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

引用本文: 刘丽, 张琦, 王海雁, 冯锋, 曹海荣, 杨震, 柯志军, 陈希尧. 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[J]. 色谱, 2017, 35(8): 860-866. doi: 10.3724/SP.J.1123.2017.03033 shu

Citation: LIU Li, ZHANG Qi, WANG Haiyan, FENG Feng, CAO Hairong, YANG Zhen, KE Zhijun, CHEN Xiyao. Determination of pyrethroid pesticides in tea by series two-solid phase extraction-columns cleanup and gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(8): 860-866. doi: 10.3724/SP.J.1123.2017.03033 shu

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.
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
基金项目:
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）.

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:

English

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

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 Date: 27 March 2017
Fund Project:
National Natural Science Foundation of China (No. 21375083)

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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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

English

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

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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