超高效液相色谱-串联质谱法测定植物油中邻氨基苯甲二酰胺类农药
目的 建立同时测定植物油中氰虫酰胺、氯虫苯甲酰胺和氟虫酰胺3种邻氨基苯甲二酰胺类杀虫剂残留量的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测方法。方法 植物油经环已烷-乙酸乙酯提取后, 采用凝胶渗透色谱(gel permeation chromatography, GPC)系统净化, UPLC采用Syncronic C18色谱柱分离, 以乙腈和5 mmol/L乙酸铵溶液作为流动相进行梯度洗脱; 质谱采用电喷雾正离子源模式和多反应监测模式测定, 以外标法定量。结果 3种邻氨基苯甲二酰胺类农药的方法检出限均能达到0.01 mg/kg, 在0.01~0.2 mg/L浓度范围内线性关系良好, 相关系数r>0.9988, 在0.01、0.02和0.1 mg/kg 3个浓度水平进行加标回收, 回收率均在72.6%~90.8%范围之间; RSD在2.9%~9.9%之间。结论 该方法快速简便、灵敏度高、净化效果好, 且显著地缩短了检测时间, 可应用于植物油中邻氨基苯甲二酰胺类农药的快速分析。
Objective To establish a method for simultaneous determination of 3 kinds of anthranilic diamide pesticide residues including cyantraniliprole, chlorantraniliprole and flubendiamide in vegetable oil by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Method Vegetable oil was extracted with cyclohexane and ethyl acetate solution, purified by gel permeation chromatography system (GPC), and separated by the Syncronic C18 column with acetonitrile and 5 mmol/L ammonium acetate solution as mobile phase for gradient elution. Mass spectrometry used electro spray ionization in positive mode (ESI+) and multiple reaction monitoring (MRM) mode for detection with external standard method for quantification. Results The limits of detection of 3 kinds of anthranilic diamide pesticides could achieve 0.01 mg/kg, and they had good linear relationships in the range of 0.01~0.2 mg/L with correlation coefficients larger than 0.9988. The recoveries spiked at 3 levels of 0.01, 0.02 and 0.1 mg/kg were between 72.6%~90.8% with the relatively standard deviations (RSDs) of 2.9%~9.9%. Conclusion The method is quick, simple and sensitive, its purifying effect is good, which can significantly shorten the detection time and be applied on the rapid analysis of anthranilic diamide pesticides in vegetable oil.
标题：超高效液相色谱-串联质谱法测定植物油中邻氨基苯甲二酰胺类农药
英文标题：Determination of anthranilic diamide pesticides in vegetable oil by ultra performance liquid chromatography-tandem mass spectrometry
作者：
张云 三明出入境检验检疫局
黄传辉 三明市食品药品审评与不良反应监督管理局测中心
陈泽宇 三明出入境检验检疫局
中文关键词:植物油,邻氨基苯甲二酰胺,凝胶渗透色谱,超高效液相色谱-串联质谱,
英文关键词:vegetable oil,anthranilic diamide,gel permeation chromatography,ultra performance liquid chromatography-tandem mass spectrometry,
发表日期：2016-05-07
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