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 |
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引用本文: | 杨小丽,仇峰,韦日伟,覃禹,杨美华,欧阳臻.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[J].药物分析杂志,2012(4):627-630. |
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作者姓名: | 杨小丽 仇峰 韦日伟 覃禹 杨美华 欧阳臻 |
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作者单位: | 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;江苏大学药学院;广西中医学院 |
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基金项目: | 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) |
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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。
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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 |
HPLC-MS/MS simultaneous determination of aflatoxins B1,B2,G1 and G2 in Pheretima |
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Affiliation: | YANG Xiao-li1,2,QIU Feng1,WEI Ri-wei1,3,QIN Yu1,3,YANG Mei-hua1,OU-YANG Zhen2(1.Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine,Ministry of Education,Institute of Medicinal Plant Development,Peking Union Medical College,Beijing 100193,China;2.School of Pharmacy,Jiangsu University,Zhenjiang 212013,China; 3.Guangxi Traditional Chinese Medical University,Nanning 530001,China) |
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Abstract: | 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. |
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Keywords: | poisonous substance carcinogen aflatoxins animal medicine Pheretima assay safety monitoring LC-MS/MS immunoaffinity column clean-up |
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