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Determination and pharmacokinetic study of norcantharidin in human serum by HPLC‐MS/MS method
Author(s) -
Wei Chunmin,
Zhang Rui,
Wang Benjie,
Yuan Guiyan,
Guo Ruichen
Publication year - 2008
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.892
Subject(s) - chemistry , chromatography , ammonium acetate , formic acid , pharmacokinetics , electrospray ionization , calibration curve , selected reaction monitoring , high performance liquid chromatography , detection limit , tandem mass spectrometry , acetone , mass spectrometry , electrospray , pharmacology , medicine , organic chemistry
A sensitive, simple and selective high‐performance liquid chromatography–tandem mass spectrometry method was developed and applied to the determination of norcantharidin concentration in human serum. Norcantharidin (NCTD) and cyclophosphamide (IS) in serum were extracted with acetone, separated on a C 18 reversed‐phase column, gradiently eluted with a mobile phase of acetonitrile–water containing 2 m m ammonium acetate and 0.1% formic acid (pH 3), ionized by positive ion pneumatically assisted electrospray and detected in the multi‐reaction monitoring mode using precursor → product ions of m/z 169.3 → 123.1 for NCTD and 261.2 → 140.2 for IS, respectively. The linear range of the calibration curve for NCTD was 2.5–50 ng/mL, with a lowest limit of quantification of 2.5 ng/mL, and the intra/inter‐day RSD was less than 10%. The method was suitable for determination of low NCTD concentration in human serum after therapeutic oral doses, and has been successfully used for pharmacokinetic studies in healthy Chinese volunteers. Copyright © 2007 John Wiley & Sons, Ltd.