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中国药物评价 ›› 2024, Vol. 41 ›› Issue (3): 198-203.

• 评价技术与方法 • 上一篇    下一篇

HPLC-一测多评法测定参葛补肾胶囊中 总黄酮醇苷的含量

   李成功1, 胡时先1, 任宾1, 潘树球2, 徐海燕1, 王涵斌1, 郝娟1*   

  1. 1.新疆华春生物药业股份有限公司, 新疆 乌鲁木齐 830000; 

    2.国药集团德众(佛山)药业有限公司, 广东 佛山 528000

  • 收稿日期:2023-12-11 修回日期:2024-04-03 出版日期:2024-06-28 发布日期:2024-06-28
  • 基金资助:
    国家重大新药创制科技重大专项资助(2018ZX09731020)

Simultaneous Determination of Total Flavonol Glycosides in Shenge Bushen Capsule by HPLC-QAMS

  1. 1.Xinjiang Huachun Biopharmaceutical Co., Ltd., Xinjiang Urumqi 830000, China; 

    2.Sinopharm Dezhong(Foshan) Pharmaceutical Co., Ltd., Guangdong Foshan 528000, China

  • Received:2023-12-11 Revised:2024-04-03 Online:2024-06-28 Published:2024-06-28

摘要: 目的:建立参葛补肾胶囊中淫羊藿苷、朝藿定A、朝藿定B、朝藿定C含量的HPLC测定方法。方法:采用高效液相色谱法,色谱柱为Waters ACQUITY UPLC HSS T3 C18(2.1×100 mm,1.8 μm),流动相为乙腈-0.05%磷酸水溶液体系,梯度洗脱,流速为0.3 mL·min-1,检测波长为320 nm,柱温为30 ℃,进样量为2 μL。以淫羊藿苷为内参物,采用斜率校正法计算其他3个成分的相对校正因子,比较外标法和一测多评法(QAMS)测定结果,验证一测多评法的可行性及准确性。结果:淫羊藿苷、朝藿定A、朝藿定B、朝藿定C分别在7.130~713.38 μg·mL-1、1.284~128.4 μg·mL-1、5.108~510.8 μg·mL-1、4.360~435.67 μg·mL-1质量浓度范围内存在良好的线性关系,线性系数R2均大于0.99,平均加样回收率分别为104.5%、99.69%、100%、98.59%,RSD分别为1.4%、2.7%、1.2%、2.8%。朝藿定A、朝藿定B、朝藿定C的相对校正因子为1.31、1.19、1.17。一测多评法和外标法测定结果比较,其差异无统计学意义(P>0.05)。结论:该方法准确、简便、重复性好,可作为参葛补肾胶囊中淫羊藿总黄酮醇苷的质量控制研究。

关键词: font-size:medium, ">参葛补肾胶囊;总黄酮醇苷;高效液相色谱;一测多评法

Abstract: Objective: To develop a HPLC method for determination of icariin, epimedin A, epimedin B, epimedin C in Shenge Bushen capsule. Methods: The chromatographic was performed on a Waters ACQUITY UPLC HSS T3 C18 column(2.1×100 mm, 1.8 μm), with acetonitrile(A)-0.05% phosphoric acid solution at the flow rate of 0.3 mL·min-1. Detection wavelength was set at 320 nm, the column temperature was maintained at 30 ℃, and the injection volume was 2 μL. The relative correction factors(fs/k) of the other three components was calculated by slope correction method with icariin as internal reference substance. Results: The linear range of icariin, epimedin A, epimedin B and epimedin were 7.13~713.38 μg·mL-1 (r=0.999 9), 1.28~128.40 μg·mL-1 (r=0.999 9), 5.11~510.80 μg·mL-1 (r=0.999 9), 4.36~435.67 μg·mL(r=0.999 9), respectively. The average recoveries were 104.56%, 99.69%, 100.00%, 98.59%, and the RSDs were 1.4%, 2.7%, 1.2%, 2.8%, respectively. By slope correction method, fs/k of epimedin A, epimedin B and epimedin C were 1.31, 1.19, 1.17. There were no significance difference in content determination results between two correction methods of QAMS and external standard(P>0.05). Conclusion: The method is simple, accurate and sensitive, and can be used for the quality control study of total Flavonol Glycosides in Shenge Bushen Capsule.

Key words: font-size:medium, ">Shenge Bushen capsules;Total flavonol glycosides; High performance liquid chromatography(HPLC);Quantitative analysis of multi-components by single marker(QAMS)

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