引火汤冻干粉HPLC指纹图谱建立及8种成分含量测定  

Establishment of HPLC fingerprints and content determination of eight constituents for freeze⁃dried powder of Yinhuo Decoction

作　　者：胡晶[2] 丁亚明[2] 刘爽 乔月 张悦[1] 徐红丹[1,2] 张宁 赵继会[4] HU Jing;DING Ya-ming;LIU Shuang;QIAO Yue;ZHANG Yue;XU Hong-dan;ZHANG Ning;ZHAO Ji-hui(College of Pharmacy,Heilongjiang University of Chinese Medicine,Harbin 150040,China;Wuxi Higher Health Vocational Technology School,Wuxi 214028,China;Wuxi Traditional Chinese Medicine Hospital,Wuxi 214071,China;Hunan Medical College,Huaihua 418000,China)

机构地区：[1]黑龙江中医药大学药学院,黑龙江哈尔滨150040 [2]无锡卫生高等职业技术学校,江苏无锡214028 [3]无锡市中医医院,江苏无锡214071 [4]湖南医药学院药学院,湖南怀化418000

出　　处：《中成药》2024年第8期2499-2505,共7页Chinese Traditional Patent Medicine

基　　金：国家自然科学基金项目(青年科学基金项目)(82003975);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(2020⁃301);无锡市卫生健康委科研项目面上项目(M202170);无锡市“双百”中青年医疗卫生拔尖人才项目(BJ2023094)。

摘　　要：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,5μm);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-C_(18)色谱柱(2.1 mm×100 mm,2.5μm);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(R^(2)>0.9906),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。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,5μm),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-C_(18) column(2.1 mm×100 mm,2.5μm),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(R^(2)>0.9906),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.

关 键 词：引火汤 冻干粉 HPLC指纹图谱 化学成分 含量测定 UPLC-MS/MS 

分 类 号：R927[医药卫生—药学]