染料木苷纯度标准物质定值及不确定度评估

Characterization and uncertainty evaluation of genistin purity reference material

中文关键词:  染料木苷  纯度标准物质  质量平衡法  定量核磁法  不确定度评估

英文关键词:genistin  purity reference material  mass balance method  quantitative nuclear magnetic method  uncertainty evaluation

中文摘要:

      目的 建立纯度标准物质的2种定值方法并对染料木苷的纯度定值和不确定度进行评估。方法 采用液相色谱质谱法和核磁氢谱法对原料进行定性确证。质量平衡法中主要采用液相色谱-面积归一化法对原料的主成分进行定量分析, 然后采用微量水分测定仪测定原料中的水分, 采用顶空气相色谱法测定挥发性杂质, 采用电感耦合等离子质谱法测定金属元素杂质。定量核磁法采用一级纯度标准物质苯甲酸为内标, 经过方法优化, 通过不同位移上氢峰的面积比进行纯度定值。结果 2个方法定值结果均为99.72%, 质量平衡法的不确定度评估为0.19%, 定量核磁法的不确定度评估为0.09%。结论 建立的2种染料木苷纯度标准物质的定值方法准确、可靠, 不确定度评估合理, 适合大豆异黄酮类纯度标准物质的准确定值。

英文摘要:

      Objective To establish 2 kinds of methods for the characterization of pure certified reference material of and characterized the purity of genistin and evaluated the uncertainty. Methods The material was qualitatively confirmed by nuclear magnetic resonance (NMR) and mass spectrometric method. In mass balance method, the liquid chromatography-area normalization method was mainly used for quantitative analysis of the principal components of raw materials, and then the moisture was determined by trace moisture meter, volatile impurities were determined by headspace gas chromatography, and metal element impurities were determined by inductively coupled plasma mass spectrometry. Benzoic acid, the standard substance of primary purity, was used as the internal standard by quantitative NMR. After optimization, the purity was determined by the area ratio of hydrogen peak at different chemical shift. Results The value of the 2 kinds of methods was 99.72%, the uncertainty of the mass balance method and quantitative NMR was 0.19% and 0.09% respectively. Conclusion The established 2 kinds of methods are accurate and reliable, and the uncertainty evaluation is reasonable. It is suitable for the characterization of other soybean isoflavone pure materials.