Collaborative Validation of the QuEChERS Procedure for the Determination of Pesticides in Food by LC–MS/MS

Autor: Chris Sack, Barbara K Neuhaus, Michael Smoker, Kai Zhang, Shaun MacMahon, Richard D. Thompson, Claude Masse, Jon W. Wong, Greg Satterfield, Irene Cassias, Eugene Chang, Greg Mercer, Robert E. Smith, Narong Chamkasem, Yi Lin
Rok vydání: 2011
Předmět:
Zdroj: Journal of Agricultural and Food Chemistry. 59:6383-6411
ISSN: 1520-5118
0021-8561
Popis: Seven FDA pesticide laboratories collaborated to develop and validate an LC-MS/MS method to determine 173 pesticides in20 min. The average determination coefficient (r²) was0.99 for all but two compounds tested. The limits of detection were20 ng/mL for all compounds and10 ng/mL for 363 of the 368 transitions reported. The method was used to determine pesticides in two AOAC sponsored proficiency samples. The LC-MS/MS determination was used for the analysis of oranges, carrots and spinach using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method. Each matrix was fortified at 20, 100, 400, and 1000 ng/g. No false positive responses were detected in controls of the three matrices. 165 pesticides had recoveries between 70 and 130%, and 161 had minimum detection levels less than 10 ng/g. Recoveries of 169 compounds for the 1000 ng/g spikes were within 50-150%. A matrix effect study indicated all three matrices caused a small net suppressing effect, the most pronounced attributable to the citrus matrix. The procedure proved to be accurate, precise, linear, sensitive and rugged, and adds 100 pesticides to the scope of the FDA pesticide program.
Databáze: OpenAIRE
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