title: Development and validation of a HPLC-MS/MS method with electrospray ionization for quantitation of potassium oxonate in human plasma: Application to a pharmacokinetic study.
abstract: A rapid, sensitive and specific HPLC-MS/MS method was developed and validated for the quantification of potassium oxonate (Oxo) in human plasma using [(13)C(2),(15)N(3)]-Oxo as an internal standard (IS). The target substance was separated from human plasma using the solid-phase extraction method. Chromatography separation was performed on a Waters:Atlantis dC(18) column (150×4.6 mm, 5.0 μm) with a mobile phase consisting of H(2)O with 0.1% formic acid in acetonitrile (90:10, v/v). The mass spectrometer works with electrospray ionization and multiple reaction monitoring in its negative ion mode, using target ions at [M-H](-) m/z 111.9 for Oxo and [M-H](-) m/z 117.0 for the IS. The mean standard curve was linear (r=0.9991) over the concentration range of 2.0-200.0 ng/ml and had good back-calculated accuracy and precision. The intra- and inter-day precision were <6.33% and the accuracy was >99.38%. The extraction recovery was >60.26%. The lower limit of quantification achieved with this method was 2.0 ng/ml. This assay method was demonstrated to be accurate, sensitive and simple and was successfully applied to a pharmacokinetic study following single oral administration of a 40-mg S-1 capsule in 12 tumor patients.
authors: Department of Pharmacology, Affiliated Hospital of the Academy of Military Medical Sciences, Beijing 100071;
authors: Guangtao
authors: G
authors: Hao
authors: Shaobo
authors: S
authors: Bai
authors: Haixia
authors: H
authors: Liang
authors: Yuguang
authors: Y
authors: Liang
authors: Hengyan
authors: H
authors: Qu
authors: Hongzhi
authors: H
authors: Gao
authors: Yuanyuan
authors: Y
authors: Li
authors: Zhuanjie
authors: Z
authors: Zheng
authors: Xiaofang
authors: X
authors: Wang
authors: Zeyuan
authors: Z
authors: Liu
keywords: HPLC-MS/MS; pharmacokinetics; potassium oxonate