高效液相色谱-串联质谱法测定中药材麦冬中74种农药残留  

Determination of 74 pesticide residues in Radix Ophiopogonis by high performance liquid chromatography-tandem mass spectrometry

作　　者：刘佳铭 李雯婷[2] 陈铭[2] 周恒[2] 兰岚[2] 曹佳音 苗水[2] 毛秀红[2] 季申[2] LIU Jiaming;LI Wenting;CHEN Ming;ZHOU Heng;LAN Lan;CAO Jiayin;MIAO Shui;MAO Xiuhong;JI Shen(China State Institute of Pharmaceutical Industry,Shanghai 201203;Shanghai Institute for Food and Drug Control,National Medical Products Asministration Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai 201203;Shanghai Institute of Pharmaceutical Industry,Shanghai 201203;Shanghai University of Traditional Chinese Medicine,Shanghai 201203)

机构地区：[1]中国医药工业研究总院,上海201203 [2]上海市食品药品检验所国家药品监督管理局中药质量控制重点实验室,上海201203 [3]上海医药工业研究院,上海2012034 [4]上海中医药大学,上海201203

出　　处：《分析试验室》2020年第7期826-833,共8页Chinese Journal of Analysis Laboratory

基　　金：中药材外源性有毒有害物质检测及控制标准研究项目(2017YFC1700800);上海市中药和保健食品品种与安全检测专业技术服务平台项目(18DZ2292200);中药外源性有毒有害物质检测关键技术研究与标准制订项目(18DZ2200900)资助。

摘　　要：采用高效液相色谱-串联质谱(HPLC-MS/MS)技术建立了同时检测麦冬中74种农药残留的方法,其中大多数是植物生长调节剂。基于甲酸铵-甲酸缓冲体系的改良QuEChERS提取方法,实现对不同理化性质的植物生长调节剂类农药残留的高通量提取;采用正负离子切换的质谱扫描模式对74种化合物实现了单次进样的同时监测,并引入同位素内标辅助定量。所建立的方法按照欧盟标准SANTE/11813/2017进行方法学验证,74种化合物线性关系良好(R^2>0.99),定量限在5~50μg/kg之间,100μg/kg加标水平下回收率在63.7%~114.1%之间,精密度均小于20%,所建立的方法满足欧盟方法学考察相关要求。采用该法对13批麦冬中的植物生长调节剂残留进行检测,并对测定结果进行了分析。A method of high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established for the simultaneous determination of 74 pesticide residues in Ophiopogon japonicus,most of which were plant growth regulators(PGRs).For sample extraction,modified Qu EChERS based on ammonium formateformic acid buffer solution system was established for high-throughput extraction of PGRs and pesticide residues with various physical and chemical properties.For the detection,74 compounds were simultaneously monitored by single injection using a mass spectrometry acquisition method including both positive and negative experiments.Isotope internal standards were used for quantitative analysis.Method validation was carried out according to the European Commission guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed(SANTE/11813/2017).74 compounds showed good linearities with R^2>0.99.The limits of quantification of most compounds were between 5-50μg/kg.The recoveries ranged from 63.7%to 114.1%with a precision less than 20%at 100μg/kg spiked level.The validation results showed that the method met the requirements of SANTE/11813/2017.The residues of PGRs in 13 batches of Ophiopogon japonicus were detected by this method.

关 键 词：麦冬 植物生长调节剂残留量 改良QuEChERS法 高效液相色谱串联质谱 

分 类 号：R932[医药卫生—生药学] O657.6[医药卫生—药学]