消乳散结胶囊多指标含量测定及化学计量学分析  

Multi-component determination and chemometric analysis of Xiaoru Sanjie capsules by HPLC

作　　者：许丽丽 林林 于凤蕊 崔伟亮 徐兴燕 王明耿 林玉梅 崔巧红 李军 林永强 林慧彬[4] XU Li-li;LIN lin;YU Feng-rui;CUI Wei-liang;XU Xing-yan;WANG Ming-geng;LIN Yu-mei;CUI Qiao-hong;LI Jun;LIN Yong-qiang;LIN Hui-bin(NMPA Key Laboratory for Quality Evaluation of Gelatin Products,Shandong Provincial Institute for Food and Drug Control,Jinan 250101,China;Shandong Shenzhou Buchang Pharmaceutical,Co.,Ltd.,Heze 274000,China;Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Academy of Chinese Medicine,Jinan 250014,China)

机构地区：[1]山东省食品药品检验研究院,国家药品监督管理局胶类产品质量评价重点实验室,济南250101 [2]山东步长神州制药有限公司,菏泽274000 [3]山东中医药大学,济南250355 [4]山东省中医药研究院,济南250014

出　　处：《药物分析杂志》2021年第4期594-602,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家重点研发计划“中医药现代化研究”重点专项(2017YFC1701500、2017YFC1701502、2017YFC1701504、2017YFC1702700、2017YFC1702701);山东省自然科学基金(ZR2017MH023、ZR2018PH040);泰山学者工程(NO.ts201511107);2018国家中医药管理局全国中药资源普查项目(GZYKJS-2018-004);山东省中医药科技发展计划(2017-519、2019-0988、2019-0987);重大新药创制子课题贞芍醇苷胶囊制备工艺及质量标准研究(2017ZX09301064010)。

摘　　要：目的:建立多指标含量测定结合化学计量学分析,评价消乳散结肢囊质量。方法:采用Hypersil GOID C18色谱柱(250 mm×4.6 mm,5μm),乙腈(A)-0.2%磷酸水溶液(B)为流动相,梯度洗脱,流速1 mL·min^(-1),检测波长230 nm。柱温25℃,进样量10μL。结果:消乳散结胶囊中芍药苷、迷迭香酸、黄芩苷、丹酚酸B、汉黄芩苷、丹皮酚的色谱峰均能达到基线分离,线性关系良好,平均回收率分别为100.0%、97.8%、99.7%、97.6%、97.4%、100.3%,RSD均≤2.0%。该方法的精密度、稳定性、重复性良好。13批消乳散结胶囊中上述6个成分的含量测定结果分别为2.5924.509、0.5820.978、2.3433.743、2.3734.743、0.5221.049、2.9493.928mg·g^(-1)。化学计量学分析表明不同批次产品存在一定差异,区分各类样品的强特征峰为芍药苷、丹酚酸B和黄芩苷。结论:建立的综合质量评价法准确、专属,可用于消乳散结胶囊的质量控制。Objective:To establish a method for overall quality evaluation of Xiaoru Sanjie capsules by multicomponent determination and chemometric analysis.Methods:Separation was performed on a Hypersil GOLD C18(250 mm×4.6 mm,5μm)column.The mobile phase was acetonitrile-0.2%phosphoric acid at a flow rate of 1 mL·min-1 with gradient elution.The column temperature was 25℃and the injection volume was 10μL.The detection wavelength was set at 230 nm.Results:The six markers reached baseline separation,the linearity was good and the average recoveries were 100.0%,97.8%,99.7%,97.6%,97.4%and 100.3%,respectively with RSDs less than 2.0%.Precision,stability and reproducibility of the method were satisfactory.The contents of the above six components in 13 batches of sample were 2.592-4.509,0.582-0.978,2.343-3.743,2.373-4.743,0.522-1.049 and 2.949-3.928 mg·g^(-1),respectively.Chemometric analysis showed that there were some differences among the samples from different years.Significant characteristic peaks for discrimination of different samples were paeoniflorin,salvianolic acid B and paeonol.Conclusion:The method is accurate and specific,which can be used for the quality control of Xiaorusanjie capsules.

关 键 词：消乳散结胶囊 白芍 牡丹皮 丹参 夏枯草 黄芩 芍药苷 迷迭香酸 黄芩苷 丹酚酸B 汉黄芩苷 丹皮酚 高效液相色谱法 化学计量学 

分 类 号：R917[医药卫生—药物分析学]