高效液相色谱法测定牛奶中黄曲霉毒素M_(1)含量的方法验证研究  

Method Validation Study for the Determination of Aflatoxin M_(1)Content in Milk by High Performance Liquid Chromatography

作　　者：纪坤发 杨爱君 何瑛 杨美丰 利志锋 陈锦璇 JI Kunfa;YANG Aijun;HE Ying;YANG Meifeng;LI Zhifeng;CHEN Jinxuan(Guangdong Yantang Dairy Co.,Ltd.,Guangzhou Guangdong 510700)

机构地区：[1]广东燕塘乳业股份有限公司,广东广州510700

出　　处：《中国乳业》2024年第11期120-132,共13页China Dairy

基　　金：广州市科技项目计划项目(2005Z3,2009Z1-E641,201508020021)。

摘　　要：根据《GB 5009.24—2016食品安全国家标准食品中黄曲霉毒素M族的测定》第二法,采用甲醇-水溶液提取,免疫亲和柱净化富集作为牛奶中黄曲霉毒素M_(1)检测前处理方法,建立高效液相色谱法测定牛奶中黄曲霉毒素M_(1)含量的方法,并从检出限、定量限、线性范围、正确度、重复性精密度5个方面对方法进行验证。结果显示,牛奶中黄曲霉毒素M_(1)在0.00250~2.02 ng/mL浓度范围内线性良好,相关系数大于0.999,仪器检出限0.00359μg/kg、方法检出限0.00180μg/kg,仪器定量限0.0108μg/kg,方法定量限0.00540μg/kg,回收率95.80%~103.37%,重复性精密度0.46%~1.66%,符合《GB 5009.295—2023食品安全国家标准化学分析方法验证通则》要求。According to GB 5009.24—2016 National Standard for Food Safety,Determination of Aflatoxins M_(1)Group in Food,the second method was extracted by methanol-water solution,a method for the determination of aflatoxins M_(1)in milk by high performance liquid chromatography with high performance liquid chromatography was developed,the detection limit,quantitative limit,linear range,accuracy and repeatability precision were tested.The results showed that the aflatoxins M_(1)in milk had a good linearity in the range of 0.00250~2.02 ng/mL,and the correlation coefficient was larger than that of the 0.999.The detection limit of the instrument was 0.00359μg/kg,and that of the method was 0.00180μg/kg,the quantitative limit of the instrument was 0.0108μg/kg,the quantitative limit of the method was 0.00540μg/kg,the recoveries were 95.80%~103.37%,the repeatability precision was 0.46%~1.66%,all accord GB 5009.295—2023 The Requirements of National Standard for Food Safety General Rules for Verification of Chemical Analysis Methods.

关 键 词：高效液相色谱法 牛奶 黄曲霉毒素M1 方法验证 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.72[轻工技术与工程—食品科学与工程]