地龙药材中六溴环十二烷三种异构体残留量的测定和风险评估  

Determination and Risk Assessment of Hexabromocyclododecane Residues in Traditional Chinese Medicine Pheretima

作　　者：孙晶 蒋丹艺 曹玲 倪倩 冯有龙 洛丹 唐丹瑞 SUN Jing;JIANG Danyi;CAO Ling;NI Qian;FENG Youlong;LUO Dan;TANG Danrui(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;China Pharmaceutical University,Nanjing 211198,China;Center for Inspection,Jiangsu Medical Products Administration,Nanjing 210019,China;Nanjing University of Chinese Medicine,Nanjing 210023,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210019 [2]中国药科大学中药学院,南京211198 [3]江苏省药品监督管理局审核查验中心,南京210019 [4]南京中医药大学药学院,南京210023

出　　处：《药学与临床研究》2024年第3期198-203,共6页Pharmaceutical and Clinical Research

基　　金：江苏省药品监督管理局科研计划项目(202205);江苏省市场监督管理局科技计划项目(KJ2023028)。

摘　　要：目的:建立一种高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定地龙药材中新污染物六溴环十二烷(HBCDs)3种异构体残留量,并评估其健康风险。方法:取地龙药材细粉,加入^(13)C_(12)-α-HBCD、^(13)C_(12)-β-HBCD和^(13)C_(12)-γ-HBCD内标溶液,经超声提取复合硅胶柱净化后,采用液相色谱串联质谱多反应监测,内标法定量。结果:HBCDs 3种立体异构体线性关系良好(r2>0.999),检出限和定量限分别约为2和6 pg·g^(-1),平均回收率为97%~120%,RSD为7.1%~7.4%,精密度为1.1%~7.4%(n=6)。78批地龙药材中有73批检出HBCDs,检出率为94%,其中以α-HBCD的含量最高。使用欧洲食品安全局建议的暴露边界值法对地龙药材中HBCDs的风险评估表明,经地龙药材摄入的HBCDs引起健康问题的风险较小。结论:建立的地龙药材中新污染物HBCDs残留量的液相色谱-串联质谱测定法灵敏、准确、可靠,适用于地龙药材中HBCDs残留量的定量分析,可为中药材外源性新污染物的安全监测提供科学参考。Objective:To establish a method for residue determination of three isomers of hexabromocyclododecanes(HBCDs)in traditional Chinese medicine Pheretima and to assess associated health risks of these emerging pollutants.Methods:The traditional Chinese medicine Pheretima powder samples were taken and added with internal standard solutions of ^(13)C_(12)-α-HBCD,^(13)C_(12)-β-HBCD,and ^(13)C_(12)-γ-HBCD.After ultrasonic extraction and purification with composite silica gel columns,samples were determined by high performance liquid chromatography-tandem mass spectrometry with multiple reaction monitoring for quantification of the three isomers by an internal standard method.Results:The three target HBCDs stereo-isomers exhibited good linearity(r2>0.999),with detection and quantification limits of approximately 2 pg·g^(-1)and 6 pg·g^(-1),respectively.The average recovery rates of the target substances ranged from 97%to 120%,with RSDs from 7.1%to 7.4%,and precisions between 1.1%and 7.4%(n=6).Out of 78 batches of Pheretima,HBCDs were detected in 73 batches,giving a detection rate of 94%,withα-HBCD being the most abundant congener.Risk assessment of HBCDs in Pheretima using the Margin of Exposure(MOE)approach recommended by the European Food Safety Authority(EFSA)indicated that the risk of health issues arising from the intake of HBCDs through Pheretima wss minimal.Conclusion:The established method is sensitive,accurate,and reliable.It is suitable for the quantitative analysis of HBCDs residues in Pheretima and can provide a scientific reference for the safety monitoring of exogenous emerging pollutants in traditional Chinese medicine.

关 键 词：地龙 中药材 六溴环十二烷 残留量 高效液相色谱-串联质谱法 风险评估 

分 类 号：R927.11[医药卫生—药学]