中成药2024,Vol.46Issue(8):2499-2505,7.DOI:10.3969/j.issn.1001-1528.2024.08.002
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
摘要
Abstract
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.关键词
引火汤/冻干粉/HPLC指纹图谱/化学成分/含量测定/UPLC-MS/MSKey words
Yinhuo Decoction/freeze-dried powder/HPLC fingerprints/chemical constituents/content determination/UPLC-MS/MS分类
医药卫生引用本文复制引用
胡晶,丁亚明,刘爽,乔月,张悦,徐红丹,张宁,赵继会..引火汤冻干粉HPLC指纹图谱建立及8种成分含量测定[J].中成药,2024,46(8):2499-2505,7.基金项目
国家自然科学基金项目(青年科学基金项目)(82003975) (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) (2021)
黑龙江省卫生健康委科研课题(2020-301) (2020-301)
无锡市卫生健康委科研项目面上项目(M202170) (M202170)
无锡市"双百"中青年医疗卫生拔尖人才项目(BJ2023094) (BJ2023094)