成分分析

消乳散结胶囊多指标含量测定及化学计量学分析*

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  • 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
第一作者 Tel:(0531)81216527;E-mail:hshpipi@163.com
* 林永强 Tel:(0531)81216521;E-mail:13864067104@163.com
林慧彬 Tel:(0531)82949822;E-mail:linhuibin68@163.com

修回日期: 2020-05-20

  网络出版日期: 2024-07-15

基金资助

* 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)

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

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  • 1. NMPA Key Laboratory for Quality Evaluation of Gelatin Products,Shandong Provincial Institute for Food and Drug Control,Jinan 250101,China;
    2. Shandong Shenzhou Buchang Pharmaceutical,Co.,Ltd.,Heze 274000,China;
    3. Shandong University of Traditional Chinese Medicine,Jinan 250355,China;
    4. Shandong Academy of Chinese Medicine,Jinan 250014,China

Revised date: 2020-05-20

  Online published: 2024-07-15

摘要

目的:建立多指标含量测定结合化学计量学分析,评价消乳散结胶囊质量。方法:采用Hypersil GOLDC18色谱柱(250 mm× 4.6 mm,5 μm),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10 μL。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2.592~4.509、0.582~0.978、2.343~3.743、2.373~4.743、0.522~1.049、2.949~3.928 mg·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。

本文引用格式

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 . 消乳散结胶囊多指标含量测定及化学计量学分析*[J]. 药物分析杂志, 2021 , 41(4) : 594 -602 . DOI: 10.16155/j.0254-1793.2021.04.05

Abstract

Objective: To establish a method for overall quality evaluation of Xiaoru Sanjie capsules by multi-component determination and chemometric analysis. Methods: Separation was performed on a Hypersil GOLD C18(250 mm×4.6 mm,5 μm)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 10 μL. 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.

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