Summary.A sensitive and simple liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for determination of dasatinib in rat plasma using one-step protein precipitation was developed. After addition of carbamazepine as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. Chromatographic separation was achieved on an SB-C18 (2.1 mm × 150 mm, 5 μm) column with methanol-0.1% formic acid as mobile phase with gradient elution. Electrospray ionization (ESI) source was applied and operated in positive ion mode; selective ion monitoring (SIM) mode was used to quantification using target fragment ions m/z 488.2 for dasatinib and m/z 338.7 for the IS. Calibration plots were linear over the range of 10-1000 ng mL −1 for dasatinib in rat plasma. Lower limit of quantification (LLOQ) for dasatinib was 10 ng mL −1 . Mean recovery of dasatinib from plasma was in the range 82.2%-93.6%. Relative standard deviation (RSD) of intra-day and inter-day precision were both less than 8%. This developed method is successfully used in pharmacokinetic study of dasatinib in rats.
A reversed-phase chiral liquid chromatographic method had been developed and validated for resolution of the enantiomers of racemic fudosteine. The effects on the separation of the amounts of anhydrous cupric sulfate and L-phenylalanine, the methanol content, mobile phase pH, and temperature were investigated. The method was validated for linearity, repeatability, intermediate precision, sample recovery, solution stability, and limits of detection (LOD). L-Phenylalanine and anhydrous cupric sulfate as chiral ligand-exchange complexes were used for separation, isomer identification, related substance investigation, and analysis of fudosteine enantiomers in fudosteine bulk drugs and fudosteine tablets.
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