Sin-QuEChERS-GC-MS/MS法快速测定人参中47种残留农药<sup>*</sup>

高娜, 乔颖, 刘雪红, 李军, 葛祥武, 孙楠, 朱殿龙, 阮维斌, 郑丽新

doi:10.16155/j.0254-1793.2022.12.11

药物分析杂志 >

2022 , Vol. 42 >Issue 12: 2145 - 2154

DOI: https://doi.org/10.16155/j.0254-1793.2022.12.11

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Sin-QuEChERS-GC-MS/MS法快速测定人参中47种残留农药^*

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1.大连市检验检测认证技术服务中心,大连 116037;
2.南开大学生命科学学院,天津 300071

第一作者 Tel:15241492052; E-mail: gaona-888@163.com

^** 李军 Tel: 17190712337; E-mail: sophie9cn@sina.com
葛祥武 Tel: 13998493956; E-mail: dlgxw@163.com

收稿日期: 2022-03-25

网络出版日期: 2024-06-26

基金资助

^* 辽宁省重点研究计划项目(2020JH2/10200002)

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Rapid determination of 47 kinds of pesticide residues in Ginseng Radix et Rhizoma by Sin-QuEChERS-GC-MS/MS^*

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1. Dalian Center for Food and Drug Control and Certification, Dalian 116037, China;
2. College of Life Science, Nankai University, Tianjin 300071, China

Received date: 2022-03-25

Online published: 2024-06-26

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摘要

目的: 建立Sin-QuEChERS技术结合气相色谱串联质谱法同时快速测定人参中47种残留的农药。方法: 人参粉末样品加水经1%甲酸乙腈提取,采用QuEChERS提取盐包进行盐析,提取液经Sin-QuEChERS-Nano净化管1步净化,浓缩,加入内标磷酸三苯酯,采用GC-MS/MS进行检测。选用DB-5MS色谱柱进行分离,进样口温度为250 ℃,初始流速为1.2 mL·min^-1,电子轰击离子源,多反应监测模式,内标法定量。结果: 47种目标化合物在一定的含量范围内线性关系良好,相关系数均大于0.993 1,低、中、高3个水平加样回收率均在72.5%~116.0%,RSD为0.70%~13.9%,定量下限为0.01 mg·kg^-1;对30 批人参样品进行测定,共检出9种农药,其中五氯硝基苯检出率最高为56.7%。结论: 该方法高效、灵敏、准确,适合于人参中多种农药的快速筛查和定量检测,具有较强的实用价值。

关键词： Sin-QuEChERs; 气相色谱-串联质谱法; 人参; 农药残留; 五氯硝基苯; 快速分析; 内标法

本文引用格式

高娜, 乔颖, 刘雪红, 李军, 葛祥武, 孙楠, 朱殿龙, 阮维斌, 郑丽新 . Sin-QuEChERS-GC-MS/MS法快速测定人参中47种残留农药^*[J]. 药物分析杂志, 2022 , 42(12) : 2145 -2154 . DOI: 10.16155/j.0254-1793.2022.12.11

Abstract

Objective: To establish a rapid analysis method of Sin-QuEChERS technology combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) to detect 47 pesticide residues in Ginseng Radix et Rhizoma. Methods: Ginseng Radix et Rhizoma powder was treated with water and extracted with 1% formic acid-acetonitrile, salted out by the QuEChERS package and purified with Sin-QuEChERS tube in one step, after concentrating internal standard triphenyl phosphate was added, then detected by GC-MS/MS. DB-5MS column was used, the inlet temperature was set to 250 ℃, the initial velocity was 1.2 mL·min^-1, the electron impact ion source was applied with multiple reaction monitoring (MRM) modes, and internal standard method was used for quantification. Results: The 47 target compounds showed good linearities within a certain content ranges, with the correlation coefficients (r²) above 0.993 1. At the low, medium, and high addition levels, the average recoveries were in the range of 72.5%-116.0% with the relative standard deviations (RSDs) within 0.70%-13.9%. And the limits of quantitation (LOQs) for the 47 compounds were 0.01 mg·kg^-1. Thirty batches of Ginseng Radix et Rhizoma samples were tested and nine pesticides were detected, among them, quintozene showed the highest detection rate of 56.7%. Conclusion: The detecting method is efficient, sensitive, and accuracy, which can be used for rapid screening and quantitative detection of various pesticide residues in ginseng, and has strong practical value.

Key words： Sin-QuEChERs; gas chromatography-tandem mass spectrometry; ginseng; pesticide residues; quintozene; quick determination; intra-standard method

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