Submitted to: Food Control
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 2/12/2016
Publication Date: 2/13/2016
Citation: Han, L., Sapozhnikova, Y.V., Lehotay, S.J. 2016. Method validation for 243 pesticides and environmental contaminants in meats and poultry by tandem mass spectrometry coupled to low-pressure gas chromatography and ultra high-performance liquid chromatography. Food Control. 66:270-282.
Interpretive Summary: The USDA Food Safety and Inspection Service (FSIS) conducts routine monitoring of pesticides in meats (cattle, swine, poultry, sheep, goats) to enforce regulatory compliance. Upon FSIS request, we developed and validated a simple, fast, wide scope, high throughput analytical method for simultaneous determination of 243 pesticides and environmental contaminants in FSIS-regulated foods (e.g. cattle, swine, and poultry) for transfer to FSIS regulatory field service laboratories and routine monitoring in their National Residue Program (NRP). The new advantageous method provides better quality of results for more chemicals of concern in more samples at higher throughput, less labor, and lower costs, and can be adopted by any requlatory or commercial laboratory worldwide for routine monitoring of contaminants in meats. FSIS obtained the needed instrumentation and is expected to further validate and implement the method in the near future.
Technical 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 less than but equal to 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.