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摘要
A sensitive and selective liquid chromatography tandem mass spectrometry (LC-MS-MS) method for determination of urapidil hydrochloride in rabbit plasma was developed and validated. After addition of doxapram hydrochloride as the internal standard (IS), protein precipitation by 10% trichloroacetic acid was used as the sample preparation. Chromatographic separation was achieved on a Zorbax SB-C18 (2.1mmx50mm, 3.5m) column with acetonitrile-water as the mobile phase with gradient elution. Electrospray ionization (ESI) source was applied and operated in positive ion mode; multiple reaction monitoring (MRM) mode was used to quantification using target fragment ions m/z 387.9204.6 for urapidil hydrochloride and m/z 378.9291.8 for the IS. Calibration plots were linear over the range of 5-1000ng/mL for urapidil hydrochloride in plasma. Lower limit of quantitation (LLOQ) for urapidil hydrochloride was 5ng/mL. Mean recovery of urapidil hydrochloride from plasma was in the range 93.5%-96.4%. RSD of intra-day and inter-day precision were both less than 12%. This developed method is successfully used in pharmacokinetic study of urapidil hydrochloride in rabbit.
- 出版日期2011
- 单位温州医科大学
