色谱指纹图谱全定性相似度和全定量相似度质控体系研究

Quality control system of overall qualitative similarities and overall quantitative similarities of chromatographic fingerprints

目的对中药色谱指纹图谱的全定性相似度和全定量相似度质控体系进行研究。方法用银杏叶提取物的HPLC指纹图谱实验结果为例,分别从化学成分分布相似性和含量相似性2个方面评价不同批次银杏叶提取物与对照指纹图谱的相似程度。提出用SF和S′F构成全定性相似度法来准确地解决色谱指纹图谱的定性评价问题;用W%与R%,C%与P%,Q%与M%,以及QF%与MF%分别构成第一、第二、第三、第四级全定量相似度。评价时,全定性相似度均〉0.9为必要条件,上述4种全定量相似度可选择任意1组,制剂控制在90%-110%,原料控制在85%-120%,组内相差不得超过10%为合格。结果当全定性相似度和全定量相似度合格时,一方面可保证削减大指纹峰影响,等权对待小指纹峰贡献;另一方面,从突出大指纹峰对体系的作用出发进行评价,这样能同时兼顾检测所有指纹峰对体系的定性定量的贡献作用。结论全定性相似度和全定量相似度的密切结合构成色谱指纹图谱新的质控体系,是利用色谱指纹图谱宏观控制中药质量的最佳方法。

Objective To determine the quality control system of both the overall qualitative similarities and the overall quantitative similarities of traditional Chinese medicine chromatographic fingerprints. Methods Taking the HPLC fingerprints of ginkgo biloba extract for example, the similarities of both the distribution proportion of chemical instituents and their contents were evaluated between the different batches of samples and the reference fingerprints. The overall qualitative similarities in which the similarity of cosine of angle SF was combined with the qualitative similarity of peak area ratio S＇F were proposed to accurately solve the qualitative assessment problem of chromatographic fingerprints. The percentage of module lengths W% combining the apparent quantitative similarity R%, the quantitative similarity calculated by vector shadow C% combining the quantitative similarity P%, the content similarity Q% combining the average percentage of mass M%, and the correction content similarity QF % combining the average correction percentage of mass MF %, respectively, to compose the first, second, third and the fourth overall quantitative similarities. During the evaluation, that both SF and S＇F were more than 0.9 was the required condition and any one of the above four pairs of quantitative similarities was selected to assess the characteristics of instituent contents, in which the pair mentioned above should be within 90%-110% for prescribed dosages, and 85%-120% for crude herbal drugs, respectively, and the differences should be less than 10% between each pair. If the results meet the requirements, we can regard the samples as qualified. Results When both the overall qualitative similarities and the overall quantitative similarities met the requirements, firstly, the important influence of big. fingerprints was cancelled and the small fingerprints were dealt with the same weight. Secondly, we emphasized the influence of the big fingerprints, and thus we could simultaneously determine the contributions of all fingerprints to the system. Conclusion A novel assessment method of chromatographic fingerprints is set up by both the overall qualitative similarities and the overall quantitative similarities,which can be used to objectively, authentically and thoroughly disclose how similar it is between the sample and the referential fingerprints, and how close the contents are between them. The quality control system of both the overall qualitative similarities and the overall quantitative similarities of chromatographic fingerprints will prove to the best of all evaluation methods.