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Determination of pinocembrin in human plasma by solid‐phase extraction and LC/MS/MS: application to pharmacokinetic studies
Authors:Bei Yan  Guoying Cao  Taohua Sun  Xi Zhao  Xin Hu  Jiling Yan  Yueying Peng  Aixin Shi  Yang Li  Wei Xue  Min Li  Kexin Li  Yingfa Liu
Affiliation:1. Department of Clinical Pharmacology, Beijing Hospital, Beijing, China;2. CSPC Zhongqi Pharmaceutical Technology (Shijiazhuang) Co. Ltd, Shijiazhuang, China
Abstract:A sensitive, fast and specific method for the quantitation of pinocembrin in human plasma based on high‐performance liquid chromatography–tandem mass spectrometry (LC/MS/MS) was developed and validated. Clonazepam was used as the internal standard (IS). After solid‐phase extraction of 500 μL plasma, pinocembrin and the IS were separated on a Luna C8 column using the mobile phase composed of acetonitrile–0.3 mm ammonium acetate solution (65:35, v/v) at a flow rate of 0.25 mL/min in isocratic mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via an electrospray ionization source in negative mode by AB SCIEX Qtrap 5500. The assay was linear from 1 to 400 ng/mL, with within‐ and between‐run accuracy (relative error) from ?1.82 to 0.54%, and within‐ and between‐run precision (CV) below 5.25%. The recovery was above 88% for the analyte at 1, 50 and 300 ng/mL. This analytical method was successful for the determination of pinocembrin in human plasma and applied to a pharmacokinetic study of pinocembrin injection in healthy volunteers after intravenous drip administration. Copyright © 2014 John Wiley & Sons, Ltd.
Keywords:pinocembrin  LC/MS/MS  human plasma  method validation  pharmacokinetics
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