作者：张群1,2, 马晨1,2, 秦安丽1,3, 段云1,2, 郇志博1,2, 吴琼1,3
作者单位：1. 中国热带农业科学院分析测试中心，海南 海口 571101;
2. 农业农村部热作产品质量安全风险评估实验室，海南 海口 571101;
3. 海南省热带果蔬产品质量安全重点实验室，海南 海口 571101
关键词：豇豆;菊酯农药;气相色谱-串联质谱;QuEChERS
摘要：
建立QuEChERS-气相色谱-串联质谱技术同时测定豇豆中6种菊酯农药(甲氰菊酯、氯氟氰菊酯、氟氯氰菊酯、氯氰菊酯、氟胺氰菊酯、氰戊菊酯)含量的快速检测方法。豇豆样品经乙腈提取，采样QuEChERS法进行净化，目标化合物经TG-5SILMS(30 m×0.25 mm，0.25 μm)色谱柱分离，采用三重串联四级杆选择反应监测模式（selected reaction monitoring, SRM）进行定性定量分析，外标法定量。结果表明，6种农药在0.001~0.5 mg/L范围内线性关系良好，相关系数均大于0.99；在3个添加浓度水平(0.01，0.05，0.10 mg/kg)下，平均回收率在89.6%~106.9%之间；5次重复的相对标准偏差在4.0%~11.9%；甲氰菊酯、氟氯氰菊酯和氰戊菊酯的定量限为0.003 mg/kg，氯氟氰菊酯、氯氰菊酯和氟胺氰菊酯的定量限为0.0015 mg/kg。该方法操作简便，结果准确，能满足豇豆中6种菊酯农药残留检测的要求。
Determination of 6 pyrethroid pesticide residues in cowpea using QuEChERS and GC-MS/MS
ZHANG Qun1,2, MA Chen1,2, QIN Anli1,3, DUAN Yun1,2, HUAN Zhibo1,2, WU Qiong1,3
1. Analysis and Testing Center, CATAS, Haikou 571101, China;
2. Laboratory of Quality and Safety Risk Assessment for Tropical Products, Ministry of Agriculture and Rural Affairs, Haikou 571101, China;
3. Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables, Haikou 571101, China
Abstract: For the determination of 6 pyrethroid pesticide residues in cowpea (fenpropathrin, cyhalothrin, cyfluthrin, cypermethrin, fluvalinate, and fenvalerate), a rapid analysis method was established by QuEChERS-gas chromatography-tandem mass spectrometry (QuEChERS-GC-MS/MS). The cowpea were extracted with acetonitrile, and purified by QuEChERS method. After that, the purification solution was separated by capillary GC columns TG-5SILMS (30 m×0.25 mm, 0.25 μm). A tandem quadrupole spectrometer operating in either full scan mode or in MS/MS mode for selected reaction monitoring (SRM) was used for the qualitative and quantitative analysis of the constituents, respectively. The results showed that the average recoveries of two pesticides were 89.6%~106.9% when the spiked levels were 0.01, 0.05, and 0.10 mg/kg, with relative standard deviations (RSDs) in the range of 4.0%~11.9% (n=5). The calibration curve showed a good linearity in the ranges of 0.001~0.5 mg/L, with the coefficient of determination was over 0.99. The limits of quantitation (LOQ) for fenpropathrin, cyfluthrin, and fenvalerate were 0.003 mg/kg; and for cyhalothrin, cypermethrin, and fluvalinate were 0.0015 mg/kg, respectively. This method is simple to operate, and accurate for the results, and also can meet the requirements for determination of 6 pyrethroid pesticide residues in cowpea.
Keywords: cowpea;pyrethroid pesticide;GC-MS/MS;QuEChERS
2021, 47(2):63-67 收稿日期: 2020-04-10;收到修改稿日期: 2020-05-21
基金项目: 海南省自然科学基金（318MS089）；国家农产品质量安全风险评估专项课题（GJFP201900605）；海南省自然科学基金高层次人才资助项目（320RC679）；海南省院士创新平台科研专项（YSPTZX202021）
作者简介: 张群(1984-),女,浙江杭州市人,助理研究员,博士,主要从事农药等有机污染物检测及污染修复方面的研究
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