperature prior to
source CID fragmentation), 190 V; skimmer voltage,
their use. Working standard solutions of a mixture
65 V and octopole RF, 750 V. LC/MS accurate mass
of pesticides were prepared by appropriate dilu-
spectra were recorded across the range 50–1,000m/z.
tions in methanol and stored at −20°C. HPLC-
The instrument performed the accurate-mass internal
grade acetonitrile (MeCN) and methanol (MeOH)
mass calibration automatically using a dual-nebulizer
were purchased from Merck (Darmstadt, Germany).
ion source combined with an automated calibrant
Reagent grade anhydrous magnesium sulphate and
delivery system, which introduced the internal.
sodium chloride were purchased from Sigma-
Aldrich (St. Louis, MO, USA). PSA sorbent was
Sample preparation
purchased from Sigma-Aldrich (SPE bulk packing,
50 μm). C18 sorbent (50 μm) and GCB cartridges
A representative 3 g portion of palm oil was weighed
with a configuration of 500 mg/6 mL were from
into a 50-mL polypropylene centrifuge tube with 7 g of
Alltech Inc. A Milli-Q-Plus ultrapure water system
water. Then, 10 mL of acetonitrile was added, along
from Millipore (Milford, MA) was used throughout
with 4 g of anhydrous magnesium sulphate and 1 g of
the study to obtain the HPLC-grade water used during
sodium chloride, and immediately, the tube was
the analyses. As pre-treatment prior to liquid chro-
vigorously shaken for 1 min to prevent coagulation of
matography time-of-flight mass spectrometry (LC-
MgSO4. The extract then was centrifuged (4,000 rpm)
TOF-MS) analysis, the oil samples were merely
for 1 min. For the freezing-out clean-up, the obtained
filtered through a 0.22-μm filter (Chromatography
extracts were horizontally stored in freezer at −20°C
Research Supplies).
for 2 h. The organic phase containing the organic
Various commercial brands of palm oil were
solvent and extracted compounds remained liquid and
purchased from local supermarkets in Kuala Lumpur,
rose to the top, whereas the oil was frozen and
Malaysia.
precipitated to the bottom of the tubes. About 5 mL of
the extract was then separated from the precipitates by
Apparatus and conditions decantation and filtration into a PTFE centrifuge tube
containing 750 mg of anhydrous magnesium sulphate,
The separation of the selected pesticides was carried out 250 mg of PSA sorbent, 250 mg of C18 sorbent and
using an HPLC system (consisting of a vacuum 250 mg of GCB sorbent. After shaking for 30 s, the
5824
contents in the tube were centrifuged at 4,000 rpm for
1 min. Three millilitres of the supernatant was then
evaporated to near dryness and reconstituted in 1 mL to
a final composition of 20% MeOH in water (similar
organic solvent percentage as that of the initial mobile
phase, 10% MeCN), and then the extract was filtered
through a 0.22-μm PTFE filter prior to LC/MS analysis.
Spiking procedure
For recovery studies, the samples were spiked with the
studied pesticides before the corresponding extraction
procedure. A representative 100 g portion of palm oil
sample was weighted and fortified homogeneously with
different volumes of working standard solution to reach
10 and 100 ng g−1 of the studied pesticides in the
spiked sample. The mixture was then gently blended
in the mortar for 1 h in order to assess the
homogeneity of the sample. Then, the sample was
incubated at room temperature for 6 h in order to
make sure the solvent was completely evaporated.
Result and discussion
Evaluation of sample treatment procedure
In this study, different pesticides used in the agricultural
process containing dimethoate, carbaryl, simazine,
atrazine, terbuhylazine, diuron and malathion were
chosen among different classes of compounds (organo-
phosphates, carbamates, triazines and phenylureas).
Due to the inherent complexity of the high fatty
matrix, the main challenge in developing the clean-up
method is the separation of co-extracted fatty matrix
from the pesticides of interest. In this study, liquid–
liquid extraction (LLE) using acetonitrile with low-
temperature precipitation followed by dispersive
solid-phase extraction (d-SPE) clean-up was evaluat-
ed for multi-residue pesticide analysis in palm oil.
Low-temperature precipitation method was performed
to decrease the amount of fatty co-extractants with
limited solubility in cold acetonitrile (Lentza Rizos et
al. 2001; Li et al. 2007; Goulart et al. 2008; Chen et
al. 2009). This clean-up method has some profits such
as simplicity of operation, rapid sample throughput
without any special required equipment. The acetoni-
trile extract obtained from LLE step was poured into
the glass test and horizontally stored in the freezer at
Environ Monit Assess (2012) 184:5821–5828
−20°C for 4 h. The organic phase containing the
organic solvent and extracted compounds (pesticides
interest) remained liquid and rose to the top, whereas
lipids were frozen and precipitated as frozen in the
bottom of the tubes. The cold extract containing
precipitated lipids was immediately filtered through a
cotton wool plug to prevent lipids from melting. After
evaporation of the extracts, the remaining matrix
constituents were weighted to evaluate the efficiency
of the extraction. The mean value (n=3) of the
remaining fat in the extract after LLE with acetoni-
trile, expressed as milligrams per gram of palm oil
extracted was found to be 3.2±0.6 mg g−1, whereas
the residue fat in the extracts after freezing-out was
found to be 0.30±0.08 mg g−1. The result showed that
freezing-out procedure was able to remove 90.6% of
lipid from the matrix. Since remaining matrix constitu-
ents would possibly interfere with the determination and
deteriorate the LC-TOF-MS system performance, an
additional dispersive solid-phase extraction (d-SPE)
clean-up is necessary. Comparative study between two
chromatograms obtained from the extracts after only
freezing-out clean-up and additional d-SPE showed
some chromatographic problems such as peak suppres-
sion of dimethoate and retention time shifts of the
dimethoate, simazine and malathion (see Fig. 1).
The proposed methodology here (dispersive SPE
clean-up procedure) is different with the protocol used
in classical QuEChERS for fruits and vegetables
(Anastassiades et al. 2003). Because of the fatty
composition of the matrix, the use of additional
sorbents (PSA, GCB, C18) and magnesium sulphate
anhydrous in the clean-up step (Cunha et al. 2007) is
necessary. The PSA is known to exhibit a strong
retaining activity for sugars, fatty acids and other
organic acids, GCB for planar molecules such as
pigments (chlorophyll and carotenoids), as well as
sterols; however, C18 has strong affinity for fats and
lipids (Lehotay et al. 2005).
An aliquot of the obtained extract from the freezing-
out step was separated from the precipitates by
decantation and filtration into a PTFE centrifuge tube
containing 750 mg of anhydrous magnesium sulphate,
250 mg of PSA sorbent, 250 mg of C18 sorbent and
250 mg of GCB sorbent, as we described in “Sample
preparation” and then analysed by LC/MS.
To evaluate the effectiveness of the extraction
method, different recovery studies were carried out.
In this case, untreated palm oil samples were spiked
Environ Monit Assess (2012) 184:5821–5828 5825

Fig. 1 Effect of clean-up on peak shape and retention time of a dimethoate, b simazine and c malathion

with appropriate volumes of composite working Method validation

standard solution at two different concentration levels:
10 and 100 ng g−1. As shown in Table 1, all pesticides The analytical performance of the proposed method
assayed fell within the acceptable range from 74.52% was studied in order to evaluate its usefulness for
to 97.1% with relative standard deviation (RSD) quantitative determination of pesticide residues in
values below 10% (n=6) except diuron. These results palm oil extract. The use of matrix-matched standards
evidence the feasibility of the studied extraction provides reliable quantitation capabilities for food
method. The obtained low recovery for diuron (with analyses (Ferrer et al. 2005). Palm oil matrix-matched
average recovery of 54.2%) indicated that this standard solutions were prepared using proposed
compound was not completely retained in the GCB sample treatment method by adding appropriate
phase during the clean-up procedure. This may be due amounts of working standard solution to the obtained
to the planar structure of diuron. extracts in order to obtain the desired concentration
range. Blank extracts of palm oil matrix were also
Table 1 Recovery studies on palm oil extracts spiked with the
measured.
pesticide mixture at two concentration levels of 10 and Linearity was estimated by analysing these matrix-
100 ng g−1 matched standard solutions prepared at different
concentration levels in the range of 2–500 ng g−1.
Mean recovery±RSD (%)
The slope and intercept values, together with relative
Pesticide Concentration level (ng g−1) standard deviations, were estimated using regression
analyses. The responses of all compounds were linear
10 μg kg−1 100 μg kg−1 in the range under study with the regression coef-
Rec±RSD (%)a Rec±RSD (%)a
ficients (R2) higher than 0.9986.
Dimethoate 88.31±6.03 93.08±7.60 The instrumental limit of detection (LOD) and
Simazine 74.52±5.18 91.23±8.32 limits of quantification (LOQ) of the prepared in
Carbaryl 84.72±4.05 88.05±6.91 overall method were estimated for signal-to-noise
Atrazine 89.33±7.12 92.65±9.75 ratio of 3 (S/N=3) and 10 (S/N=10), respectively,
Diuron 51.62±8.24 57.08±8.11 measured by peak-to-peak method at the lowest
Terbuthylazine 76.47±4.60 86.74±7.54
calibration level. These LOD and LOQ levels are
Malathion 90.85±6.27 97.10±9.05
considerably low since they are far below the
maximum residue level regulations established for
a
n=6 selected pesticides in this study. These results
5826 Environ Monit Assess (2012) 184:5821–5828

Table 2 Retention times, MS ions (m/z), method precision expressed as the average standard deviation (RSD%), calibration data, matrix effects expressed as the ratio between the

LOQ (ng g−1)

demonstrate the high sensibility of the proposed

6.6
2.5
3.2

2.8
3.2
method based on low temperature followed by d-

9
SPE clean-up and LC-TOF-MS for the detection and
quantification of the selected pesticides in palm oil.

LOD (ng g−1)

The obtained values are summarized together with

calibration curve slopes of matrix-matched standards and solvent-based standards, LOD and LOQ of the pesticides analysed in palm oil sample by LC-TOF-MS
intra- and inter-day %RSD in Table 2. The relative

0.6
0.8
2
1
1

1
5
standard deviation (RSD) (n=6) values for run-to-run
studies (running in single day) were in the range 3.6–
8.5% and inter-day (running within 6 days) RSD (n=

Inter-day

6.3
4.2

4.9

7.5
5.8
10.4

10.2
6) values were between 4.2% and 10.4%, which

RSD (%) n=6

indicated that the present method provides a reason-
able precision for selected pesticides. The typical

Intra-day

4.7
3.8
8.1
3.6
8.5
5.0
4.1
chromatograms obtained by LC-TOF-MS for both,
spiked palm oil and blank palm oil extract sample are

−4.21
−3.06
+13.65

+17.02
+16.56
−22.45
+0.58
shown in Fig. 2.

(Δ%)
Matrix effects

(Slope M/slope St)a

Matrix components can provide variation in the

Matrix effect

1.006
1.14

0.96
0.97
1.17
1.17
0.77
detector response to pesticides. Matrix effect can
reduce or enhance the response of the detector, and it
can be evaluated by comparing the detector response
for pesticide standards prepared in solvent with that
Linearity (R2)

for standards prepared in sample extract. In this study,

0.9986
0.9991
0.9992
0.9991
0.9987
0.9990
0.9994
these possible effects were evaluated by comparing
the slopes obtained in the calibration with matrix-
matched standards and those obtained with solvent-
MRL (ng g−1)b

Ref. (National Bureau of Agricultural Commodity and Food Standards 2008)

based standards, to calculate matrix/solvent slope

bold font = m/z ions selected for quantification and confirmation of pesticides
100
50

20
nr

nr
nr

nr
ratio for each pesticide (see Table 2). A value <1
indicates signal suppression due to the matrix, while
values >1 involve enhancing effect of the matrix on
170.9694, 124.9778

127.0354, 124.9810

analyte signal. Regarding to the obtained result in

Table 2, quantitation of pesticides was performed with
matrix-matched calibration, using the same matrix as Percentage of signal enhancement (+) or suppression (−)
132.0323

72.0444

the sample analysed.

The percentages of signal suppression or enhance-
ment (calculated by formula: matrix/solvent slope
202.0854, 174.0541,
230.0063, 198.6910,

233.0243, 255.0063,

331.0397, 284.9880,
202.0865, 145,0485
216.1010, 174.0541

230.1167, 174.0541

ratio×100−100) are also shown in Table 2. Depend-

ing on the decrease/increase in the percentage of the
slope, different matrix effect could be observed.
Negative values indicate signal suppression of the
m/z

matrix, while positive results show enhancement due

to the matrix. The obtained positive values in more
tR (mm)

14.275
17.622
20.015
20.123
20.648
22.747
24.879

cases showed an enhancement signal for palm oil

extracts, whereas, carbaryl, atrazine and malathion
nr non-reported
Terbuthylazine

indicated signal suppression. The overall results

Dimethoate

Malathion
Simazine
Carbaryl
Atrazine
Diuron

showed the matrix effects less than ±20% signal

Pesticide

enhancement and suppression in most cases except

malathion (−22.45%). Therefore, low-temperature
b
a
Environ Monit Assess (2012) 184:5821–5828
Fig. 2 a Total ion chromatogram (TIC) corresponding to the
LC-TOF-MS analysis of palm oil sample spiked with 50 ng g−1
of pesticides. b The extracted ion chromatogram (XIC) for the
precipitation followed by d-SPE clean-up procedure
can be effective to remove interfering species from
the palm oil samples.
Application of the method to real samples
Three different brands of palm oil samples purchased
from local supermarkets in Kuala Lumpur, Malaysia
were sampled and analysed following the purposed
sample preparation method for the determination of
seven multi-class pesticide residues. Positive findings of
dimethoate and malathion were found in the samples
with a concentration of 1.5 ng g−1 and 3.5 ng g−1, lower
than the obtained detection limit for these pesticides.
The results showed that no pesticide residues at
concentrations above the detection limit and the
permitted MRL published by Thai Agricultural Stand-
ards on Pesticide Residues (TAS 9002–2008) for
palm oil (National Bureau of Agricultural Commodity
and Food Standards 2008).
5827
corresponding protonated molecules of pesticides. c Typical
chromatograms obtained by LC-TOF-MS of blank palm oil
extract sample
Conclusions
In this work, an efficient, fast, economical and
environmental friendly sample preparation method
based on freezing-out and QuEChERS method was
successfully evaluated to determine seven multi-
residue pesticides in palm oil. The obtained
satisfactory results from analytical performance
parameters such as linearity, precision, accuracy,
and detection and quantification limits illustrated
the potential of LC-TOF-MS for the rapid analysis
of the targeted pesticides in palm oil samples. For
quantitative evaluation, matrix effects were evalu-
ated by comparing the slopes of the matrix-
matched and solvent-based calibration curves. The
minor effects were observed by most of pesticides
studied. In addition, the purposed method offers
considerable saving in terms of solvent consump-
tion, cost of materials, sample manipulation and
analysis time.
5828
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