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| 基于HPLC法及UPLC-MS法测定芫花饮片炮制前后7种成分的含量变化 |
| Determination of 7 compounds of Daphne genkwa decoction pieces before and after processed by HPLC and UPLC-MS method |
| 投稿时间：2023-12-04 修订日期：2024-04-09 |
| DOI： |
| 中文关键词: 芫花 炮制 化学成分 含量测定 液相色谱 液质联用色谱 |
| 英文关键词: Daphne genkwa, Processing, Chemical components, Determination, HPLC, UPLC-MS |
| 基金项目:]国家中医药现代化研究专项(2018YFC1707003)[ |
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| 中文摘要: |
| 目的：建立HPLC法及UPLC-MS法测定芫花中银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素、芫花素及芫花酯甲7 种化学成分含量的方法,分析芫花炮制前后化学成分的变化。方法：采用HPLC法,测定银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素和芫花素6种成分的含量,色谱柱为Agilent Eclipse Plus C18(250×4.6 mm,5 μm),流动相为乙腈(A)-0.1%甲酸(B)梯度洗脱,流速为1.0ml/min,进样量10ul。同时采用UPLC-MS方法测定芫花酯甲的含量,色谱柱为ACQUITY UPLC HSS T3 C18 色谱柱(2.1 mm × 100 mm, 1.8 μm),流动相为乙腈(A)-0.1%甲酸(B)梯度洗脱,流速0.3 ml.min-1,柱温35℃,进样量1ul。结果：7种成分的含量由高到低依次为芫花素 >绿原酸 > 银椴苷 > 芹菜素 > 羟基芫花素 > 木犀草素 > 芫花酯甲。芫花炮制后7种成分的含量均发生一定程度的变化,其中绿原酸成分在炮制前后含量有升高有降低,变化不明显；对于银椴苷和芹菜素成分,炮制后含量有降低趋势；对于木犀草素、羟基芫花素和芫花素3个成分,炮制后含量有升高的趋势；对于芫花酯甲成分,炮制后含量趋于降低。结论：该方法简便、灵敏、高效,为考察芫花饮片炮制前后的质量变化提供了技术支持。 |
| 英文摘要: |
| Objective: To establish HPLC method and UPLC-MS method for the determination of tiliroside、luteolin、apigenin、chlorogenic acid、hydroxygenkwanin、genkwanin and yuanhuacine in Daphne genkwa. To analyze the contents change of 7 chemical components before and after processing. Methods: The determinations of tiliroside、luteolin、apigenin、chlorogenic acid、hydroxygenkwanin and genkwanin were analyzed by HPLC. The chromatographic column was Agilent Eclipse Plus C18 (250 mm × 4.6 mm, 5 μm) with mobile phase gradient elution of acetonitrile (A) -0.1% formic acid (B). The flow rate was 1.0 mL.min-1 and the injection volume was 10 μL. The determinations of yuanhuacine was analyzed by UPLC-MS. The chromatography was performed on ACQUITY UPLC HSS T3 C18 column (2.1 mm × 100 mm, 1.8 μm) with gradient elution of acetonitrile (A) -0.1% formic acid (B) as mobile phase at the flow rate of 0.3 mL.min-1. The column temperature was 35 ℃ and the injection volume was 1 μL. Results: The contents of the 7 components in the order of high to low were genkwanin > chlorogenic acid > tiliroside > apigenin > hydroxygenkwanin > luteolin > yuanhuacine. The contents of 7 components in Daphne genkwa were changed to a certain extent after processing, and the content of chlorogenic acid was increased and decreased before and after processing, but the change was not obvious. The contents of tiliroside and apigenin were decreased after processing. The contents of luteolin, hydroxygenkwanin and genkwanin were increased after processing. For the components of yuanhuacine, its content was tended to decrease after processing. Conclusion: The method was efficient, sensitive and simple, and it provided technical support for investigating the quality changes of Daphne genkwa decoction slices before and after processing. |
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