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

Yelena Sapozhnikova
Journal of agricultural and food chemistry 2014 v.62 no.17 pp. 3684-3689
heptachlor, chlorpyrifos, DDT (pesticide), solid phase extraction, lindane, detection limit, food analysis, dimethoate, pesticide residues, mirex, DDE (pesticide), DDD (pesticide), acetonitrile, hexachlorobenzene, markets, trifluralin, food contamination, trans-chlordane, tandem mass spectrometry, multiresidue analysis, catfish, gas chromatography
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.