金银花质量标准中木犀草苷含量测定方法探讨及不确定度分析

Discussion on the Determination Method and Uncertainty of Luteolin in the Current Quality Standard of Lonicerae Japonicae Flos

目的:探讨金银花现行质量标准中木犀草苷的含量测定方法的测量不确定度,为完善金银花药材及饮片的质量标准提供参考。方法:采用《中国药典》2020年版中金银花项下含量测定方法,测定金银花饮片中木犀草苷的含量,并评估方法的测量不确定度及其对检验结果判定的影响。结果:实验发现,按照《中国药典》2020年版四部高效液相色谱法的色谱参数调整要求,调整流动相比例,同批次金银花样品的木犀草苷含量测定结果存在差异。金银花中木犀草苷含量测定结果为(0.048±0.015)%(置信概率为95%,k=2)。结论:通过评估方法的测量不确定度发现,色谱参数调整是本实验贡献最大的不确定度分量,调整前后测定结果差异较大,并影响检验结果的符合性判定,金银花药材及饮片中木犀草苷的含量测定方法亟需完善和修订。

Objective:To explore the measurement uncertainty of the content determination method luteolin in the current quality standard of Lonicerae Japonicae Flos.Methods:The content of luteolin was determined using the method specified in the Chinese Phar-macopoeia 2020 edition for Lonicerae Japonicae Flos.The measurement uncertainty of the method was calculated and its impact on the judgment of the inspection results was evaluated.Results:The experimental results indicate that there are differences in the determination results of luteolin content in the same batch of Lonicerae Japonicae Flos samples after adjusting the mobile phase ratio in accordance with the chromatographic parameter adjustment requirements of high-performance liquid chromatography in the Chinese Pharmacopoeia 2020 edition volumeⅣ.The determination result of luteolin content in Lonicerae Japonicae Flos was(0.048±0.015)%(the confidence prob-ability was 95%,k=2).Conclusion:The measurement uncertainty results of the method indicate that the adjustment of chromatographic parameters contributes the most to the uncertainty component of this experiment.There is a significant difference in the determination results before and after the adjustment of chromatographic parameters,which affects the conformity judgment of the test results.The deter-mination method of luteolin in Lonicerae Japonicae Flos needs to be improved and revised.