乳粉中己烯雌酚分析标准样品的研制  

Development of standard sample for diethylstilbestrol analysis in milk powder

作　　者：段建华 赵静 白艳梅 吴晓莉 张立佳 胡雪 李翠枝 吕志勇 DUAN Jianhua;ZHAO Jing;BAI Yanmei;WU Xiaoli;ZHANG Lijia;HU Xue;LI Cuizhi;LYU Zhiyong(Inner Mongolia Yili Industrial Group Co.,Ltd.,Key Laboratory of Cattle and Sheep Milk and Meat Products Risk Control and Key Technology,State Administration for Market Regulation,Hohhot 010110,China)

机构地区：[1]内蒙古伊利实业集团股份有限公司,国家市场监督管理总局重点实验室(牛羊乳肉制品风险防控与关键技术),呼和浩特010110

出　　处：《化学分析计量》2025年第2期1-7,共7页Chemical Analysis And Meterage

摘　　要：研制乳粉基体己烯雌酚分析标准样品。筛选未检出己烯雌酚的进口全脂乳粉为原料,人工添加目标物,采用湿法-喷雾干燥工艺制备乳粉样品,选用双层包装,每包按10 g分装。采用液相色谱-串联质谱法进行均匀性、稳定性评估,协同9家实验室进行定值,评定特性值的测量不确定度。结果表明,该标准样品均匀性良好,稳定性达到18个月,特性值为12.8μg/kg,扩展不确定为0.8μg/kg(k=2)。该标准样品可用于乳粉中己烯雌酚含量检测和分析全程的质量保证与控制,以及对检测分析方法和检测能力的评价。A standard sample for the analysis of diethylstilbestrol in milk powder matrix was developed.The imported full-fat milk powder without diethylstilbestrol was selected as raw material,and the target substance was artificially added.The milk powder samples were prepared by wet-spray drying process,and double-layer packaging was selected,each package was packed at 10 g.The uniformity and stability were evaluated by liquid chromatography-tandem quadrupole mass spectrometry,and the measurement uncertainty of the characteristic values determined by 9 laboratories was evaluated.The results showed that the uniformity was good,the stability reached 18 months,the characteristic value was 12.8μg/kg,and the extended uncertainty was 0.8μg/kg(k=2).The standard sample can be used for quality assurance and control in the whole process of detection and analysis of diethylstilbestrol content in milk powder,as well as the evaluation of detection methods and detection capabilities.

关 键 词：乳粉 己烯雌酚 标准样品 均匀性 稳定性 定值 

分 类 号：O652[理学—分析化学]