QuEChERS/UPLC-MS/MS法测定雷公藤及根际土壤中3种农药残留  

Determining three pesticide residues content in Tripterygium wilfordii root and its rhizosphere soil with QuEChER/UPLC-MS/MS method

作　　者：李凤凤 张毅鹏 龚达林 刘三波 黄麒元 梅之南 王学奎[1] 舒少华[1] LI Fengfeng;ZHANG Yipeng;GONG Dalin;LIU Sanbo;HUANG Qiyuan;MEI Zhinan;WANG Xuekui;SHU Shaohua(College of Plant Science and Technology,Huazhong Agricultural University,Wuhan 430070,China;China Resources Sanjiu(Huangshi)Pharmaceutical Co.,Ltd,Huangshi 435000,China;Sinopharm Zhonglian Pharmaceutical Co.,Ltd,Wuhan 430070,China)

机构地区：[1]华中农业大学植物科学技术学院,武汉430070 [2]华润三九(黄石)药业有限公司,黄石435000 [3]国药集团中联药业有限公司,武汉430070

出　　处：《华中农业大学学报》2023年第1期205-211,共7页Journal of Huazhong Agricultural University

基　　金：华润三九(黄石)药业有限公司资助项目;“十三五”重点研发计划中药现代化专项(2017YFC1700700)。

摘　　要：为建立雷公藤种植过程中常用农药的残留含量检测方法,采用快速样品前处理结合超高效液相色谱-串联质谱法(quick,easy,cheap,effective,rugged and safe/ultra performance liquid chromatography tandem mass spectrometry,QuEChERS/UPLC-MS/MS)测定雷公藤及根际土壤中辛硫磷、氯氰菊酯和乙基多杀菌素的含量。样品中加入适量的水浸润后用乙腈超声提取,N-丙基乙二胺(PSA)吸附净化,利用优化后的UPLC-MS/MS方法进行检测,基质外标法定量。结果显示,3种农药在根样基质中的检出限(LOD)为0.001~0.714μg/kg,定量限(LOQ)为0.002~2.380μg/kg;在土壤基质中的检出限(LOD)为0.002~0.810μg/kg,定量限(LOQ)为0.006~2.410μg/kg。线性关系、回收率和相对标准偏差均符合农药残留检测的相关规定。结果表明,该方法能满足雷公藤及根际土壤中3种农药残留含量的快速检测要求。QuEChERS pretreatment combined with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was developed and used to determine pesticide residues including phoxim,cypermethrin and spinetoram in T.wilfordii root and its rhizosphere soil to establish the method for detecting the content of three pesticide residues commonly used in the process of planting Tripterygium wilfordii.The sample was soaked with appropriate amount of water and then extracted by acetonitrile ultrasonic,purified by N-propyl ethylenediamine(PSA)adsorption,detected by optimized UPLCMS/MS method,and quantified by matrix external standard method.The results showed that the detection limit of pesticides in root like matrix was 0.001-0.714μg/kg,LOQ was 0.002-2.380μg/kg.The limit of detection(LOD)of three pesticides in root and soil samples was 0.001-0.714μg/kg and 0.002-0.810μg/kg,respectively.The limit of quantitation(LOQ)of three pesticides in root and soil samples was 0.002-2.380μg/kg and 0.006-2.410μg/kg,respectively.The linear relationship,recovery rate and relative standard deviation were in line with the relevant provisions of detecting pesticide residue.It is indicated that the method established is simple,rapid,sensitive and accurate,and can meet the requirements of rapidly determining three pesticide residues in Tripterygium wilfordii and rhizosphere related soil.

关 键 词：雷公藤 QUECHERS 超高效液相色谱-串联质谱 农药残留 快速检测 中草药 

分 类 号：S481.8[农业科学—农药学]