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| Determination of Thiacloprid in Soil and Peanut Samples by Dispersive Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:high performance liquid chromatography-electrospray tandem mass spectrometry thiacloprid soil peanut dispersive solid phase extraction |
| Author | Institution |
| LI Min-jie, JIN Fen*, YANG Li-li, SHAO Hua, JIN Mao-jun, WANG Jing |
中国农业科学院农业质量标准与检测技术研究所，农业部农产品质量安全重点实验室 |
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| Abstract: |
| A sensitive high performance liquid chromatography-electrospray tandem mass spectrometric （HPLC-MS/MS） method with dispersive solid phase extraction （DSPE） was developed for the determination of thiacloprid in soil,plant,peanut and peanut hull samples.The extraction solvent,dispersive solid phase extraction sorbents were optimized.The analyte was extracted with acetonitrile containing 0.1% acetic acid,and purified with 50 mg PSA,50 mg C18 and 10 mg GCB dispersive solid phase extraction sorbents.Thiacloprid in the extract was separated by gradient elution using a mobie phase of water-methanol.Qualitative analysis was performed using electrospray ionization in positive ion mode（ESI+） under multiple reaction monitoring （MRM） mode.Matrix-matched calibrations were used to quantify the residue concentrations.The calibration curve was linear in the range of 0.1 -50 μg/kg with correlation coefficients more than 0.996.The recoveries of thiacloprid ranged from 70.6% to 119% at three spiked concentration levels in soil,plants,peanut and peanut hull,with relative standard deviations（RSDs）not more than 16.6%.The limits of quantitation（LOQs） were in the range of 1.0 -5.0 μg/kg.The method could match the requirements for the maximum residue limits （MRLs） in the world. |
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