Author(s): Jamalapuram S, Vuppala PK, Mesangeau C, McCurdy CR, Avery BA
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Abstract A selective, rapid and sensitive ultra performance liquid chromatography mass spectrometry (UPLC/MS) method was developed and validated to quantitate a highly selective mixed-affinity sigma receptor ligand, CM156 (3-(4-(4-cyclohexylpiperazin-1-yl)butyl)benzo[d] thiazole-2(3H)-thione), in rat plasma. CM156 and the internal standard (aripiprazole) were extracted from plasma samples by a single step liquid-liquid extraction using chloroform. The analysis was carried out on an ACQUITY UPLC™ BEH HILIC column (1.7 μm, 2.1 mm×50 mm) with isocratic elution at flow rate of 0.2 mL/min using 10mM ammonium formate in 0.1\% formic acid and acetonitrile (10:90) as the mobile phase. The detection of the analyte was performed on a mass spectrometer operated in selected ion recording (SIR) mode with positive electrospray ionization (ESI). The validated analytical method resulted in a run time of 4 min and the retention times observed were 2.6±0.1 and 2.1±0.1 min for CM156 and the IS, respectively. The calibration curve exhibited excellent linearity over a concentration range of 5-4000 ng/mL with the lower limit of quantification of 5 ng/mL. The intra- and inter-day precision values were below 15\% and accuracy ranged from -6.5\% to 5.0\%. The mean recovery of CM156 from plasma was 96.8\%. The validated method was applied to a pilot intravenous pharmacokinetic study in rats. Copyright Â© 2012 Elsevier B.V. All rights reserved.
This article was published in J Chromatogr B Analyt Technol Biomed Life Sci
and referenced in Journal of Bioequivalence & Bioavailability