Simultaneous Determination of 167 Pesticide Residues in Soybean by Liquid Chromatography-Electrospray Tandem Mass Spectrometry[J]. 2014,33(5):499-505.DOI:
A high sensitivity and throughput method was developed for the simultaneous determination of 167 pesticide residues in soybean by liquid chromatography-electrospray tandem mass spectrometry(LC-MS/MS).Sample was soaked with water and extracted with acetonitrile,followed by salting out with anhydrous MgSO4,NaCl,Na3Citrate dihydrate and Na2HCitrat sesquihydrate mixture.The extract was added to C18 and PSA solid phase extraction columns,and eluted with 2% formic acid methanol solution.The eluent was concentrated to a constant volume and separated on an Atlantis C18 column(100 mm×2.1 mm,3 μm) .The analyte was analyzed by HPLC-MS/MS with a positive and negative ions switching mechanism under multiple reaction monitoring mode.The results were quantified with matrix-matched standard solutions as the external standard.The average recoveries of the pesticides at three spiked concentration levels of 0.01,0.02,0.05 mg/kg were in the range of 67.3%-123.5%,with RSDs of 4.7%-13.9%.All the pesticides in matrix-matched standard solutions were linear in the range of 0-50.0 μg/L with correlation coefficients more than 0.99.The limits of quantitation(S/N>10) for all pesticides were 0.01 mg/kg.The proposed method was suitable for the screening of multi-pesticide residues in soybean for its high sample throughput,low LOQ,good accuracy and precision.
关键词
高效液相色谱-串联质谱大豆农药多残留高通量
Keywords
liquid chromatography-electrospray tandem mass spectrometry(LC-MS/MS)soybeanmulti-pesticide residueshigh-throughput