Simplified pesticide multiresidues analysis in fish by low-temperature cleanup and solid-phase extraction coupled with gas chromatography/mass spectrometry

A simple and fast method for the simultaneous analysis of thiobericarb, deltamethrin and 19 organochlorine pesticide residues in fish by gas chromatography-mass spectrometry was investigated in this Study. Samples are extracted with acetonitrile. Most of lipids in the extract are eliminated by low-temperature cleanup prior to solid-phase extraction cleanup. The lipids extracted from the fish samples were easily removed Without ally significant losses Of the pesticides. Aminopropyl (NH2) Cartridge Was effective to eliminate the remaining interference. Spiked experiments were carried Out to determine the recovery, precision and limits of detection (LODs) of the method. The method detection limits ranged from 0.5 mu g kg(-1) to 20 mu g kg(-1) whilst recoveries of tile pesticides were in file range of 8 1.3-113.7% with relative standard deviations 13.5% at a spiked concentration of 0.05 mg kg(-1), 0.02 mg kg(-1) and 0.1 mg kg(-1). The newly developed method is demonstrated to give efficient recoveries and LODs for detecting pesticide multiresidues in fish. (C) 2008 Elsevier Ltd. All rights reserved.