色谱 ›› 2017, Vol. 35 ›› Issue (8): 860-866.DOI: 10.3724/SP.J.1123.2017.03033

• 研究论文 • 上一篇    下一篇

串联双柱固相萃取-气相色谱-串联质谱法检测茶叶中拟除虫菊酯

刘丽1, 张琦1,2, 王海雁2, 冯锋2, 曹海荣2, 杨震2, 柯志军2, 陈希尧3   

  1. 1. 大同市疾病预防控制中心理化检验科, 山西 大同 037008;
    2. 山西大同大学化学与环境工程学院, 山西 大同 037009;
    3. 上海市计量测试技术研究院, 上海 200233
  • 收稿日期:2017-03-27 出版日期:2017-08-08 发布日期:2013-11-25
  • 通讯作者: 王海雁,E-mail:why7135280@126.com
  • 基金资助:

    国家自然科学基金(21375083);山西省高等学校大学生创新创业训练项目(2015348);山西大同大学博士科研启动项目(2008K3); 2016-度山西省留学人员科技活动择优资助项目(No.14).

Determination of pyrethroid pesticides in tea by series two-solid phase extraction-columns cleanup and gas chromatography-tandem mass spectrometry

LIU Li1, ZHANG Qi1,2, WANG Haiyan2, FENG Feng2, CAO Hairong2, YANG Zhen2, KE Zhijun2, CHEN Xiyao3   

  1. 1. Physical and Chemical Inspection Institute, Datong Center for Disease Control and Prevention, Datong 037008, China;
    2. School of Chemistry and Environment Engineering, Shanxi Datong University, Datong 037009, China;
    3. Shanghai Institute of Technology and Strict Testing Measurement, Shanghai 200233, China
  • Received:2017-03-27 Online:2017-08-08 Published:2013-11-25
  • Supported by:

    National Natural Science Foundation of China (No. 21375083); Training Project of Shanxi Datong University Students' Innovation and Entrepreneurship (No. 2015348); Shanxi Datong University launched Doctoral Research Program (No. 2008K3); Fund Program for the Scientific Activities of Selected Returned Oversea Professionals in Shanxi Province (No. 14).

摘要:

建立了气相色谱-串联质谱定量检测花茶、绿茶、红茶和黑茶4类茶叶中氟氯氰菊酯、氯氰菊酯和氰戊菊酯3种拟除虫菊酯农药残留量的方法。样品采用乙腈进行提取,优化洗脱液配比,选择Carb/NH2和SLH双柱串联净化富集。采用外标法定量,30 min内完成农药残留检测。3种拟除虫菊酯的检出限分别为0.4、1.0和0.3 μ g/kg,在0.05~2.00 mg/kg内线性关系良好,相关系数均大于0.999。在0.10、0.50和2.00 mg/L 3个添加水平下,空白加标样品的回收率为80.6%~116.3%。茶叶实际样品检测结果的日内相对标准偏差(RSD)为1.3%~12.6%,日间RSD为2.7%~12.1%。该法操作简单,重现性好,适用于茶叶中拟除虫菊酯类农药残留的检测。

关键词: 茶叶, 拟除虫菊酯农药, 气相色谱-串联质谱

Abstract:

A rapid determination method of three pyrethroid pesticides (cyfluthrin, cypermethrin and fenvalerate) in tea was developed by series two-solid phase extraction-column cleanup and external standard method coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) in 30 min. The pesticide residues in tea were extracted with acetonitrile, and cleaned up by Carb/NH2 and SLH solid-phase extraction columns. After filtration, the target compounds were analyzed by GC-MS and quantified by the external standard method. Under the optimized conditions, good linear ranges of 0.05-2.00 mg/kg were obtained. The limits of detection varied from 0.3 to 1.0 μ g/kg. The linear correlation coefficients were greater than 0.999. At three spiked levels (0.10, 0.50 and 2.00 mg/L), the average recoveries were determined between 80.6% and 116.3% in the four matrices. The inter-day relative standard deviations were between 1.3%-12.6%, and the intra-day relative standard deviations were between 2.7% and 12.1%. This method is simple, fast, and has a good reproducibility, which can meet the requirements of the rapid detection of pyrethroid pesticides in tea.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), pyrethroid pesticides, tea

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