期刊
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
卷 877, 期 31, 页码 4059-4064出版社
ELSEVIER
DOI: 10.1016/j.jchromb.2009.10.011
关键词
Cephradine; LC-MS/MS; Protein precipitation; Bioequivalence
资金
- Korea government (MOST) [R13-2002-020-03002-0 (2007)]
- Seoul Research and Business Development Program [10524]
- National Research Foundation of Korea [R13-2002-020-03002-0] Funding Source: Korea Institute of Science & Technology Information (KISTI), National Science & Technology Information Service (NTIS)
A rapid and simple procedure was developed for the determination of cephradine in human plasma using liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). After trichloroacetic acid (TCA) precipitation of proteins from plasma samples, cephradine and cefaclor (the internal standard: IS) were eluted on a CN column. The isocratic mobile phase used consisted of acetonitrile-water-formic acid (25:75:0.1, v/v/v). Cephradine and the IS were both detected in multiple reaction monitoring (MRM) mode at the transitions: m/z 350.0 -> 90.8 for cephradine and m/z 368.1 -> 106.0 for the IS, respectively. The calibration curve was linear over the concentration range from 0.05 to 50 mu g/ml, and correlation coefficients were greater than 0.996. The coefficient of variation of assay precision was less than 9.36%, and its accuracy ranged from 87.92% to 111.16%. The chromatographic run time for each plasma sample was less than 3 min. The developed method was successfully applied to a bioequivalence study of cephradine in healthy male volunteers. (C) 2009 Elsevier B.V. All rights reserved.
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