Method validation for 243 pesticides and environmental contaminants in meats and poultry by tandem mass spectrometry coupled to low-pressure gas chromatography and ultrahigh-performance liquid chromatography

Abstract

An easy and reliable high-throughput analysis method was developed and validated for 192 diverse pesticides and 51 environmental contaminants (13 PCB congeners, 14 PAHs, 7 PBDE congeners, and 17 novel flame retardants) in cattle, swine, and poultry muscle. Sample preparation was based on the “quick, easy, cheap, effective, rugged and safe” (QuEChERS) approach using filter-vial dispersive solid-phase extraction (d-SPE) cleanup. Split final extracts were analyzed in parallel by low-pressure (vacuum outlet) GC-MS/MS and UHPLC-MS/MS (10 min each), providing an additional degree of confirmation for 55 overlapping LC- and GC-amenable pesticides. Analyte protectants were utilized to improve sensitivity and decrease matrix effects in GC analysis, and only filtration of initial extracts was enough to avoid ion suppression in UHPLC-MS/MS. The method was validated at three spiking levels (10, 25, and 100 ng/g) at or below established tolerance levels in the sample types. Satisfactory recoveries (70–120%) and RSDs ≤ 20% were achieved for 200 analytes. The validated method was successfully applied to the analysis of real-world incurred meat samples, further demonstrating the utility of the method for implementation in regulatory and commercial laboratories.