三七中二硫代氨基甲酸酯(盐)类杀菌剂及其代谢物残留量测定  

Determination of fungicidal dithiocarbamates and the metabolites in Panax notoginseng

作　　者：兰岚[1,2] 周恒 袁佳佳[1,2] 陈铭 苗水 季申[1,2] LAN Lan;ZHOU Heng;YUAN Jia-jia;CHEN Ming;MIAO Shui;JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China;NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203 [2]国家药品监督管理局中药质量控制重点实验室,上海201203

出　　处：《中成药》2020年第10期2656-2661,共6页Chinese Traditional Patent Medicine

基　　金：国家中药标准化项目(ZYBZH-C-GX-09);国家药品医疗器械审评审批制度改革课题(ZG2016-2-02);上海市科技人才计划项目(17YF1417100);2018上海科委研发平台专项(18DZ2292200)。

摘　　要：目的测定三七中二硫代氨基甲酸酯(盐)类杀菌剂及其2种残留物乙撑硫脲和丙撑硫脲的含有量。方法采用顶空气相色谱-串联质谱(HS/GC-MS)分析二硫代氨基甲酸酯(盐)类杀菌剂的残留总量(以二硫化碳计),乙撑硫脲和丙撑硫脲的残留量采用QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)测定。结果在优化的前处理方法下,二硫化碳在0.02~4.0μg范围内线性关系良好(r=0.9963),加样回收率及RSD均符合农残检测要求,方法定量限为0.02 mg/kg。2种代谢物在0.005~0.4 mg/L范围内线性关系良好(r>0.9900),回收率80.4%~92.6%,RSD均小于10%,方法定量限均为0.005 mg/kg。结论该方法可用于三七中二硫代氨基甲酸酯(盐)类杀菌剂及乙撑硫脲和丙撑硫脲残留的日常检验。AIM To determine the content of dithiocarbamates, and the metabolites ethylenethiourea(ETU) and propylenethiourea(PTU) in Panax notoginseng(Burk.) F. H. Chen. METHODS The total residue of dithiocarbamates was determined as carbon disulfide(CS2) by headspace gas chromatography-mass spectrometry(HS/GC-MS). Residual analysis of ETU and PTU were performed by the method of QuEChERS combined with ultra-high performance liquid chromatography tanderm mass spectrometry(UPLC-MS/MS). RESULTS Under optimized conditions, CS2 showed good linear relationships within the range of 0.02-4.0 μg(r=0.996 3). The recoveries and RSDs met the requirements of pesticide residue detection. The limit of quantification(LOQ) was 0.02 mg/kg. The two metabolites showed good linear relationships within the range of 0.005-0.4 mg/L(r>0.990 0). The recoveries were 80.4%-92.6% with the RSDs of less than 10%. The LOQs of ETU and PTU were both 0.005 mg/kg.CONCLUSION This method can be used for the residual evaluation of dithiocarbamates and the metabolites in the routine analysis.

关 键 词：三七 二硫代氨基甲酸酯(盐) 乙撑硫脲 丙撑硫脲 HS/GC-MS QuEChERS/UPLC-MS/MS 

分 类 号：R284.1[医药卫生—中药学]