首页> 中文期刊> 《中国粮油学报》 >凝胶渗透色谱净化结合气相色谱-三重四极杆质谱法测定植物油中多农药残留量

凝胶渗透色谱净化结合气相色谱-三重四极杆质谱法测定植物油中多农药残留量

         

摘要

A method was established for the determination of various kinds of pesticides residues in vegetable oil (including organophosphorus pesticides,organochlorine pesticides,pyrethroid pesticides,carbamate pesticides and triazole fungicides etc.),using gel permeation chromatography method and gas chromatography tandem mass spectrometry.Samples were dissolved by ethyl acetate:cyclohexane (1 ∶ 1,V/V),and purified by automatic gel permeation chromatography instrument.The column flow rate was 5 mL/min,collection time was from 7 to 20 min,samples were concentrated by on-line vacuum concentration instrument,and dissolved by 1.0 mL hexane solution,and finally analyte qualification and confirmation was performed using GC-MS/MS with selected reaction monitoring (SRM) mode.A good linearity was observed for all compounds in the concentration range investigated with correlation coefficients of 0.990 0 ~ 0.998 5.At the fortification level of 0.05 ~ 0.40 mg/kg,the average recoveries were in the range of 60.5 % ~ 118.0%,and the relative standard deviations (RSDs,n =6) ranged from 1.3 % to 14.5 %,limit of detections(LODs)were in the range of 0.002 ~0.01 mg/kg.This method could meet the requirements of pesticides maximum residue limits(MRLs) in vegetable oil home and abroad.%建立了凝胶渗透色谱法结合气相色谱-三重四极杆质谱测定植物油中多种类型农药残留的方法(有机磷农药、有机氯农药、拟除虫菊酯农药、氨基甲酸酯农药、三唑类杀菌剂、植物生长调节剂等).样品使用乙酸乙酯-环己烷(1∶1,V/V)溶解后,经全自动凝胶渗透色谱仪净化,色谱柱流速为5 mL/min,收集时间为7 ~20 min,然后进行在线自动真空浓缩,正己烷溶剂将样品定容到1.0 mL,使用气相色谱-三重四极杆质谱仪的选择反应监测模式进行定性和定量分析.在相应线性范围内,所有化合物线性关系良好,线性相关系数R2在0.990 0~0.998 5之间.在0.05 ~0.40 mg/kg添加水平时,平均回收率为60.5% ~ 118.0%,相对标准偏差(RSDs,n=6)为1.3% ~14.5%,检出限在0.002 ~0.01 mg/kg之间,满足国内外对植物油中农药最大残留限量的标准要求.

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