QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留

杨路平; 邵立君; 王国玲; 王锡宁; 任晓菲; 刘拥军

doi:10.13386/j.issn1002-0306.2019.14.040

QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留

杨路平^1,2,
邵立君^1,2,
王国玲^1,2,
王锡宁^1,2,
任晓菲^1,2,
刘拥军^3, ,

1. 山东大学预防医学研究院, 山东济南 250012;
2. 山东省疾病预防控制中心, 山东济南 250012;
3. 山东省医学科学院药物研究所, 山东济南 250062

基金项目:

山东省中医药科技发展计划(2017-182)。

山东省医药卫生科技发展计划(2015WS0273)

详细信息

作者简介:
杨路平(1977),女,硕士,副主任技师,研究方向:食品与环境相关理化检验,E-mail:18615281930@163.com。

通讯作者:
刘拥军(1968),男,硕士,研究员,研究方向:质谱分析相关研究,E-mail:doudou131415@163.com。

中图分类号: TS207.5⁺3
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出版历程
- 收稿日期: 2018-07-10
- 网络出版日期: 2020-11-12
- 刊出日期: 2019-07-14

Determination of Thirteen Pesticides in Edible Mushrooms by QuEChERS with UPLC MS/MS

1. Preventive medicine Research Institute of Shandong University, Jinan 250012, China;
2. Shandong Center for Disease Control and Prevention, Jinan 250012, China;
3. Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, China

摘要

摘要: 目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0 g用乙腈-水(4:1)15 mL超声提取,经N-丙基乙二胺(PSA)30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5~200 μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3 μg/kg。加标回收率84.3%~102%,相对标准偏差(n=6)2.8%~6.3%。结论:该方法可用于食用菌中13种农药残留的检测。
- QuEChERS /
- 液相色谱-串联质谱法 /
- 食用菌 /
- 农药残留
Abstract: Objective:Determination of thirteen pesticides in edible mushrooms by QuEChERS with UPLC MS/MS. Methods:5.0 g sample was extracted ultrasonically for 5 min with 15 mL of 4:1 acetonitrile and water. The extract was purified by N-propyl ethylenediamine (PSA) 30.0 mg, anhydrous Magnesium sulfate 15.0 mg dispersive solid-phase extraction adsorbent.The purified solution was separated by UPLC using HSS T3 column, 0.1% formic acid and acetonitrile as mobile phase in gradient elution. Positive ESI and MRM were adopted in MS analysis. Results:Linear relationships were found between the peak area and the mass concentration of 13 pesticides within 0.5~200 μg/L. With detection limits (S/N=3) in the range of 0.03~0.3 μg/kg, recovery rates obtained by standard addition method ranged from 84.3% to 102% and RSDs (n=6) were in the range of 2.8%~6.3%. Conclusion:The proposed method was successfully applied to the detection of 13 pesticides in mushrooms.
- QuEChERS /
- UPLC MS/MS /
- edible mushrooms /
- pesticides residue