This method reports on in-house validation results and
assessment of performance parameters of a complete
multi-residue pesticide analysis method employing
QuEChERS sample preparation kits, sample measure-
ment by the newly developed Thermo Scientific
™
TSQ
™
8000 Pesticide Analyzer system and rapid data analysis
by Thermo Scientific
™
TraceFinder
™
software.
3. Scope
The objective of this validation study was to prove a
complete workflow solution (delivered by Thermo
Scientific chemicals, consumables and instrumentation)
that can be implemented for routine multi-residue
pesticide analysis (approximately 140 priority pesticides)
in representative matrices (strawberry, wheat flour and
leek). This was achieved in accordance with current
legislation requirements, demonstrating that sensitivity
of the assay conforms with the MRL values at the limits
of detection (LOQ).
1-4
4. Principle
Sub-portions of previously homogenized (for some instable
compound cryogenic milling is recommended) samples
were treated according to a standard QuEChERS
method protocol (extraction and clean-up) prior to
injection in the TSQ 8000 Triple-Stage Quadrupole
GC-MS system.
5, 6
Ready to use QuEChERS kit containing both extraction
and clean-up tubes and associated protocol were used for
sample preparation (Thermo Fisher Scientific, Runcorn
UK). Identification of pesticide residues was based on
retention time and ion-ratio confirmation using selective
reaction monitoring (SRM) of characteristic transition
ions, while quantification was calculated on matrix
matched calibration and internal standardization. All
method performance criteria were established according
to the relevant guidelines.
1-4, 7
5. Reagent List
Part Number
5.1 Acetone, HPLC Grade
A/0606/17
5.2 Acetonitrile, LC-MS Grade
A/0638/17
5.3 Methanol, Optima LC-MS grade
A456-212
5.4 Toluene, HPLC grade
T/2200/08
5.5 Water, LC-MS grade
W/0112/17
5.6 Sorbitol, 500 g
10396733
6. Standard List
6.1 Pesticides
All individual pesticide compounds – Acephate, Acrinathrin,
Amitraz, Azinphos-methyl, Azoxystrobin, Bifenthrin,
Bitertanol, Boscalid, Bromopropylate, Bromuconazole,
Bupirimate, Buprofezin, Cadusafos, Captan, Carbaryl,
Carbofuran, Carboxin, Chlorfenapyr, Chlorfenvinphos,
Chlorobenzilate, Chlorothalonil, Chlorpropham,
Chlorpyrifos-ethyl, Chlorpyrifos-methyl, Cyfluthrin,
Cyhalothrin, Cypermethrin, Cyproconazole, Cyprodinil,
DDD, DDE,DDT, Deltamethrin, Demeton-S-methyl,
Diazinon, Dichlofluanid, Dichloran, Dichlorbenzophenon,
Dichlorvos, Dicofol, Difenoconazole, Dimethoate,
Dimethomorph, Diphenylamine, Endosulfan, Endosulfan
sulfate, EPN, Epoxiconazole, Ethion, Ethoprop (Ethop-
rophos), Etofenprox, Fenamiphos, Fenamiphos sulfone,
Fenamiphos-sulfoxid, Fenarimol, Fenbuconazol,
Fenitrothion, Fenoxycarb, Fenpropathrin, Fenpropidin,
Fenpropimorph, Fenthion, Fenvalerate, Fipronil,
Fludioxonil, Fluquinconazole, Flusilazole, Flutolanil,
Flutriafol, Fluvalinate, Folpet, HCH alpha, HCH beta,
HCH gamma Lindane, Hexaconazole, Imazalil,
Iprodione, Isofenphos-methyl, Kresoxim-methyl, Linuron,
Malathion, Mepanipyrim, Metalaxyl, Methacrifos,
Methamidophos, Methidathion, Methiocarb, Metribuzin,
Monocrotophos, Myclobutanil, Ortho-phenylphenol,
Oxadiazon, Oxadixyl, Paclobutrazol, Paraoxon-methyl,
Parathion (ethyl), Parathion-methyl, Pendimethalin,
Permethrin, Phenthoate, Phosalone, Phosmet, Phos-
phamidon, Pirimicarb, Pirimicarb-p-desmetyl,
Pirimiphos methyl, Prochloraz, Procymidone, Profenofos,
Propargite, Propiconazole, Propyzamide, Prothiofos,
Pyraclostrobin, Pyridaben, Pyrimethanil, Pyriproxyfen,
Quinoxyfen, Spirodiclofen, Tebuconazole, Tebufenocide,
Tebufenpyrad, Tefluthrin, Tetraconazole, Tetradifon,
Tetrahydrophthalimide, Thiabendazole, Tolclofos-methyl,
Tolyfluanid, Triadimefon, Triadimenol, Trifloxystrobin,
Trifluralin, Triticonazole, Vinclozolin) were obtained from
Sigma-Aldrich
®
(Germany) and Laboratory Instruments
Srl (CASTELLANA GROTTE, Italy).
6.2 Internal standards
1-bromo-4-fluorobenzene (BFB), triphenylphosphate
(TPP) (both from Sigma-Aldrich, Germany)
6.3 Quality Control Materials
FAPAS #19140QC (lettuce), FAPAS #19141QC (green
bean) and FAPAS #19142QC (melon puree)
Note: FAPAS samples were selected primarily on content of target pesticides. However,
due to limited availability, matrices are slightly different from the validated matrices.
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