Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:total haloxyfop  alkaline hydrolysis  dispersive solid phase extraction  plant-derived foods  liquid chromatography-tandem mass spectrometry
  
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WANG Xing-ning,WANG Tao,LI Jie,LI Zhi,TANG Ya-feng,LIANG Yi-xin,ZHU Ming 1. Center for Comprehensive Technology of Guiyang Customs,Guiyang ,China; 2. Guizhou Light Industrial Vocational College,Guiyang ,China
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Abstract:
      A simple,fast and reliable method was developed for quantitative determination of total haloxyfop in plant-derived foods using liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS).The sample preparation consisted of a dispersive solid phase extraction(dispersive-SPE) method by addition of an alkaline hydrolysis step to release total haloxyfop.The target compound was extracted with acetonitrile,and then purified using anhydrous MgSO4,octadecyl(C18) and graphitized carbon black(GCB).A mixture of 0.1% formic acid acetonitrile and 0.1% formic acid aqueous solution was used as the mobile phase,followed by binary gradient elution,C18 (2.1 mm × 50 mm,1.7 μm) column separation.The analysis was performed in positive ion mode under multiple reaction monitoring(MRM) mode,and internal standard method was used for quantitative analysis.Results showed that there was a good linear relationship for haloxyfop over the range of 2.5-50 ng/mL with a correlation coefficient(r2) greater than 0.999.At three spiked levels(0.01,0.05 and 0.1 mg/kg),average recoveries for total haloxyfop ranged from 80.7% to 114%,with relative standard deviations(RSD) of 1.4%-11%.The limit of quantitation was as low as 0.01 mg/kg.The method showed a fully converted step from haloxyfop-esters to haloxyfop,and it was suitable for the analysis of total haloxyfop residues in plant-derived foods.
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