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采用基于QuEChERS的方法和气相色谱-三重四极杆质谱法对韭菜和大蒜中的213种农药进行多残留分析。

Multiresidue analysis of 213 pesticides in leek and garlic using QuEChERS-based method and gas chromatography-triple quadrupole mass spectrometry.

作者信息

He Zeying, Chen Shanshan, Wang Lu, Peng Yi, Luo Ming, Wang Wenwen, Liu Xiaowei

机构信息

Agro-Environmental Protection Institute, Ministry of Agriculture, Tianjin, 300191, China.

出版信息

Anal Bioanal Chem. 2015 Mar;407(9):2637-43. doi: 10.1007/s00216-015-8485-9. Epub 2015 Jan 27.

DOI:10.1007/s00216-015-8485-9
PMID:25619986
Abstract

A simple and sensitive multiresidue pesticide analysis method was developed and validated for 213 pesticides in leek and garlic based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure combined with gas chromatography-triple quadrupole mass spectrometry. In the QuEChERS method, commercial extraction salt packet, dispersive solid-phase extraction adsorbent packet, and ceramic homogenizer were used to simplify the extraction procedure. The gas chromatography-tandem mass spectrometry (GC-MS/MS) parameters were optimized for analysis of 213 pesticides within a 38-min run time with a limit of quantification for most of the pesticides at 2 μg kg(-1). The coefficient of determination (r(2)) was >0.99 within the calibration linearity range of 2-400 μg kg(-1). Most recoveries at 2, 5, 10, 20, 50, 100, and 200 μg kg(-1) were in the range of 70-120% (n = 6) with associated relative standard deviations (RSDs) of <20%, indicating satisfactory precision. Real leek and garlic samples were analyzed for method application.

摘要

基于QuEChERS(快速、简便、廉价、高效、耐用且安全)方法结合气相色谱 - 三重四极杆质谱联用技术,开发并验证了一种用于韭菜和大蒜中213种农药多残留的简单灵敏分析方法。在QuEChERS方法中,使用市售萃取盐包、分散固相萃取吸附剂包和陶瓷匀浆器简化萃取过程。优化了气相色谱 - 串联质谱(GC-MS/MS)参数,以便在38分钟的运行时间内分析213种农药,大多数农药的定量限为2 μg kg⁻¹。在校准线性范围2 - 400 μg kg⁻¹内,测定系数(r²)>0.99。在2、5、10、20、50、100和200 μg kg⁻¹添加水平下,大多数回收率在70 - 120%范围内(n = 6),相关相对标准偏差(RSD)<20%,表明精密度良好。对实际的韭菜和大蒜样品进行了方法应用分析。

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