Submitted to: Journal of Chromatography A
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 8/10/2018
Publication Date: 8/16/2018
Citation: Sapozhnikova, Y.V. 2018. Development and validation of a semi-automated high-throughput analytical method for 265 pesticides and environmental contaminants in meats and poultry. Journal of Chromatography A. 1572:203-211. https://doi.org/10.1016/j.chroma.2018.08.025.
Interpretive Summary: In the US, the USDA Food Safety and Inspection Service (FSIS) is responsible for routine analysis of pesticides in meats and poultry. We have developed a new high-throughput method for fast analysis of 200 FSIS-priority pesticides and 65 environmental contaminants in meat (cattle, swine) and poultry (chicken) muscles for subsequent transfer to the USDA FSIS laboratory. The new method was fast, cost-effective and sensitive, and was successfully validated at and below US tolerance/levels of concern, and applied to the analysis of real-world chicken, swine, cattle, goat and turkey samples. The method is expected to be further validated and implemented by FSIS for routine monitoring of contaminants in meats and poultry in the National Residue Program.
Technical Abstract: A new method for the high-throughput analysis of 200 pesticides and 65 environmental contaminants (PCBs, PAHs, PBDEs and other flame retardants) in swine, cattle and poultry (chicken) muscles was developed and validated. Sample preparation was based on QuEChERS extraction with acetonitrile and simultaneous salting-out. One portion of the extract underwent automated cleanup with solid phase extraction (SPE) mini-columns using Instrument Top Sample Preparation (ITSP), and subsequent low pressure (LP)GC-MS/MS analysis for 152 pesticides and 65 environmental contaminants. Another aliquot of the initial extract was analyzed by UHPLC-MS/MS for 101 pesticides, with 53 overlapping in both GC- and LC-MS/MS analysis (10 min each). The method was validated in cattle, pork and chicken muscles at three spiking levels at and below the US regulatory levels of concern. Overall, satisfactory recoveries (70-120%) and RSDs = 20% were demonstrated for 219 analytes. With the use of analyte protectants and split injection in LPGC-MS/MS, 78-97% of GC analytes had matrix effects within ±20%. In UHPLC analysis, matrix effects were ±20% for 83-90% of LC pesticides. The validated method was successfully applied for analysis of real-world incurred meat and poultry samples, and residual amounts of 11 pesticides and 5 environmental contaminants were found in the samples not exceeding the levels of concern.