七叶神安滴丸UPLC指纹图谱和一测多评含量测定方法研究<sup>*</sup>

王京辉, 于密密, 陈晶, 王安琪, 房爽, 陈有根, 张云生, 傅欣彤, 郭洪祝

doi:10.16155/j.0254-1793.2024.03.03

药物分析杂志 >

2024 , Vol. 44 >Issue 3: 386 - 394

DOI: https://doi.org/10.16155/j.0254-1793.2024.03.03

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七叶神安滴丸UPLC指纹图谱和一测多评含量测定方法研究^*

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1.北京市药品检验研究院国家药品监督管理局中成药质量评价重点实验室中药成分分析与生物评价北京市重点实验室,北京 102206;
2.沃特世科技(北京)有限公司,北京 101111;
3.金七药业股份有限公司,云南 663100

第一作者王京辉 Tel:18010281092;E-mail:wangjinghui@bidc.org.cn
于密密 Tel:18010281099;E-mail:123171052@qq.com

^**郭洪祝 Tel:18010281003;E-mail:guohz@bidc.org.cn
傅欣彤 Tel:18010281078;E-mail:fuxintong68@163.com

收稿日期: 2024-02-26

网络出版日期: 2024-06-21

基金资助

^*国家药典委员会标准制修订研究课题(2020Z006)

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Study on UPLC fingerprint and quantitative analysis of multi-components by single marker of Qiye Shen'an dropping pills^*

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1. Beijing Institute for Drug Control, NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine), Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing 102206, China;
2. Waters Technologies Beijing Limited, Beijing 101111, China;
3. Jinqi Pharmaceutical Co., Ltd., Yunnan 663100, China

Received date: 2024-02-26

Online published: 2024-06-21

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摘要

目的: 建立七叶神安滴丸的超高效液相色谱(UPLC)指纹图谱鉴别方法,同色谱条件下完成一测多评法同时测定8个指标成分的含量。方法: 采用Waters CORTECS^®T3(150 mm×2.1 mm,1.6 μm)色谱柱,以乙腈-0.1%磷酸水为流动相进行梯度洗脱,流速0.40 mL·min^-1,柱温35 ℃,检测波长203 nm。结果: 建立七叶神安滴丸UPLC指纹图谱,确立了15个共有峰,15批样品相似度均大于0.99。并对其含量较高的8个成分人参皂苷Rb₁、人参皂苷Rc、三七皂苷Fc、人参皂苷Rb₂、人参皂苷Rb₃、人参皂苷Rd、三七皂苷Fe和三七皂苷Fd采用一测多评的方法进行含量测定,15批次样品每丸8个成分含量之和在7.6~10.0 mg。8个成分在相应浓度范围内与峰面积的线性关系良好,平均加样回收率分别为99.8%、99.7%、99.1%、99.4%、101.8%、102.0%、99.2%和100.2%,RSD分别为2.3%、2.2%、2.0%、1.5%、1.7%、1.2%、2.4%和2.6%。结论: 本研究建立的七叶神安滴丸的UPLC指纹图谱及一测多评的含量测定方法,操作简单,重复性好,稳定可靠,可为七叶神安滴丸的质量控制提供更加全面的依据。

关键词： 七叶神安滴丸; 三七叶总皂苷; 人参皂苷; 三七皂苷; 超高效液相色谱法; 指纹图谱; 一测多评; 含量测定

本文引用格式

王京辉, 于密密, 陈晶, 王安琪, 房爽, 陈有根, 张云生, 傅欣彤, 郭洪祝 . 七叶神安滴丸UPLC指纹图谱和一测多评含量测定方法研究^*[J]. 药物分析杂志, 2024 , 44(3) : 386 -394 . DOI: 10.16155/j.0254-1793.2024.03.03

Abstract

Objective: To establish the ultra high performance liquid chromatography (UPLC) fingerprint of Qiye Shen'an dropping pills, and to determine the contents of 8 index components by quantitative analysis of multi-components by single marker at the same time. Methods: Waters CORTECS^® T3 (150 mm×2.1 mm, 1.6 μm) chromatography column was used for gradient elution with acetonitrile-0.1% phosphoric acid as mobile phase, flow rate was 0.40 mL·min^-1, column temperature was 35 ℃, detection wavelength was 203 nm. Results: The UPLC fingerprint of Qiye Shen'an dropping pills was established, 8 common peaks were established, and the similarity of 15 batches of samples was greater than 0.99. Ginsenoside Rb₁, ginsenoside RC, panax notoginseng saponin FC, ginsenoside Rb₂, ginsenoside Rb₃, ginsenoside Rd, panax notoginseng saponin Fe and panax notoginseng saponin Fd were determined by quantitative analysis of multi-components by single marker method. The contents of 8 components in 15 batches were between 7.6-10.0 mg per pill. The average recoveries were 99.8%, 100.6%, 99.8%, 101.2%, 102.1%, 101.9%, 99.7% and 100.2% respectively, and the RSDs were 2.3%, 2.2%, 2.0%, 1.5%, 1.7%, 1.2%, 2.4% and 2.6% respectively. Conclusion: The UPLC fingerprint of Qiye Shen'an dropping pills and the content determination method of quantitative analysis of multi-components by single marker method established in this study are simple to operation, and have good repeatability, stability and reliability, and can provide a more comprehensive basis for the quality control of Qiye Shen'an dropping pills.

Key words： Qiye Shen'an dropping pills; total saponins from panaxnotpginseng stem and leaf; ginsenoside; panax notoginseng saponin; UPLC; fingerprint; quantitative analysis of multi-components by single marker; quality control

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