Development and validation of a liquid chromatography/tandem mass spectrometry method for the determination of DMXAA in human and mouse plasma
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- 作者：Xiaosong Zhang ; Ming Zhao ; Michelle A. Rudek ; Ping He ; Bert Vogelstein
- 关键词：DMXAA ; LC/MS/MS ; Pharmacokinetics
- 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
- 出版年：2007
- 出版时间：1 June 2007
- 年：2007
- 卷：852
- 期：1-2
- 页码：217-222
- 全文大小：302 K
文摘
A rapid, sensitive, and specific LC/MS/MS-based method was developed for determining the concentration of DMXAA in human and mouse plasma. Sample preparation involved a single protein precipitation step using acetonitrile. Separation of DMXAA and 6-isopropoxy-9-oxoxanthene-2-carboxylic acid, the internal standard, was achieved on a Waters X-Terra™ C18 (50 mm × 2.1 mm i.d., 3.5 μm) analytical column using a mobile phase consisting of acetonitrile/10 mM ammonium acetate (55:45, v/v) containing 0.1 % formic acid and isocratic flow at 0.2 mL/min for 3 min. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated over the range of 5–3000 ng/mL. The values for precision and accuracy were <9.6 % , except at the LLOQ (5 ng/mL) level, which was within 16.8 % . Recovery of DMXAA in mouse plasma was >65 % . DMXAA was stable through 2 freeze/thaw cycles, to 2 h in mouse plasma or 50 % acetonitrile, and on the autosampler to 5.1 h. This method was subsequently used to measure concentrations of DMXAA in mice following intraperitoneal administration.