标准研讨

超高效液相色谱法同时测定固本消疹方中10个成分的含量*

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  • 1.广州中医药大学第二临床医学院,广东省中医院,广东省中医药科学院,广州 510006;
    2.广东省中医证候临床研究重点实验室,广州 510120
第一作者 Tel:18820143936;E-mail:18820143936@163.com
**Tel:(020) 81887233-31223;E-mail:lcj@gzucm.edu.cn

收稿日期: 2022-01-27

  网络出版日期: 2024-06-24

基金资助

*国家中医药管理局“岐黄工程”项目[国中医药办人教函(2019)62号];广东省科技计划项目(No.2017B030314166);广东省中医药局科研项目(No.20203005)

Simultaneous determination of ten components in Guben Kangmin decoction by UPLC*

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  • 1. The Second Clinical Medical College of Guangzhou University of Chinese Medicine (Guangdong Academy of Traditional Chinese Medicine, Guangdong Provincial Hospital of Chinese Medicine), Guangzhou 510006, China;
    2. Guangdong Provincial Key Laboratory of Clinical Research on Traditional Chinese Medicine Syndrome, Guangzhou 510120, China

Received date: 2022-01-27

  Online published: 2024-06-24

摘要

目的: 建立超高效液相色谱(UPLC)法同时测定固本消疹方中5-羟甲基糠醛、升麻素苷、毛蕊异黄酮苷、升麻素、5-O-甲基维斯阿米醇苷、毛蕊异黄酮、亥茅酚苷、6-姜酚、五味子醇甲和梣酮10个成分的含量,明确配伍对10个成分含量变化的影响。方法: 应用UPLC梯度洗脱技术,采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7 μm),以乙腈-0.1%甲酸水溶液为流动相,流速为0.25 mL·min-1,检测波长为254 nm,柱温为30 ℃。结果: 5-羟甲基糠醛、升麻素苷、毛蕊异黄酮苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、毛蕊异黄酮、6-姜酚、五味子醇甲和梣酮质量浓度分别在156.00~10 000、12.50~1 600、3.12~400、12.50~1 600、6.25~800、0.78~100、3.90~500、20.50~1 600、0.58~75、12.50~200 ng范围内与峰面积呈良好的线性关系(r=0.999 5~1.000),平均加样回收率在98.3%~102.3%(RSD<3%,n=6)。固本消疹方中6-姜酚、毛蕊异黄酮苷、5-羟甲基糠醛、五味子醇甲、梣酮含量显著增加(P<0.05或P<0.01);而毛蕊异黄酮、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷和亥茅酚苷含量无明显变化。结论: 该方法可用于固本消疹方及其制剂的质量控制,为其新药开发奠定基础,为其临床应用提供科学依据。

本文引用格式

刘丽娟, 赵亚, 吴亚运, 赵瑞芝, 卢传坚 . 超高效液相色谱法同时测定固本消疹方中10个成分的含量*[J]. 药物分析杂志, 2023 , 43(3) : 516 -524 . DOI: 10.16155/j.0254-1793.2023.03.19

Abstract

Objective: To establish an UPLC method for simultaneous determination of 5-hydroxymethyl furfuraldehyde (5-HMF), cimicifugoside, calycosin-7-glucoside, cimicifugin, 4’-O-beta-glucopyranosyl-5-O-methylvisamminol, calycosin, sec-O-glucosylhamaudol, 6-gingerol, schisandrin and fraxinellone in Guben Kangmin decoction, so as to analyze the variation of the 10 ingredients after compatibility. Methods: The samples were separated on an ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) by gradient elution with acetonitrile-0.1% formic acid aqueous solution at a flow rate of 0.25 mL·min-1. The detection wavelength was 254 nm. The column temperature was controlled at 30 ℃. Results: 5-HMF,cimicifugoside, calycosin-7-glucoside, cimicifugin, 4’-O-beta-glucopyranosyl-5-O-methyl-visamminol, calycosin, sec-O-glucosylhamaudol, 6-gingerol, schisandrin and fraxinellone exhibited good linearity(r2=0.999 5-1.000)among the ranges of 156.00-10000, 12.50-1600, 3.12-400, 12.50-1600, 6.25-800, 0.78-100, 3.90-500, 20.50-1600, 0.58-75 and 12.50-200 ng, respectively. The average recoveries (RSD<3%, n=6) were between 98.3%-102.3%. After the compatibility, the contents of 6-gingerol, calycosin-7-glucoside, 5-HMF, schisandrin and fraxinellone increased significantly (P<0.05 or P<0.01), while there was no significant change in the contents of cimicifugoside, cimicifugin, 4’-O-beta-glucopyranosyl-5-O-methyl-visamminol, calycosin and sec-O-glucosylhamaudol. Conclusion: The method can be used for the quality control of Guben Kangmin decoction and its preparations, and can provide scientific basis for the clinical compatibility and application of Guben Kangmin decoction.

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