Abstract

A high throughput method for simultaneous determination of 200 pesticides and 65 environmental contaminants: polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and other flame retardants, was developed and validated in cattle, swine and poultry muscle tissues. The method was based on sample preparation with QuEChERS extraction followed by an automated robotic sample cleanup with solid phase extraction (SPE) mini-columns using Instrument Top Sample Preparation (ITSP). The automated robotic ITSP was integrated with instrumental analysis (low pressure (LP)GC–MS/MS) to conduct sample cleanup and analysis in parallel. Another aliquot of the initial QuEChERS extract was subjected to UHPLC-MS/MS analysis, and 53 overlapping pesticides were analyzed by both LPGC- and UHPLC-MS/MS (10 min each). Fit-for-purpose LOQs<5 ng/g were achieved for ≥90% of the analytes. The method was validated in cattle, swine and chicken muscles at three spiking levels at and below the US regulatory levels of concern, and satisfactory recoveries (70–120%) and RSDs ≤ 20% were demonstrated for 219 analytes. Matrix effects were within ±20% for 78–97% of LC- and GC-amenable analytes. The validated method was successfully applied for the analysis of real-world incurred meat and poultry samples, further demonstrating its applicability to real-world samples, and potential for implementation in routine monitoring of contaminants.

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