title: 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 500mg for 2.5mL 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 5-10ng/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.
authors.affiliation: College of Science, China Agricultural University, Beijing, 100193, China; U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA.
authors.forename: Lijun
authors.initials: L
authors.lastname: Han
authors.affiliation: U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA; Centro de Investigación en Contaminación Ambiental, Universidad de Costa Rica, San José, Costa Rica.
authors.forename: Jessie
authors.initials: J
authors.lastname: Matarrita
authors.affiliation: U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA.
authors.forename: Yelena
authors.initials: Y
authors.lastname: Sapozhnikova
authors.affiliation: U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038, USA. Electronic address: Steven.Lehotay@ars.usda.gov.
authors.forename: Steven J
authors.initials: SJ
authors.lastname: Lehotay
mesh_terms: D000818:Animals; D001937:Brassica / Q000737:chemistry; D004785:Environmental Pollutants / Q000032:analysis*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis; D008055:Lipids / Q000302:isolation & purification*; D027421:Persea / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis*; D011078:Polychlorinated Biphenyls / Q000032:analysis; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*; D000069466:Red Meat / Q000032:analysis; D012474:Salmon; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers; D008055:Lipids; D010573:Pesticide Residues; D011084:Polycyclic Aromatic Hydrocarbons; D011078:Polychlorinated Biphenyls
keywords: Analyte protectants; Cleanup; EMR-Lipid; Environmental contaminants; Fast GC–MS/MS; Foods; Pesticide residue analysis; QuEChERS; Sample preparation