| 气相色谱-串联质谱法快速检测当归中102种农药残留 |
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| 引用本文： | 闫君,赵波,张文,瓦晓霞,王小乔,陈婷.气相色谱-串联质谱法快速检测当归中102种农药残留[J].农药学学报,2019,21(3):315-326. |
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| 作者姓名： | 闫君 赵波 张文 瓦晓霞 王小乔 陈婷 |
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| 作者单位： | 1.兰州市食品药品检验所，兰州 730050 |
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| 基金项目： | 甘肃省食品药品监督管理局青年科技创新项目（2018GSFDA045） |
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| 摘 要： | 建立了当归中102种农药残留的快速检测方法。样品采用优化的QuEChERS前处理方法，利用气相色谱-串联质谱 (GC-MS/MS) 检测，动态多反应监测 (dMRM) 模式，基质匹配外标法定量。结果表明:在样品前处理过程中，经对提取溶剂、提取体系、净化体系的组成和用量进行筛选优化后，样品采用乙腈、1.0 g氯化钠、4.0 g无水硫酸镁、1.0 g柠檬酸钠和0.5 g柠檬酸二钠盐提取，无水硫酸镁800 mg、PSA 150 mg、C18 150 mg净化，通过基质匹配外标法校正，当归中基质效应对目标化合物的定性、定量影响明显减弱。在0.02~0.64 mg/kg范围内，102种农药的质量浓度与对应的峰面积间呈良好的线性关系，R2均大于0.99，检出限为0.002 5~0.025 mg/kg，定量限为0.005~0.05 mg/kg；在0.04、0.08和0.32 mg/kg 3个添加水平下，102种农药的平均回收率为52 %~128%，RSD为1.0%~10 %。该方法快速简便、耗时短，具有良好的灵敏度、正确度和精密度，为提高当归中农药安全水平，降低健康风险提供了一种快速、高效、可靠的分析手段。
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| 关 键 词： | QuEChERS 气相色谱-串联质谱 动态多反应监测 当归 快速筛查 农药残留 |
| 收稿时间： | 2018/12/9 0:00:00 |
Rapid detection of 102 pesticides residues in Angelica sinensis using gas chromatography-tandem mass spectrometry |
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| YAN Jun,ZHAO Bo,ZHANG Wen,WA Xiaoxi,WANG Xiaoqiao and CHEN Ting.Rapid detection of 102 pesticides residues in Angelica sinensis using gas chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2019,21(3):315-326. |
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| Authors: | YAN Jun ZHAO Bo ZHANG Wen WA Xiaoxi WANG Xiaoqiao and CHEN Ting |
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| Institution: | 1.Lanzhou Institutes for Food and Drug Control, Lanzhou 730050, China2.Basic Medical College, Gansu University of Chinese Medicine, Lanzhou 730030, China |
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| Abstract: | Established a rapid determination method for 102 kinds of pesticide residues in angelica sinensis of genuine medicinal materials in Gansu. Optimized the QuEChERS pretreatment method, used pattern detection with gas chromatography-tandem mass spectrometry (GC-MS/MS), dynamic multi response monitoring (dMRM), and matrix matching external standard method, studied the influence of extraction agent, extraction system, composition and dosage of purification system on sample extraction and purification in the pre-treatment process of angelica pesticide residues, as well as the influence of matrix effect on the detection results. Optimized and used acetonitrile, 1.0 g sodium chloride, 4.0 g anhydrous magnesium sulfate, 1.0 g sodium citrate, 0.5 g disodium citrate for extraction, and 800 mg anhydrous magnesium sulfate, 150 mg PSA, 150 mg C18 for purification. The influence of matrix effect on qualitative and quantitative on target compounds in angelica significantly reduced by the correction with matrix matching external standard method. The methodological validation indicators was well that 102 kinds of pesticide residues show a good linear relationship within the range of 0.02 mg/kg to 0.64 mg/kg, and the R2 was greater than 0.99. Method detection limit is from 0.002 5 mg/kg to 0.025 0 mg/kg. Method quantitative limit is from 0.005 0 mg/kg to 0.050 0 mg/kg. The average recovery rate was from 52% to 128%, and the RSD was from 1.0 % to 10%. The method was rapid, simple, time-consuming and has good sensitivity, accuracy and precision, provided a fast, efficient and reliable analytical method for improve the level of pesticide safety in angelica sinensis and reduce health risks. |
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| Keywords: | QuEChERS gas chromatography-tandem mass spectrometry (GC-MS/MS) dynamic multi response monitoring (dMRM) Angelica sinensis rapid screening pesticide residues |
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