基于液质联用对《中国药典》(2020版)禁用农药多残留测定法的探讨  

Discussion on the multi-residue detection method for banned pesticides in Chinese Pharmacopoeia(2020 edition)based on LC-MS/MS

作　　者：童婷婷 冀晓雯[1] 廖苏奇 付金娥[1,3] 夏祥华 TONG Tingting;JI Xiaowen;LIAO Suqi;FU Jin'e;XIA Xianghua(Guangxi Botanical Garden of Medicinal Plants,Nanning 530023,China;National Engineering Laboratory for Development of Endangered Medicinal Materials Resources in Southwest China,Nanning 530023,China;Key Laboratory of Guangxi for High-quality Formation and Utilization of Dao-di Herbs,Nanning 530023,China)

机构地区：[1]广西壮族自治区药用植物园,南宁530023 [2]西南濒危药材资源开发国家工程实验室,南宁530023 [3]广西道地药材高品质形成与应用重点实验室,南宁530023

出　　处：《农药》2024年第3期196-203,223,共9页Agrochemicals

基　　金：广西中药材品质创新研究团队(GZKJ2305)。

摘　　要：[目的]探讨《中国药典》(2020版)禁用农药多残留测定法。[方法]以《中国药典》(2020版)禁用农药多残留测定法为检测方法,选择适用于液质联用测定的29个禁用农药,以党参为基质对检测方法进行验证,测定根类(党参)、叶类(杜仲叶)、花类(槐米)、果类(化橘红)4种中药材的禁用农药残留情况,并对测定结果进行比较分析。[结果]各禁用农药在各自范围内线性关系良好(r>0.993),方法定量限(LOQ)在0.1~9.7μg/kg之间,平均加标回收率为65.1%~107.2%,精密度RSD为0.5%~9.0%。同一种农药在不同药材基质中,基质效应差别不大;不同性质的中药材、不同的前处理方法对除杂效果及回收率的影响较大。[结论]使用《中国药典》(2020版)禁用农药多残留测定法时,建议对药材进行分类分级,丰富通用技术要求,期望对中药材禁用农药的分析检测提供借鉴和参考。[Aims] Discussion on the detection method for multi-residue of banned pesticides in Chinese Pharmacopoeia(2020 edition). [Methods] Based on the detection method for banned pesticides multi-residue in Chinese Pharmacopoeia(2020 edition), 29 banned pesticides suitable for LC-MS/MS were selected and tested with Codonopsis radix as matrix, the residues of banned pesticides in roots(CODONOPSIS RADIX), leaves(EUCOMMIAE FOLIUM), flowers(SOPHORAE FLOS) and fruits(CITRI GRANDIS EXOCARPIUM) were determined, then the results were compared and analyzed. [Results] The linear relationship of the banned pesticides was good(r>0.993). The limit of quantification(LOQ) was 0.1-9.7 μg/kg. The average recovery was 65.1%-107.2%and the RSD was 0.5%-9.0%. The matrix effect of the same pesticide had little difference among different materials,and the effect of different materials and different pretreatment methods on impurity removal and recovery were obvious. [Conclusions] When the detection method for banned pesticides multi-residue in Chinese Pharmacopoeia(2020 edition) is used, it is suggested to classify the medicinal materials and enrich the general technical requirements, expected to provide reference for the analysis and detection of banned pesticides in Chinese medicinal materials.

关 键 词：禁用农药多残留 液相色谱-串联质谱法 党参 基质效应 

分 类 号：TQ450.2[化学工程—农药化工]