Development of a liquid chromatography-mass spectrometry method for the determination of ursolic acid in rat plasma and tissue: Application to the pharmacokinetic and tissue distribution study.
Summary of "Development of a liquid chromatography-mass spectrometry method for the determination of ursolic acid in rat plasma and tissue: Application to the pharmacokinetic and tissue distribution study."
A fast and sensitive liquid chromatography-mass spectrometry method was developed for the determination of ursolic acid (UA) in rat plasma and tissues. Glycyrrhetinic acid was used as the internal standard (IS). Chromatographic separation was performed on a 3.5 μm Zorbax SB-C18 column (30 mm × 2.1 mm) with a mobile phase consisting of methanol and aqueous 10 mM ammonium acetate using gradient elution. Quantification was performed by selected ion monitoring with (m/z)(-) 455 for UA and (m/z)(-) 469 for the IS. The method was validated in the concentration range of 2.5 - 1470 ng mL(-1) for plasma samples and 20 - 11760 ng g(-1) for tissue homogenates. The intra- and inter-day assay of precision in plasma and tissues ranged from 1.6% to 7.1% and 3.7% to 9.0%, respectively, and the intra- and inter-day assay accuracy was 84.2 - 106.9% and 82.1 - 108.1%, respectively. Recoveries in plasma and tissues ranged from 83.2% to 106.2%. The limits of detections were 0.5 ng mL(-1) or 4.0 ng g(-1). The recoveries for all samples were >90%, except for liver, which indicated that ursolic acid may metabolize in liver. The main pharmacokinetic parameters obtained were T (max) = 0.42 ± 0.11 h, C (max) = 1.10 ± 0.31 μg mL(-1), AUC = 1.45 ± 0.21 μg h mL(-1) and K (a) = 5.64 ± 1.89 h(-1). The concentrations of UA in rat lung, spleen, liver, heart, and cerebellum were studied for the first time. This method is validated and could be applicable to the investigation of the pharmacokinetics and tissue distribution of UA in rats.
Affiliation
Institute of Pharmaceutical Analysis, College of Pharmacy, Wuhan University, Wuhan, 430072, China.
Journal Details
This article was published in the following journal.
Name: Analytical and bioanalytical chemistry
ISSN: 1618-2650
Pages:
Links
- PubMed Source: http://www.ncbi.nlm.nih.gov/pubmed/21249342
- DOI: http://dx.doi.org/10.1007/s00216-011-4651-x
Medical and Biotech [MESH] Definitions
Tandem Mass Spectrometry
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.
Gas Chromatography-mass Spectrometry
A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds.
Mass Spectrometry
An analytical method used in determining the identity of a chemical based on its mass using mass analyzers/mass spectrometers.
Countercurrent Distribution
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)
Spectrometry, Mass, Electrospray Ionization
A mass spectrometry technique used for analysis of nonvolatile compounds such as proteins and macromolecules. The technique involves preparing electrically charged droplets from analyte molecules dissolved in solvent. The electrically charged droplets enter a vacuum chamber where the solvent is evaporated. Evaporation of solvent reduces the droplet size, thereby increasing the coulombic repulsion within the droplet. As the charged droplets get smaller, the excess charge within them causes them to disintegrate and release analyte molecules. The volatilized analyte molecules are then analyzed by mass spectrometry.
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