奶粉中睾酮和甲睾酮基体标准物质的定值及不确定度评定

Certification and Uncertainty Evaluation of Testosterone and Methyltestosterone Matrix Reference Material in Milk Powder

建立了奶粉中睾酮和甲睾酮的同位素稀释质谱高准确度测量方法,对样品前处理方法和基质效应进行优化和考察,结果表明同位素稀释质谱和溶液稀释法可以有效减少基质效应对检测的影响,显著提高分析效率。应用该方法对奶粉中睾酮和甲睾酮基体标准物质进行均匀性检验和准确定值,并对不确定度进行详细评估。奶粉中睾酮和甲睾酮均匀性良好,特性量值分别为(19.4±1.4)μg/kg(k=2)、(21.0±1.4)μg/kg(k=2)。标准物质适用于质量控制、检测方法开发、实验室能力验证等领域。

A highly accurate method for the determination of testosterone and methyltestosterone in milk powder by isotope dilution mass spectrometry was developed,and the sample pretreatment methods and matrix effects were optimized.The result shows that isotope dilution mass spectrometry and solution dilution methods could effectively reduce the influence of matrix effects and significantly improve the analytical efficiency.The method was applied to test the homogeneity and accurately,determine the values of testosterone and methyltestosterone in milk powder,and the uncertainties were evaluated in detail.The homogeneities of testosterone and methyltestosterone in milk powder were good,with characteristic values of(19.4±1.4)μg/kg(k=2)and(21.0±1.4)μg/kg(k=2),respectively.This standard is suitable for quality control,assay development,laboratory proficiency testing and other fields.