Development and validation of a column high-performance liquid chromatographic method for determination of sibutramine in capsules.
The development and validation of a reversed-phase liquid chromatographic (LC) method for the determination of sibutramine hydrochloride monohydrate in capsules is described. An isocratic LC analysis was performed on a reversed-phase RP-18 column (250 x 4.6 mm id, 5 microm particle size). The mobile phase consisted of methanol-water-triethylamine (80 + 20 + 0.5, v/v/v), with pH adjusted to 5.65 with 85% phosphoric acid, and was pumped at a constant flow rate of 1.0 mL/min. Measurements were made at a wavelength of 223 nm. The calibration curve was linear over the range of 15-40 microg/mL [correlation coefficient (r2) = 0.9998]. The relative standard deviation (RSD) value for intraday precision was 0.84%. The RSD value for interday precision was 0.90%. Recoveries ranged from 99.64 to 100.66%. No interferences from the excipients were observed. Because of its simplicity and accuracy, the method is suitable for routine quality control analysis of sibutramine in capsules.
Diefenbach
Isabel Cristina Fração
IC
Universidade Federal de Santa Maria, Programa de Pós-graduação em Ciências Farmacêuticas, Santa Maria, RS, Brazil. isabel.diefenbach@terra.com.br
Friedrich
Milene
M
Dos Santos
Marcos Roberto
MR
Bittencourt
Celso Figueiredo
CF
D000928:Antidepressive Agents / Q000032:analysis; D001067:Appetite Depressants / Q000032:analysis; D002214:Capsules / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003503:Cyclobutanes / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D015203:Reproducibility of Results
D000928:Antidepressive Agents; D001067:Appetite Depressants; D002214:Capsules; D003503:Cyclobutanes; C058254:sibutramine