A simple, rapid, specific, sensitive and liquid chromatography coupled with tandem mass spectrophotometric method was developed and validated for the estimation of azathioprine and its metabolite 6-mercaptopurine in human plasma by using lamivudine and 6-mercaptopurine D3 as the internal standard. Azathioprine and 6-mercaptopurine were extracted from human plasma by solid-phase extraction (SPE)-Evaporation method, using Oasis MCX cartridge for cleaning procedure. The stationary phase was chromatographed on a ZORBAX SB CN, (75X50 mm, 5 µ) column where as mobile phase constitutes of acetonitrile: 2mM ammonium acetate (70:30 v/v) at a flow rate of 0.800 ml/min. The detection was performed with an Applied Biosystems Sciex API 4000 mass spectrometer by multiple reaction monitoring (MRM). The method validation proofs were carried out as per the USFDA guidelines as described, showing a linearity system (r2 > 0.99) over a range of 2.455 ng/mL to 106.568 ng/mL for azathioprine and 1.165 ng/mL to 101.143 ng/mL concentrations for 6-mercaptopurine and a recovery shows 99.36% and 100.44% for azathioprine and 6-mercaptopurine respectively. The results show that this proposed approach is effective and can be applied to the extraction and analysis of other pharmaceutical compounds.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12059 International Current Pharmaceutical Journal 2012, 1(11): 342-352
Background: Tetrabenazine was approved in the year of 2008 by USFDA. It was indicated mainly as an antipsychotic drug but now-a-days it is used for the treatment of hyperkinetic disorders. Objective: The objective of the study was to develop a simple and cost-effective spectrophotometric methods for the determination of tetrabenazine in tablets. Materials and Methods: The UV-Visible spectrophotometric studies carried out by Shimadzu UV 1800 with UV probe software and FT-IR studies using bruker alpha with opus software. The UV spectrum at 284 nm (Method A) and visible spectrum at 454 nm (Method B) are recorded. The FT-IR band of carbonyl group in tetrabenazine appeared at 1700 cm −1 with two-point baseline between 1650-1750 cm −1 (Method C). Results: Method A: The UV method was proved linear over the range of 10-50 µg/mL with correlation coefficient r 2 =0.9988 and mean recovery of 99.02% to 101.54%. Method B: The colorimetric method involves oxidative reaction of tetrabenazine and it yields green color chromogen. The linear concentrations over the range of 3-15 µg/mL with correlation coefficient of r 2 =0.9981 and mean recovery of 99.93% to 100.50%. Method C: The FT-IR method was showed linear over the range of 5-25 µg/mg, with correlation coefficient r 2 =0.9998 and mean recovery of 100.75% to 100.91%. The results of tetrabenazine tablets showed good agreement with their label claim. The results of ANOVA declare there was no significant difference between these spectrophotometric methods. Conclusion: Hence, these spectroscopic methods can be used for routine quality testing analysis of tetrabenazine in pharmaceutical laboratories.
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