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.doc

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 史晓梅 章晴 杨永坛 杨悠悠 （中粮营养健康研究院 营养健康与食品安全北京市重点实验室，北京 102209） 摘 要 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。 关键词 凝胶渗透色谱 气相色谱-三重四极杆质谱 农药残留 植物油 中图分类号：TS207.3 文献标识码：A 文章编号：1003-0174（ ） - - Determination of Multi-pesticides Residues in Vegetable Oil by Gel Permeation Chromatography Purifying Method Combined with Gas Chromatography Tandem Mass Spectrometry Shi Xiaomei Zhang Qing Yang Yongtan Yang Youyou (COFCO Nutrition Health Research Institute, Beijing Key Laboratory of Nutrition Health and Food Safety, Beijing 102209) 收稿日期：2016-08-23 作者简介：史晓梅，女，1986年出生，硕士， 食品质量与安全 通讯作者：杨永坛，男，1971年出生，研究员， 食品质量与安全 Abstract 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 et al.), using gel permeation chromatography method and gas chromatography tandem mass spectrometry. Samples were dissolved by ethyl acetate: cyclohexane (1:1, V/V), and cleaned up by automatic gel permeation chromatography instrument. The column flow rate was 5 mL/min, collection time was from 7 min to 20 min, samples were concentrated by on-line vacuum concentration instrument, and dissolved by 1.0 mL hexane solution, 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