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Evaluation of Low-Pressure Gas Chromatography-Tandem Mass Spectrometry Method for the Analysis of > 140 Pesticides in Fish

Sapozhnikova, Yelena
Journal of agricultural and food chemistry 2014 v.62 no.17 pp. 3684
DDD (pesticide), trifluralin, trans-chlordane, tandem mass spectrometry, solid phase extraction, pesticide residues, multiresidue analysis, mirex, markets, lindane, hexachlorobenzene, heptachlor, gas chromatography, dimethoate, detection limit, chlorpyrifos, catfish, acetonitrile, DDT (pesticide), DDE (pesticide), chlordane, food analysis, food contamination, mass spectrometry
A multiresidue method for the analysis of 143 pesticide residues in fish was developed and evaluated using fast, low-pressure gas chromatography/triple-quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) cleanup with zirconium-based sorbent. The developed method was evaluated at four spiking levels (1, 5, 50, and 100 ng/g) and further validated by analysis of NIST Standard Reference Materials (SRMs) 197413 and 1947 for selected pesticides with certified concentrations. Acceptable recoveries (70-120%) and standard deviations below 20% were achieved for the majority of pesticides from fortified samples. The measured values for both SRMs agreed with certified values (71-115% accuracy, 4-14% relative standard deviations) for all pesticides, except for p,p-DDD + o,p-DDT (45%) and heptachlor (133%) in SRM 1974b and except for mirex (58%) and trans-chlordane (136%) in SRM 1947. The developed method is fast, simple, and inexpensive with detection limits of 0.5-5 ng/g. Residues of dimethoate, hexachlorobenzene, BHC, lindane, nonachlor, chlorpyrifos, trifluralin, p,p-DDE, p,p-DDD, o,p-DDD, o,p-DDT, p,p-DDD, and chlordane were measured in catfish samples from the market.