Title HPLC-DAD-MSn analysis and HPLC quantitation of chemical constituents in Xian-ling-gu-bao capsules
Authors Guan, Xiang-Yu
Li, Hui-Fang
Yang, Wen-Zhi
Lin, Chang-Hu
Sun, Chao
Wang, Bao-Rong
Guo, De-An
Ye, Min
Affiliation Peking Univ, Sch Pharmaceut Sci, State Key Lab Nat & Biomimet Drugs, Beijing 100191, Peoples R China.
Guizhou Acad Sci, Inst Biol, Guiyang 550005, Peoples R China.
Guizhou Acad Sci, Guiyang 550001, Peoples R China.
Keywords XLGB
Quality control
HPLC-DAD-MSn
HPLC
Epimedii Herba
LIQUID-CHROMATOGRAPHY
FLAVONOL GLYCOSIDES
MASS-SPECTROMETRY
PSORALEA-CORYLIFOLIA
EPIMEDIUM-SAGITTATUM
Issue Date 2011
Publisher 药学与生物医学分析杂志
Citation JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS.2011,55,(5),923-933.
Abstract In this study, a systematic method was established for the global quality control of Xian-ling-gu-bao capsules (XLGB), a popular six-herb Traditional Chinese Patent Medicine (TCPM) for the treatment of osteoporosis. Both qualitative and quantitative analyses were conducted. In qualitative analysis part, a fast and sensitive method based on high-performance liquid chromatography coupled with diode-array detection and electrospray ionization tandem mass spectrometry (HPLC-DAD-MSn) was established for rapid separation and sensitive identification. Samples were separated on a Waters Symmetry C-18 column (250 mm x 4.6 mm, 5 mu m) by gradient elution using acetonitrile (A) and water-formic acid (B; 0.03%, v/v) as mobile phase at a flow rate of 1.0 ml/min. Based on the mass spectra, UV spectra and retention time, 47 compounds were identified or tentatively characterized, including 27 flavonols (all from Epimedii Herba, the major component herb), 4 coumarins, 3 flavonones, 1 chalcone, 3 isoflavones, 1 coumestrol, 3 triterpenoid saponins, 1 iridoid, 3 steroidal saponins, and I phenolic acid. Among them, 18 compounds were confirmed by comparing with reference standards. In quantitative analysis part, 10 major compounds in 18 batches of XLGB were simultaneously determined by HPLC/UV detected at 270 nm. The method was validated with respect to intra- and inter-day precision, repeatability and stability, with RSD less than 1.0%, 1.5%, 2.9% and 1.8%, respectively. All the 10 analytes showed good linearity in wide linear ranges (r(2) = 0.9999), and their average recoveries varied between 97.8% and 104.9%. (C) 2011 Elsevier B.V. All rights reserved.
URI http://hdl.handle.net/20.500.11897/156682
ISSN 0731-7085
DOI 10.1016/j.jpba.2011.03.021
Indexed SCI(E)
PubMed
Appears in Collections: 药学院
天然药物与仿生药物国家重点实验室

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