童婷婷¹，栗 平¹，李洁琼¹，王安首¹，蒲祖怡¹，付金娥¹，^2*

（1.广西壮族自治区药用植物园，西南濒危药材资源开发国家工程实验室，南宁530023；

2.广西道地药材高品质形成与应用重点实验室，南宁530023）

摘要：选择QuEChERS快速处理法，建立液相色谱串联三重四极杆质谱（LC-MS/MS）测定广西5种山野菜中15种农药残留的方法。试样经乙腈提取，加QuEChERS复合提取盐包继续提取，再经无水硫酸镁、N-丙基乙二胺、石墨化炭黑进行分散固相萃取净化，采用LC-MS/MS在多反应监测（MRM）模式下，以5mmol/L甲酸铵-0.1%甲酸水溶液为水相、乙腈为有机相，以基质匹配标准曲线计算结果，对5种山野菜中15种农药残留进行测定。15种农药残留在2～100 μg/L范围内线性关系良好，相关系数（r）在0.992 5～0.999 2之间，加标回收率在60.2%～119.1%之间，相对标准偏差（RSD）在1.9%～9.7%之间，检出限（LOD）在0.003～2.450μg/kg之间，能满足农药残留测定要求。该方法可用于山野菜中农药残留的检测分析。

关键词：农药残留；液相色谱串联三重四极杆质谱；山野菜；分散固相萃取

中图分类号：TS207.5 文献标识码：A 文章编号：1674-506X（2025）04-0133-0007

Determination of 15 Pesticide Residues in 5 Kinds of Wild Vegetables in Guangxi by QuEChERS-LC-MS/MS Method

TONG Tingting¹，LI Ping¹，LI Jieqiong¹，WANG Anshou¹，PU Zuyi¹，FU Jin’e¹，^2*

(1.Guangxi Botanical Garden of Medicinal Plants，National Engineering Laboratory for Development of Endangered Medicinal Materials Resources in Southwest China，Nanning 530023，China；

2.Key Laboratory of Guangxi for High-quality Formation and Utilization of Dao-di Herbs，Nanning 530023，China)

Abstract: Rapid treatment method of QuEChERS was chosen to establish a method based on liquid chromatograph-tandem mass spectrometry （LC-MS/MS） for the determination of 15 pesticide residues in 5 kinds of wild vegetables in Guangxi. Samples were extracted with acetonitrile，then QuEChERS extraction pouch was added and continued the extraction， and the extract was purified by dispersive solid- phase extraction with magnesium sulfate，N-propyl ethylenediamine，and graphitized carbon black. The 15 pesticide residues in 5 kinds of wild vegetables were determined by LC-MS/MS in multiple reaction monitoring （MRM） mode，using 5 mmol/L ammonium formate- 0.1% formic acid water solution as aqueous phase and acetonitrile as organic phase， the results were calculated by matrix matching standard curve. The linear relationship among 15 pesticide residues was good between 2～100 μg/L，the correlation coefficient （r） was 0.992 5～0.999 2，the spiked recovery rate was 60.2% ～119.1% ， the relative standard deviation （RSD） was 1.9% ～9.7% ， and the limit of detection （LOD） was 0.003～2.450 μg/kg，able to meet the requirements of pesticide residue determination. The method can be used for the detection and analysis of pesticide residues in the wild vegetables.

Keywords: pesticide residues；liquid chromatograph-tandem mass spectrometry （LC-MS/MS）；wild vegetables；dispersive solid-phase extraction

doi: 10.3969/j.issn.1674-506X.2025.04-019