高效液相色谱-串联质谱法同时测定地龙中4个黄曲霉毒素  

HPLC-MS/MS simultaneous determination of aflatoxins B_1,B_2,G_1 and G_2 in Pheretima

作　　者：杨小丽[1,2] 仇峰[1] 韦日伟[1,3] 覃禹[1,3] 杨美华[1] 欧阳臻[2] 

机构地区：[1]北京协和医学院药用植研究所中草药物质基础与资源利用教育部重点实验室,北京100193 [2]江苏大学药学院,镇江212013 [3]广西中医学院,南宁530001

出　　处：《药物分析杂志》2012年第4期627-630,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：科技部重大新药创制专项(2009ZX09502-025);国家中医药管理局2008年度中医药行业科研专项(200807042)

摘　　要：目的:建立同时测定地龙中4个黄曲霉毒素含量的高效液相色谱串联质谱法。方法:样品经甲醇-水(80∶20,v/v)提取,通过免疫亲和柱净化后,采用高效液相色谱串联质谱法测定其中4个黄曲霉毒素的含量,以多反应监测(MRM)方式分别监测离子对m/z 313→241(黄曲霉毒素B1,CE 50 eV),m/z 315→259(黄曲霉毒素B2,CE 43 eV),m/z 329→243(黄曲霉毒素G1,CE 38 eV)和m/z 331→245(黄曲霉毒素G2,CE 40 eV)。结果:黄曲霉毒素B1、B2、G1、G2的检测限分别为0.03,0.02,0.03,0.02μg.kg-1,回收率在88.0%～100.3%范围内,RSD均低于6.1%。结论:该方法快速、灵敏,结果准确,适用于地龙中4个黄曲霉毒素的同时检测。Objective：To establish a sensitive and accurate liquid chromatography-tandem mass spectrometry method（LC-MS/MS） for simultaneous determination of four aflatoxins in Pheretima.Methods：The samples were firstly extracted with methanol-water solution（80：20,v/v）,and then cleaned up by immunoaffinity columns.The mass spectrometer was operated in the positive ionization electrospray（ESI） mode using multiple reaction monitoring（MRM） for analysis of four aflatoxins.The transitions of m/z 313→241（aflatoxin B1,CE 50 eV）,m/z 315→259（aflatoxin B2,CE 43 eV）,m/z 329→243（aflatoxin G1,CE 38 eV） and m/z 331→245（aflatoxin G2,CE 40 eV） were used to quantify four aflatoxins,respectively.Results：The detection limits of aflatoxin B1,B2,G1 and G2 were 0.03,0.02,0.03 and 0.02 μg·kg-1,respectively.The recoveries of four analytes ranged from 88.0% to 100.3% and the relative standard deviations were all below 6.1%.Conclusion：The method is sensitive,simple and accurate,and proved to be suitable for the simultaneous determination of four aflatoxins in Pheretima.

关 键 词：有毒物质 致癌剂 黄曲霉毒素 动物药 地龙 含量测定 安全监测 高效液相色谱串联质谱法 免疫亲和柱净化 

分 类 号：R917[医药卫生—药物分析学]