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In this study, a simple, fast and sensitive LC/MS/MS method was developed and validated for the determination of GW9508 in rat plasma. The sample was precipitated with acetonitrile and subsequently separated on ZORBAX Eclipse XDB C column (50 mm × 2.1 mm, 5 μm). Mobile phase was composed of 0.1% formic acid in water and acetonitrile with gradient elution, at a flow rate of 0.4 mL/min. The analyte and internal standard were quantitatively monitored with precursor-to-product transitions of m/z 348.2→183.1 and m/z 397.2→260.2, respectively. The linearity of the assay was evident in the range of 1-1000 ng/mL with correlation coefficient more than 0.998. The validation parameters were all within the acceptable limits. The validated method has been successfully applied to the pharmacokinetics study of GW9508 in rat plasma, and our results demonstrated that GW9508 showed low clearance, moderate half-life and ideal bioavailability (54.88%). Furthermore, metabolites stemmed from rat plasma, rat hepatocytes and human hepatocytes were analyzed by an LC-Q-Exactive-Orbitrap-MS assay, resulting in the identification of seven metabolites based on the accurate mass and fragment ions. Acylglucuronide conjugate (M6) was found as the most abundant metabolite in all tested matrices. The metabolic pathways were proposed as hydroxylation and glucuronidation. This study provided an overview of disposition of GW9508, which is highly instructive for better understanding the effectiveness and toxicity of this drug.
This article was published in the following journal.
Name: Journal of pharmaceutical and biomedical analysis
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A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection.
Fractionation of a vaporized sample as a consequence of partition between a mobile gaseous phase and a stationary phase held in a column. Two types are gas-solid chromatography, where the fixed phase is a solid, and gas-liquid, in which the stationary phase is a nonvolatile liquid supported on an inert solid matrix.
A method of separation of two or more substances by repeated distribution between two immiscible liquid phases that move past each other in opposite directions. It is a form of liquid-liquid chromatography. (Stedman, 25th ed)
Chromatographic techniques in which the mobile phase is a liquid.
Pyrolysis of organic compounds at the temperature of a hydrogen-air flame to produce ionic intermediates which can be collected and the resulting ion current measured by gas chromatography.
Multiple Sclerosis MS
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An assay is an analytic procedure for qualitatively assessing or quantitatively measuring the presence or amount or the functional activity of a target entity. This can be a drug or biochemical substance or a cell in an organism or organic sample. ...