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 |