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串联双固相萃取柱净化-气相色谱-串联质谱法测定茶叶中的拟除虫菊酯类农药

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

作者信息

Liu Li, Zhang Qi, Wang Haiyan, Feng Feng, Cao Hairong, Yang Zhen, Ke Zhijun, Chen Xiyao

机构信息

Physical and Chemical Inspection Institute, Datong Center for Disease Control and Prevention, Datong 037008, China.

School of Chemistry and Environment Engineering, Shanxi Datong University, Datong 037009, China.

出版信息

Se Pu. 2017 Aug 8;35(8):860-866. doi: 10.3724/SP.J.1123.2017.03033.

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/NH 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.

摘要

建立了一种在30分钟内通过串联双固相萃取柱净化和外标法结合气相色谱 - 串联质谱(GC - MS/MS)快速测定茶叶中三种拟除虫菊酯类农药(氟氯氰菊酯、氯氰菊酯和氰戊菊酯)的方法。茶叶中的农药残留用乙腈提取,并用Carb/NH和SLH固相萃取柱净化。过滤后,用GC - MS对目标化合物进行分析,并用外标法进行定量。在优化条件下,获得了0.05 - 2.00 mg/kg的良好线性范围。检测限为0.3至1.0μg/kg。线性相关系数大于0.999。在三个加标水平(0.10、0.50和2.00 mg/L)下,四种基质中的平均回收率在80.6%至116.3%之间。日间相对标准偏差在1.3% - 12.6%之间,日内相对标准偏差在2.7%至12.1%之间。该方法简单、快速,具有良好的重现性,能够满足茶叶中拟除虫菊酯类农药快速检测的要求。

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