中国乳业2024,Issue(11) :120-132.DOI:10.12377/1671-4393.24.11.20

高效液相色谱法测定牛奶中黄曲霉毒素M1含量的方法验证研究

Method Validation Study for the Determination of Aflatoxin M1 Content in Milk by High Performance Liquid Chromatography

纪坤发 杨爱君 何瑛 杨美丰 利志锋 陈锦璇
中国乳业2024,Issue(11) :120-132.DOI:10.12377/1671-4393.24.11.20

高效液相色谱法测定牛奶中黄曲霉毒素M1含量的方法验证研究

Method Validation Study for the Determination of Aflatoxin M1 Content in Milk by High Performance Liquid Chromatography

纪坤发 1杨爱君 1何瑛 1杨美丰 1利志锋 1陈锦璇1
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作者信息

  • 1. 广东燕塘乳业股份有限公司,广东广州 510700
  • 折叠

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M1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M1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M1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.

Abstract

According to GB 5009.24—2016 National Standard for Food Safety,Determination of Aflatoxins M1 Group in Food,the second method was extracted by methanol-water solution,a method for the determination of aflatoxins M1 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 M1 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 0.00359 μg/kg,and that of the method was 0.00180 μg/kg,the quantitative limit of the instrument was 0.0108 μg/kg,the quantitative limit of the method was 0.00540 μg/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

Key words

high performance liquid chromatography/milk/aflatoxins M1/method validation

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出版年

2024
中国乳业
中国奶业协会 中国农业科学院信息研究所

中国乳业

影响因子:0.152
ISSN:1671-4393
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