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Methods of Pesticide Residue Analysis

Article  in  Journal of AOAC International · September 2012

DOI: 10.5740/jaoacint.SGE_Tuzimski_intro · Source: PubMed

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Tomasz Tuzimski
Medical University of Lublin
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1256  Tuzimski: Journal of AOAC International Vol. 95, No. 5, 2012
SPECIAL GUEST EDITOR SECTION
Methods of Pesticide Residue Analysis
T he determination of pesticide
residues in a wide variety
of matrixes is a formidable
challenge mainly because of the small
quantities of analytes and large amounts
of interfering substances that can be
coextracted with the analytes and,
in most cases, adversely affect the
results of the analysis. However, safety
considerations require that pesticides of
the wide range of chemical properties
should be monitored. That is why
analytical chemists are faced with the
need to devise new methodologies for
determining such residues in a single
analytical run. Many of these topics are
covered in this special issue, composed
of three reviews and 10 experimental
papers.
Sample preparation is a very
important part of the analytical method
because the sample must initially be
cleaned up before a final analysis.
Due to the low levels of pesticides
that may be found in environmental
samples, the analyte concentration must
be enriched before its instrumental
determination. The first review by
Tadeo et al. (paper 1) includes the main
extraction and cleanup procedures
applied to the analytical determination
of pesticides in soil samples based
on differences in their chemical and
physical properties (solubility, polarity,
molecular weight, and volatility). The
review covers important aspects of
pesticide analysis, including classical
and modern extraction methods and
new sample preparation techniques
(e.g., QuEChERS: Quick, Easy, Cheap,
Effective, Rugged, and Safe).
The second review paper by
Abdulra’uf et al. covers the modes and
types of solid phase microextraction
(SPME) techniques including fiber
types, optimization of extraction
conditions, calibration methods, and
the various analytical instruments used
in application of the technique for
determination of pesticide residues in
fruits and vegetables.
DOI: 10.5740/jaoacint.SGE_Tuzimski_intro
Paper 3 by Beceiro-González et al.
reviews the applicability, advantages,
and disadvantages of various traditional
and new sample preparation techniques
for the determination of organochlorine
pesticides in a wide range of vegetation
samples—different plants and plant
materials.
The experimental papers illustrate
new directions and applications of
pesticide residue analysis and include
some original, recent methodologies
(e.g., QuEChERS) and separation
mechanisms [e.g., hydrophilic
interaction chromatography (HILIC)].
For these reasons the special section
has a high degree of novelty. Paper 4
by Geis-Asteggiante et al. describes
the testing of three different variations
in the QuEChERS method: (1) using
anhydrous MgSO4 ≥99% purity in
the extraction step, as applied in most
QuEChERS commercial products;
(2) using anhydrous MgSO4 ≥97%
purity in the extraction step; and (3)
using anhydrous MgSO4 ≥99% with
an ice bath for lowering the extraction
temperature. The authors evaluated
the effect of temperature and purity of
anhydrous MgSO4 during extraction by
comparing recoveries of 38 pesticide
residues in limes and broccoli. For
analysis they used LC/electrospray
ionization-triple quadrupole
MS/MS, and programmable temperature
vaporization injection, and speed
GC/MS/MS with low pressure and an
analyte protectant mixture that included
shikimic acid.
Garrido Frenich et al. (paper 5)
describe a multiresidue method to
determine 84 pesticides in potato and
carrot samples by ultra performance
liquid chromatography (UPLC)
coupled to MS/MS, with the use of a
QuEChERS sample preparation method.
Ðurović et al. (paper 6) present
a multiresidue method for the
determination of five pesticides
belonging to different pesticide groups
in soil samples, based on a combination
of liquid-solid sample preparation
followed by a headspace SPME method.
Tomasz Tuzimski
Special Guest Editor
After optimization of microextraction
conditions, the described method
was satisfactory for quick pesticide
screening in contaminated soil samples
by a high-throughput laboratory.
Paper 7 by Aquino et al. reports
an investigation of potential metal-
organic frameworks materials, which
were tested as adsorbents for matrix
solid-phase dispersion extraction and
applied to the multiclass analysis
of pesticides in dehydrated Hyptis
pectinata medicinal plant. The proposed
material can be successfully used for
the determination of pesticides in the
medicinal plant. A comparison of the
results with C18-bonded silica showed
good accordance and indicated no
significant difference in accuracy and
precision.
Ozcan et al. (paper 8) describe the
application of a novel SPE method in
the determination of organochlorine
pesticides in environmental water
samples by the use of Fe3O4-magnetic
nanoparticles coated with oleic acid
followed by GC/mass selective
detection-MS. The new method was
found to be a useful alternative to
conventional SPE for the extraction of
nonpolar pollutant compounds from
water samples.
Raina and Smith (paper 9) describe
a column LC/MS/MS method for the
determination of azole fungicides

in the atmosphere at low pg/m3
concentrations. The paper reports
the first detection of propiconazole,
prothioconazole-desthio, and trace
levels of hexaconazole in gas phase
atmospheric samples collected in a
Canadian agricultural region.
Paper 10 by Tuzimski shows the
potential of RP-HPLC with a diode
array detector (DAD) after ultrasound-
assisted solvent extraction and SPE
for the determination of pesticides
in food samples. The application of
HPLC-DAD after SPE for identification
and quantitative analysis of selected
pesticides from different chemical
groups, i.e., metamitron, metalaxyl,
linuron, and prometryn, in red and green
pepper samples is demonstrated. The
method was validated for precision,
repeatability, and accuracy.
Paper 11 by Noga et al. presents a
study of the retention of fungicides on
different polar stationary phases as a
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Tuzimski: Journal of AOAC International Vol. 95, No. 5, 2012  1257
function of the mobile phase solvent
acetonitrile concentration in the per
aqueous LC and HILIC systems. This
excellent paper includes different
parts with clear-sighted studies, e.g.,
selectivity of different HILIC phases
and effects of the mobile phase on
separation.
HPTLC using a multienzyme
inhibition assay for the determination
of organophosphorus and carbamate
insecticides in fresh fruits and
vegetables down to their maximum
residue limits as recorded by the
European Union is excellently described
by Akkad and Schwack (paper 12).
Paper 13 by Bojanowska-Czajka et
al. shows that radiolytic decomposition
of parathion seems to be an attractive
alternative to other developed advanced
oxidation processes for decomposition
of this pesticide for environmental
protection. This study examined the
decomposition of parathion in aqueous
solutions by gamma radiation in
different conditions. The samples were
analyzed, and amounts of residual
parathion and intermediate products
were monitored using LC and GC
methods. Qualitative determinations
were carried out with GC/MS after SPE.
As the Guest Editor of this special
section, I would like to thank all
the authors, known specialists who
contributed papers for completion of
this project; the reviewers for their
valuable work; Joseph Sherma, the
Acquisition Editor of the Journal of
AOAC International; and, last but
not least, the editorial staff of AOAC,
in particular Catherine Wattenberg,
Jennifer Diatz, and Robert Rathbone for
their assistance.
—Tomasz Tuzimski
Department of Physical Chemistry
Medical University of Lublin, Poland