Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods

Abstract

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography – tandem mass spectrometry (LPGC–MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid (“enhanced matrix removal of lipids”) and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500 mg for 2.5 mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83–98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC–MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70–120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76–85 of the 117 analytes achieved satisfactory results (recoveries of 70–120% and RSD ≤ 20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5–10 ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods.