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Simultaneous determination of organochlorine and pyrethriod pesticide residues in the Chinese patent medicines by gas chromatography-tandem mass spectrometry
Authors:Xue J Mao  Yao Zhong  Ai P Yan  Bin Wang
Institution:1. State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang, People's Republic of China;2. Pharmaceutical College of Nanchang University, Nanchang, People's Republic of China;3. Center of Analysis and Testing, Nanchang University, Nanchang, People's Republic of China
Abstract:A simple, sensitive, reliable method was developed for the simultaneous determination of organochlorine and pyrethriod pesticide residues in Chinese patent medicines Six ingredient rehmannia pills and Xiaoyao pills. These pesticides were extracted by ethyl acetate. The extraction time and volume of ethyl acetate were optimized. Cleanup of extracts was performed with dispersive-solid phase extraction using graphitized carbon black as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography–tandem mass spectrometry in multiple reaction monitoring mode (GC-MS/MS, MRM). The linearity of the calibration curves is good in matrix-matched standard and yields the coefficients of determination (R2) ≥0.99 for all of the target analytes. Under optimized conditions, the average recoveries (five replicates) for most pesticides range from 75.5% to 114.6%, and RSDs are less than 10.0%. The LODs of 18 pesticides in Six ingredient rehmannia pill and Xiaoyao pills are in the range of 0.01–8.82 μg kg?1. The developed method meets the requirements of pesticide residue analysis and could be effectively used for routine analysis of the organochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pills and Xiaoyao pills.
Keywords:Organochlorine pesticides  pyrethroid pesticides  gas chromatography-tandem mass spectrometry  ultrasound-assisted extraction  dispersive-solid phase extraction  Chinese patent medicines
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