首页|引火汤冻干粉HPLC指纹图谱建立及8种成分含量测定

引火汤冻干粉HPLC指纹图谱建立及8种成分含量测定

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  • 国家科技期刊平台
  • NETL
  • NSTL
  • 万方数据
目的 建立引火汤冻干粉HPLC指纹图谱,并测定地黄苷D、麦冬甲基黄烷酮A、毛蕊花糖苷、原儿茶酸、梓醇、五味子醇甲、五味子乙素、五味子甲素的含量.方法 指纹图谱建立采用Supersil AQ18 色谱柱(4.6 mm×250 mm,5 μm);流动相乙腈-0.1%磷酸,梯度洗脱;体积流量 1.0 mL/min;柱温 30℃;检测波长 230 nm.UPLC-MS/MS含量测定采用Alphasil VC-C18色谱柱(2.1 mm×100 mm,2.5 μm);流动相乙腈-0.1%甲酸,梯度洗脱;体积流量0.3 mL/min;柱温30℃;电喷雾离子源;正负离子扫描;多反应监测模式.结果 10 批冻干粉指纹图谱中有17 个共有峰,相似度大于 0.90,指认出毛蕊花糖苷、水晶兰苷、去乙酰车叶草苷酸、五味子醇甲.8 种成分在各自范围内线性关系良好(R2＞0.990 6),平均加样回收率 98.7%～101.1%,RSD 2.0%～5.2%.结论 指纹图谱结合含量测定能完整表征引火汤基准样品质量,从而为其关键化学属性质量评价提供参考.
Establishment of HPLC fingerprints and content determination of eight constituents for freeze-dried powder of Yinhuo Decoction
AIM To establish the HPLC fingerprints for freeze-dried powder of Yinhuo Decoction,and to determine the contents of rehmannitin D,methylophiopogonanone A,verbascoside,protocatechuic acid,catalpol,schisandrol A,schisandrin B,schisandrin A.METHODS The fingerprint esablishment was performed on a 30℃thermostatic Supersil AQ18 column(4.6 mm×250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1%phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 230 nm.The UPLC-MS/MS content determination was performed on a 30℃thermostatic Alphasil VC-C18 column(2.1 mm×100 mm,2.5 μm),with the mobile phase comprising of acetonitrile-0.1%formic acid flowing at 0.3 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode.RESULTS There were 17 common peaks in the fingerprints for 10 batches of freeze-dried powder with the similarities of more than 0.90.and piloside,crystal blue glycoside,deacetylated caryoside schisandrin A were identified.Eight constituents showed good linear relationships within their own ranges(R2＞0.990 6),whose average recoveries were 98.7%-101.1%with the RSDs of 2.0%-5.2%.CONCLUSION The combination of fingerprints and content determination can completely characterize the quality of Yinhuo Decoction reference sample,thus provide a reference for the quality evaluation of its key chemical properties.

Yinhuo Decoctionfreeze-dried powderHPLC fingerprintschemical constituentscontent determinationUPLC-MS/MS

胡晶、丁亚明、刘爽、乔月、张悦、徐红丹、张宁、赵继会

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无锡卫生高等职业技术学校,江苏 无锡 214028

黑龙江中医药大学药学院,黑龙江 哈尔滨 150040

无锡市中医医院,江苏 无锡 214071

湖南医药学院药学院,湖南 怀化 418000

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引火汤 冻干粉 HPLC指纹图谱 化学成分 含量测定 UPLC-MS/MS

国家自然科学基金项目(青年科学基金项目)中央支持地方高校改革发展资金人才培养项目(2021)黑龙江省卫生健康委科研课题无锡市卫生健康委科研项目面上项目无锡市"双百"中青年医疗卫生拔尖人才项目

820039752020-301M202170BJ2023094

2024

10.3969/j.issn.1001-1528.2024.08.002

中成药
国家食品药品监督管理局,信息中心中成药信息站,上海中药行业协会

中成药

CSTPCD北大核心
影响因子：1.217
ISSN：1001-1528
年,卷(期)：2024.46(8)
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