A highly sensitive LC-MS/MS method for the determination of S-raclopride in rat plasma: application to a pharmacokinetic study in rats

✍ Scribed by Suresh P. S; Ravindra Ramachandra Punde; Manish Gupta; Abhishek Dixit; Sanjeev Giri; Sriram Rajagopal; Ramesh Mullangi

• Publisher: John Wiley and Sons
• Year: 2010
• Tongue: English
• Weight: 560 KB
• Volume: 25
• Category: Article
• ISSN: 0269-3879
• DOI: 10.1002/bmc.1547

✦ Synopsis

A highly sensitive and rapid assay method has been developed and validated for the estimation of S-(-)-raclopride (S-RCP) in rat plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive ion mode. The assay procedure involves a simple liquid-liquid extraction technique for extraction of S-RCP and phenacetin (internal standard, IS) from rat plasma. Chromatographic separation was achieved with 0.2% formic acid : acetonitrile (80:20, v/v) at a flow rate of 0.30 mL/min on a Phenomenex Prodigy C18 column with a total run time of 4.5 min. The MS/MS ion transitions monitored were 347.2 , 112.1 for S-RCP and 180.1 , 110.1 for IS.

Method validation and pre-clinical sample analysis were performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.05 ng/mL and the linearity range was extended from 0.05 to 152 ng/mL in rat plasma. The intra-day and inter-day precisions were 0.23-10.5 and 3.74-7.29%, respectively. This novel method was applied to a pharmacokinetic study of S-RCP in rats.