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当前位置: 首页 > 文章 > 多功能柱净化液相色谱–质谱–质谱法测定牛奶中黄曲霉毒素M_1 现代农药 2011,10 (4) 38-40
Position: Home > Articles > Multifunctional Column Clean-up and Determination of Aflatoxin M_1 in Milk by Liquid Chromatography-tandem Mass Spectrometry Modern Agrochemicals 2011,10 (4) 38-40

多功能柱净化液相色谱–质谱–质谱法测定牛奶中黄曲霉毒素M_1

作  者：
董彬;杨立新;李斌;刘印平;曾凡刚
单  位：
河北省疾病预防控制中心;中国人民大学环境学院
关键词：
黄曲霉毒素M1;牛奶;多功能柱;液质联用技术
摘  要：
建立了简单、快速测定牛奶中黄曲霉毒素M1的液相色谱–质谱–质谱确证方法。样品经乙腈/水溶液(V/V,86/14)提取,226多功能柱净化,离心、吹干、定容和过滤,高压液相Xtera色谱柱(150 mm×2.1 mm×5μm)分离,选用0.1%甲酸溶液和乙腈/甲醇(V/V,50/50)作为流动相,采用外标法定量。结果经方法学研究验证,LOD=0.15 ng/mL,LOQ=0.5 ng/mL,线性相关系数R=0.9961;两种浓度加标回收率为71.5%和83.5%,相对标准偏差为2.7%和8.4%。该方法具有预处理简单、检测速度快、灵敏度高的优点,可适用于牛奶中黄曲霉毒素M1的确认和准确定量检测。
译  名：
Multifunctional Column Clean-up and Determination of Aflatoxin M_1 in Milk by Liquid Chromatography-tandem Mass Spectrometry
作  者：
DONG Bin1,YANG Li-xin1,LI Bin2,LIU Yin-ping1,ZEN Fan-gang2(1.Hebei Center of Disease Control and Prevention,Shijiazhuang 050021,China;2.School of Environment and Natural Resources,Renmin Univercity of China,Beijing 100872,China)
关键词：
aflatoxin M1;milk;multifunctional column;LC-MS/MS
摘  要：
A simple and rapid determination method of aflatoxin M1 in milk by liquid chromatography-tandem mass spectrometry has be established.The samples were extracted by acetonitrile/water(V/V,86/14),226 multi-function columns were used as purification technology.After centrifugation,drying,constant-volume and filtration,the samples were detected by liquid chromatography-tandem mass spectrometry with C18 column(Waters,Xtera,150 mm×2.1 mm×5 mm).0.1% Formic acid and acetonitrile/methanol(V/V,50/50) were selected as mobile phases.The samples were detected by external standard method.The results of methodology verification were as follows: LOD=0.15 ng/mL,LOQ=0.5 ng/mL,the linear correlation R=0.996 1.The recovery experiments were performed by blank sample spiked at the two levels,the recoveries were 71.5% and 83.5%,with the relative standard deviations(RSD,n=6) were 2.7% and 8.4%.The advantages of this method included simple pre-treatment,high speed and sensitivity.It was suitable for aflatoxin M1 detection in milk.

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