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分散固相萃取-气相色谱-三重四极杆质谱法测定代用茶中的农药残留量

[Determination of pesticide residues in substitutional tea by dispersive solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry].

作者信息

Li Ye, Zhao Danying, Guo Aihua, Wen Ya, Li Kun, Wu Guohua

机构信息

Beijing Xicheng District Center for Disease Control and Prevention, Beijing 100120, China.

出版信息

Wei Sheng Yan Jiu. 2018 Jul;47(4):621-627.

Abstract

OBJECTIVE

The method was established for determination 14 kinds of psticide residues in substitutional tea using gas chromatography-triple quadrupole mass spectrometry( GC-MS/MS) for instrument method and dispersive solid-phase extraction( dSPE) for sample preparation.

METHODS

The samples extracted with acetonitrile, and purified by N-propyl ethlene diamine( PSA), the extracts were separated on DB-5MS column( 30 m × 0. 25 mm, 0. 25 μm) with programmed temperature and determined by GCMS/MS in multi-reaction monitoring( MRM) model. The external standard method was applied to quantify the pesticides.

RESULTS

The method showed a good linearity( r ≥0. 999) in certain ranges for 14 kinds of pesticides. The limits of quantification( LOQ)were 4-40 μg/kg. The average recoveries range were 65. 6%-116. 6% in three add levels of 20, 40 and 200 μg/kg, and relative standard deviations( RSD S) of 1. 5%-15. 7%( n = 6).

CONCLUSION

This method is simple, fast, sensitive, selective and can satisfy the request of simultaneous analysis of multiple pesticide residues in substitutional tea.

摘要

目的

建立气相色谱 - 三重四极杆质谱法(GC-MS/MS)结合分散固相萃取(dSPE)测定代用茶中14种农药残留的方法。

方法

样品用乙腈提取,经N-丙基乙二胺(PSA)净化,提取物在DB-5MS柱(30 m×0.25 mm,0.25μm)上采用程序升温分离,用GC-MS/MS在多反应监测(MRM)模式下测定。采用外标法对农药进行定量。

结果

该方法对14种农药在一定范围内线性良好(r≥0.999)。定量限(LOQ)为4 - 40μg/kg。在20、40和200μg/kg三个添加水平下,平均回收率范围为65.6% - 116.6%,相对标准偏差(RSD)为1.5% - 15.7%(n = 6)。

结论

该方法简便、快速、灵敏、选择性好,能满足代用茶中多种农药残留同时分析的要求。

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