摘要
目的建立何首乌中87种农药的液相色谱-串联质谱(LC-MS/MS)测定方法,并应用于53批何首乌样品的农药初步筛查,为何首乌安全性研究提供借鉴。方法样品经乙腈高速匀浆提取,采用LC-MS/MS,基质匹配法进行测定。质谱采用动态多反应监测模式(MRM)采集数据。结果87种农药及其代谢物共计100个指标线性关系良好,相关系数均大于0.99,加标回收率实验中全部指标回收率在70.4%~107.4%之间,RSD均小于11.40%,符合痕量测定的要求。53批何首乌样品中共检出3种农药,分别为多菌灵、啶虫脒和吡唑醚菌酯,残留量均低于0.01 mg·kg^(-1)。结论此方法检测指标包括LC-MS/MS检测的绝大多数禁用农药,方法灵敏度高、准确性好,可应用于何首乌中农药残留的筛查检测,可为基质类似中药材的农药残留检测方法提供借鉴参考。
Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of 87 types of pesticides and their metabolites in Polygonum Multiflori Radix in order to screen pesticides in 53 batches of samples of Polygonum Multiflori Radix,provide reference for safety study of Polygoni Multiflori Radix.Methods The samples were extracted with acetonitrile via high speed homogenate,concentrated and added with analytical protective agents before being determined with LC-MS/MS.The multi reaction monitoring mode(MRM)was used to collect data,and the blank matrix matching-protective agent standard was adopted for quantitative analysis to increase the accuracy and improve the peak shape.Results The calibration curves of all the targets showed good linearity with correlation coefficients of 0.99.The average recovery of the target compounds ranged from 70.4%to 107.4%at three spike levels,with relative standard deviations less than 11.40%,which met the requirements of trace determination.Carbendazim,acetamiprid and pyrazolidate were detected in 53 batches of samples of Polygonum Multiflori Radix,and the residues were all below 0.01 mg·kg^(-1).Conclusion The detection indicators of this method involve the vast majority of banned pesticides detected by LC-MS/MS.This method is highly sensitive and accurate so that it can be applied to the screening and detection of pesticide residues in Polygonum Multiflori Radix,which can provide reference for the detection of pesticide residues in similar Chinese herbal medicines.
作者
刘芫汐
辜冬琳
汪祺
姚令文
王莹
金红宇
马双成
LIU Yuanxi;GU Donglin;WANG Qi;YAO Lingwen;WANG Ying;JIN Hongyu;MA Shuangcheng(Institute for Control of Chinese Traditional Medicine and Ethnic Medicine,National Institutes for Food and Drug Control,Beijing 102629,China)
出处
《中国药物警戒》
2023年第6期601-608,共8页
Chinese Journal of Pharmacovigilance
基金
国家自然科学基金资助项目(81973476)。
关键词
何首乌
多菌灵
啶虫脒
吡唑醚菌酯
农药
液相色谱-串联质谱法
基质效应
多反应监测
安全性
Polygoni Multiflori Radix
carbendazim
acetamiprid
pyraclostrobin
pesticide residues
LC-MS/MS
matrix effect
multi-response monitoring mode(MRM)
safety
