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Validated LC‐MS method for simultaneous quantitation of catalpol and harpagide in rat plasma: application to a comparative pharmacokinetic study in normal and diabetic rats after oral administration of Zeng‐Ye‐Decoction
Author(s) -
Feng Yukun,
Liu Zhenzhen,
Peng Ying,
Zhang Lunhui,
Ju Ping,
Bi Kaishun,
Chen Xiaohui
Publication year - 2013
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.2949
Subject(s) - catalpol , chemistry , chromatography , protein precipitation , electrospray ionization , analyte , extraction (chemistry) , mass spectrometry , calibration curve , detection limit , glycoside , organic chemistry
A simple and efficient liquid chromatography‐mass spectrometry (LC‐MS) method was developed and validated for simultaneous quantitation of catalpol and harpagide in normal and diabetic rat plasma. Protein precipitation extraction with acetonitrile was carried out using salidroside as the internal standard (IS). The LC separation was performed on an Elite C 18 column (150 × 4.6 mm, 5 µm) with the mobile phase consisting of acetonitrile and water within a runtime of 12.0 min. The analytes were detected without endogenous interference in the selected ion monitoring mode with positive electrospray ionization. Calibration curves offered satisfactory linearity ( r > 0.99) at linear range of 0.05–50.0 µg/mL for catalpol and 0.025–5.0 µg/mL for harpagide with the lower limits of quantitation of 0.05 and 0.025 µg/mL, respectively. Intra‐ and inter‐day precisions (RSD) were <9.4%, and accuracy (RE) was in the −6.6 to 4.9% range. The extraction efficiencies of catalpol, harpagide and IS were all >76.5% and the matrix effects of the analytes ranged from 86.5 to 106.0%. The method was successfully applied to the pharmacokinetic study of catalpol and harpagide after oral administration of Zeng‐Ye‐Decoction to normal and diabetic rats, respectively. Copyright © 2013 John Wiley & Sons, Ltd.