HPLC-MS/MS法同时测定牛奶中黄曲霉毒素M_(1)和M_(2)  

Simultaneous Determination of Aflatoxins M_(1)and M_(2)in Milk by HPLC-MS/MS

作　　者：罗会兵 万方云 王玲莉 吴磊磊 双杨 LUO Huibing;WAN Fangyun;WANG Lingli;WU Leilei;SHUANG Yang(Powdery(Hubei)Health Industry Co.,Ltd.,Jingmen 431821;Shiyan Institute for Food and Drug Control,Shiyan 442000)

机构地区：[1]宝得瑞(湖北)健康产业有限公司,荆门431821 [2]十堰市食品药品检验检测所,十堰442000

出　　处：《食品工业》2024年第12期319-322,共4页The Food Industry

摘　　要：采用高效液相色谱-串联质谱法测定牛奶中黄曲霉毒素M_(1)和M_(2)。该方法用甲醇-水溶液提取,上清液用水稀释后,通过免疫亲和柱净化和富集,净化液浓缩、定容和过滤后经液相色谱分离,串联质谱检测,同位素内标法定量。结果显示,在0.05~5.0 ng/mL质量浓度范围内黄曲霉毒素M_(1)和M_(2)线性关系良好,线性相关系数均大于0.999,方法检出限为0.005μg/kg时,响应值均大于3,方法定量限为0.015μg/kg时,响应值均大于10。在0.05,0.25和0.50μg/kg质量分数水平上加标回收率为80.0%~114.0%,相对标准偏差(n=7)为2.31%~5.15%,满足方法验证要求。Aflatoxins M_(1) and M_(2)in milk by High-performance liquid chromatography tandem mass spectrometry are determined.This method extracts aflatoxins M_(1) and M_(2)from the sample by methanol water solution,and the extraction solution is diluted with water,purified and enriched through an immunoaffinity column.After concentration,constant volume and filtration of the purified liquid,it is separated by liquid chromatography,detected by tandem mass spectrometry and quantified by isotope internal standard method.The results showed that the linear relationship between the aflatoxins M_(1) and M_(2)was good in the concentration range of 0.05-5.0 ng/mL.The linear correlation coefficients were greater than 0.999.When the detection limit of the method was 0.005μg/kg,the response values of all three compounds were greater than 3.When the limit of quantification of the method was 0.015μg/kg,the response values of all three compounds were greater than 10.The recoveries were 80.0%-114.0%at the concentrations of 0.05,0.25 and 0.50μg/kg,and the relative standard deviations were 2.31%-5.15%(n=7).The results met the requirement of method verification.

关 键 词：高效液相色谱-串联质谱法 牛奶 黄曲霉毒素 

分 类 号：R28[医药卫生—中药学]