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  

Multifunctional Column Clean-up and Determination of Aflatoxin M_1 in Milk by Liquid Chromatography-tandem Mass Spectrometry

作　　者：董彬[1] 杨立新[1] 李斌[2] 刘印平[1] 曾凡刚[2] 

机构地区：[1]河北省疾病预防控制中心,石家庄050021 [2]中国人民大学环境学院,北京100872

出　　处：《现代农药》2011年第4期38-40,共3页MODERN AGROCHEMICALS

基　　金：中国人民大学亚洲研究中心资助项目(20072003)

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。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.

关 键 词：黄曲霉毒素M1 牛奶 多功能柱 液质联用技术 

分 类 号：O657.63[理学—分析化学] TS252.2[理学—化学]