title: Evaluation of different parameters in the extraction of incurred pesticides and environmental contaminants in fish.
abstract: Sample processing is often ignored during analytical method development and validation, but accurate results for real samples depend on all aspects of the analytical process. Also, validation is often conducted using only spiked samples, but extraction yields may be lower in incurred samples. In this study, different variables in extraction for incurred pesticides and environmental contaminants in fish were investigated. Among 207 analytes screened using low-pressure gas chromatography-tandem mass spectrometry, consisting of 150 pesticides, 15 polycyclic aromatic hydrocarbons (PAHs), 14 polychlorinated biphenyls (PCBs), 6 polybrominated diphenyl ethers (PBDEs), and 22 other flame retardants (FRs), 35 (16 pesticides, 9 PCBs, 5 PBDEs, and 5 PAHs) were identified for quantification in samples of salmon, croaker, and NIST Standard Reference Material 1947 (Lake Michigan Fish Tissue). Extraction efficiencies using different extraction devices (blending, vortexing, and vibrating) versus time, sample size, and sample/solvent ratio were determined. In comparison to blending results, use of a pulsed-vortexer for 1 min with 1/1 (g/mL) sample/acetonitrile ratio was generally sufficient to extract the incurred contaminants in the homogenized fish tissues. Conversely, extraction with a prototype vibration shaker often took 60 min to achieve 100% extraction efficiency. A main conclusion from this study is that accurate results for real samples can be obtained using batch extraction with a pulsed-vortexer in a simple and efficient method that achieves high sample throughput.
authors: Eastern Regional Research Center, Agricultural Research Service, U.S. Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, United States.
authors: Yelena
authors: Y
authors: Sapozhnikova
authors: Eastern Regional Research Center, Agricultural Research Service, U.S. Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, United States.
authors: Steven J
authors: SJ
authors: Lehotay
mesh_terms: D053000:Analytic Sample Preparation Methods / Q000295:instrumentation / Q000379:methods*; D000818:Animals; D004787:Environmental Pollution; D005399:Fishes; D005411:Flame Retardants / Q000032:analysis / Q000302:isolation & purification*; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D010575:Pesticides / Q000737:chemistry / Q000302:isolation & purification*; D017747:Seafood / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000737:chemistry / Q000302:isolation & purification*
chemical_list: D005411:Flame Retardants; D010575:Pesticides; D014874:Water Pollutants, Chemical
keywords: environmental contaminants; extractability; fish; pesticides; residue analysis; sample preparation