液相色谱-串联质谱法同时测定丹参中139种农药残留  

Simultaneous Determination of 139 Pesticide Residues in Salvia miltiorrhiza by LC-MS/MS

作　　者：李雯婷[1] 苗水[1] 陈铭[1] 周恒[1] 兰岚[1] 毛秀红[1] 季申[1] Li Wenting;Miao Shui;Chen Ming;Zhou Heng;Lan Lan;Mao Xiuhong;Ji Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《世界中医药》2019年第4期783-792,797,共11页World Chinese Medicine

基　　金：广西壮族自治区科学技术厅重大专项计划(2015AC05038);国家中药标准化项目(ZYBZH-C-GX-09);国家药典委员会项目(ZG2016-2)

摘　　要：目的:采用液相色谱-串联质谱法建立丹参中农药多残留的测定方法。方法:样品经改良的QuEChERS方法提取,采用分散固相萃取(d-SPE)二次净化法净化,并采用液相色谱-串联质谱技术在多反应监测(MRM)模式下测定,内标法定量。结果:丹参中139种农药在0. 005～0. 2 mg/L范围内线性关系均良好;在10、50和100μg/kg添加水平下,除了噻菌灵回收率偏低(67. 2～67. 9)外,其余农药的平均回收率为70. 2%～126. 1%,相对标准偏差(RSD)为1. 2%～19. 5%,139种农药的检测限为0. 005～0. 05 mg/kg。结论:该方法样品前处理简单快速,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于丹参中139种农药残留的快速筛查测定。Objective: To study the multi-residues detection methods for Salvia miltiorrhiza by LC-MS/MS. Methods: A method using a modified QuEChERS and d-SPE clean-up followed by LC-MS/MS has been established for the quantitative determination of the residues.The extract was determined by LC-MS/MS in multi-reaction monitoring(MRM)mode,and internal standard method was applied to quantify the pesticides. Results: All the 139 pesticides showed good linearity in the range of 0.005~0.2 mg/L.The average recoveries of the pesticides at the spiked levels of 10,50,100 μg/kg ranged from 70.2~126.1% with the RSDs of 1.2~19.5%,except for Thiabendazole(67.2~67.9%).The limits of detection(LODs)of 139 pesticides were 0.005~0.05 mg/kg.The results demonstrated that this method was simple,rapid and suitable for the determination of 139 pesticide residues in Salvia miltiorrhiza. Conclusion: The analytical sensitivity and accuracy can meet the requirements of multiple pesticide residue analysis.

关 键 词：液相色谱-串联质谱法 农药残留 QuEChERS法 丹参 分散固相萃取 固相萃取 盐析剂 匀浆法 

分 类 号：R284.1[医药卫生—中药学]