Determination of Thiacloprid in Soil and Peanut Samples by Dispersive Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry[J]. 2014,33(4):479-482.
Determination of Thiacloprid in Soil and Peanut Samples by Dispersive Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry[J]. 2014,33(4):479-482.DOI:
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.
关键词
液相色谱-串联质谱噻虫啉土壤花生分散固相萃取
Keywords
high performance liquid chromatography-electrospray tandem mass spectrometrythiaclopridsoilpeanutdispersive solid phase extraction