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 m L/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 m L,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。
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.
出处
《中国粮油学报》
EI
CAS
CSCD
北大核心
2017年第10期156-162,共7页
Journal of the Chinese Cereals and Oils Association
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
gel permeation chromatography, gas chromatography tandem mass spectrometry, pesticides, vegetable oil
