苦杏仁苷纯度标准物质研制和纯度标准值及不确定度分析方法研究

Research on Value Assignment and Uncertainty Evaluation of Purity Reference Material of Amygdalin

目的研制具有溯源性、具备量值传递功能、高准确度量值的苦杏仁苷高纯度国家级有证标准物质,建立准确定量的定值分析方法。方法根据我国一级标准物质研制技术规范和国家计量相关法规要求,建立基于高效液相色谱(HPLC)面积归一化法和差示扫描量热法(DSC)的两种不同原理技术的苦杏仁苷纯度标准物质的标准值及不确定度评估联合定值方法。结果研制的苦杏仁苷纯度标准物质符合国家一级有证标准物质技术要求,其标准值及不确定度值为(99.3"0.4)%(k=2,P=0.95)。结论采用不同原理技术方法定值可有效克服一种技术的缺陷影响,保证苦杏仁苷纯度标准物质定值结果准确,该研究研制的国家一级有证标准物质,属国际公认的有证标准物质,它将为我国相关药品走向国际参与竞争市场提供了标准物质、物质标准、标准方法的科学依据。

Objective To develop the purity certified reference material of amygdalin which has traceability, value transmission and high-accuracy quantity value, and to establish an accurate definite value analytical method. Methods The purity value of purity certified reference material of amygdalin was determined by combined value assignment of high performance liquid chromatography （HPLC） area normalization method and differential scanning calorimetry （DSC） on the basis of Technical Norm of Primary Reference Material and related documents requirements. Results The developed purity certified reference material of amygdalin was in accordance with Technical Norm of Primary Reference Material requirements and the standard value and uncertainty was （99.3±0.4）% （k=2, P=0.95）. Conclusion The combined different principles analytical technology method could overcome the defects of one method and guarantee for the accurate value assignment results of the purity reference material of amygdalin in this study and it was an internationally accepted National Certified Reference Material which could provide reference material, material standard and scientific foundation of standard method for the international competition of related medicines.