Simultaneous Determination of Six Pyrazole Fungicides in Grape Wine by Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:grape wine  pyrazole fungicides  solid phase extraction(SPE)  liquid chromatography-tandem mass spectrometry(LC-MS/MS)
  
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CHEN Xiang-zhun,XIA Bi-qi,HUANG Fu-zhen,CHENG Jie,SHEN Yan,HAN Chao* 1.温州出入境检验检疫局;2.温州大学化学与材料工程学院
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Abstract:
      A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was developed for the simultaneous determination of six pyrazole fungicides,including penflufen,fluxapyroxad,isopyrazam,furametpyr,bixafen and rabenzazole in grape wine samples.The sample was diluted with ultrapure water,and then cleaned up by HLB solid phase extraction.The separation was performed on an Agilent ZOBRAX C18 column(2.1 mm×150 mm,5 μm)using a gradient elution program with a mobile phase of 0.1%acetic acid-acetonitrile.The analyte was determined by electrospray ionization tandem mass spectrometry in multiple reaction monitoring(MRM)mode,and quantified by the external standard method.The results indicated that the calibration curves for pyrazole fungicides were linear(r2≥0999 3) in the range of 1.0-50.0 μg?L-1.The limits of quantitation(LOQs) were in the range of 0.1-0.4 μg?kg-1.The average recoveries at three spiked levels ranged from 72.8%to 92.6%with RSDs not more than 6.7%.This method is simple,rapid and sensitive,and is suitable for the analysis of six pyrazole fungicides in grape wines sample.
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