Submitted to: Journal of Agricultural and Food Chemistry
Publication Type: Peer reviewed journal
Publication Acceptance Date: 1/3/2014
Publication Date: 1/3/2014
Publication URL: http://handle.nal.usda.gov/10113/58819
Citation: Sapozhnikova, Y.V. 2014. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for analysis of greater than 140 pesticides in fish. Journal of Agricultural and Food Chemistry. 62:3684-3689. DOI: 10/1021/jf404389e. Interpretive Summary: With an increasing global trading of agricultural goods, fast and efficient monitoring of imported/exported food is needed to comply with food safety regulations. We developed and evaluated a laboratory-based multi-residue method for analysis of 143 pesticides in catfish. The method is based on QuEChERS sample preparation coupled to low-pressure gas chromatography-tandem mass spectrometry (LP-GC/MS-MS) for improved high throughput analysis of over 140 pesticides simultaneously. With low detection limits achieved by this method, it can be easily applicable to analysis of pesticide residues at environmental relevant concentrations, and the generated data on their occurrence may aid in future risk assessment and regulations.
Technical Abstract: A multi-residue method for 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) clean-up 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) 1974b 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 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 and p,p-DDD, and chlordane were measured in catfish samples from the market.