超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定果蔬中10种新型除草剂及杀虫剂的残留量  

Determination of 10 New Herbicides and Insecticides Residues in Fruits and Vegetables by UPLC-Q/Orbitrap HRMS

作　　者：严旭旭 戴唯 王缅 王兴宁 黄小焕 李志 YAN Xu-Xu;DAI Wei;WANG Mian;WANG Xing-Ning;HUANG Xiao-Huan;LI Zhi(Guiyang Customs,Guiyang 550000)

机构地区：[1]贵阳海关,贵阳550000

出　　处：《中国口岸科学技术》2025年第1期70-79,共10页China Port Science and Technology

基　　金：海关总署科研项目(2022HK132)。

摘　　要：本研究利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(Ultra Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry,UPLC-Q/Orbitrap HRMS)技术,建立了同时测定果蔬中10种新型除草剂及杀虫剂残留量的分析方法。果蔬样品经乙腈提取,采用QuEChERS前处理方法,150 mg无水硫酸镁(MgSO4)+25 mg十八烷基硅烷(C_(18))粉末净化处理。以乙腈-0.1%甲酸水溶液作为流动相进行梯度洗脱,Thermo Hypersil GOLD C_(18)(100 mm×2.1 mm,1.9μm)色谱柱分离待测物,在全扫描和自动触发二级质谱(Full MS/ddMS2)模式下,采用四极杆/静电场轨道阱高分辨质谱进行测定,基质匹配外标法定量。结果显示,10种新型除草剂及杀虫剂在0.5~100 ng/mL范围内线性良好,相关系数(r^(2))>0.99,选择3个浓度水平进行添加回收率试验(n=6),平均回收率为70.7%~113.4%,相对标准偏差(Relative Standard Deviations,RSDs)为1.3%~19.0%,定量限为1~5μg/kg。结果表明,该方法操作简单、快速高效,具有高灵敏度和较好的重复性,适用于果蔬中除草剂及杀虫剂的定性定量分析。This study employed ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q/Orbitrap HRMS)to establish an analytical method for the simultaneous determination of residues of 10 new herbicides and insecticides in fruits and vegetables.The fruits and vegetables samples were extracted by acetonitrile,treated by the QuEChERS pretreatment method and purified by using a mixture of 150 mg anhydrous magnesium sulfate(MgSO4)and 25 mg octadecyl silane(C_(18)).With acetonitrile and 0.1%formic acid solution as mobile phases for gradient elution,the analytes were separated on a Thermo Hypersil GOLD C_(18)(100 mm×2.1 mm,1.9μm)column,and then determined by HRMS in Full MS/ddMS2 modes and quantified by matrix matching external standard method.The 10 new herbicides and insecticides showed a good linear relationship in the range of 0.5-100 ng/mL,and the correlation coefficients(r2)greater than 0.99.Under the three spiked levels(n=6),the average recoveries were in the range of 70.7%-113.4%,the relative standard deviations(RSDs)ranging 1.3%-19.0%,and the limits of quantitation(LOQ)ranging 1-5μg/kg.The method is simple,rapid and efficient,with high sensitivity and good repeatability,which is suitable for qualitative and quantitative analysis of herbicides and insecticides in fruits and vegetables.

关 键 词：除草剂 杀虫剂 QUECHERS 高分辨质谱 果蔬 

分 类 号：O65[理学—分析化学]