ABSTRACT
An isocratic normal phase high-performance liquid chromatographic (NP-HPLC) method has been developed and validated for the quantitation of Z-isomer in lanoconazole. Separation was achieved with a Thermo Hypersil Silica column. The ratio of 2-propanol, n-hexane and triethylamine in the mobile phase were optimized to obtain the best separation. UV detection was performed at 296 nm. The described method is linear over a range of LOQ--15.0 microg/ml of Z-isomer. The mean recovery of Z-isomer was found to be in the range of 97-99%. The method is simple, rapid, selective, accurate and precise, useful in the quality control of bulk manufacturing.
Subject(s)
Antifungal Agents/analysis , Chromatography, High Pressure Liquid/methods , Imidazoles/analysis , Antifungal Agents/chemistry , Imidazoles/chemistry , Quality Control , Reproducibility of Results , StereoisomerismABSTRACT
An isocratic reversed phase liquid chromatographic (RP-LC) method has been developed and subsequently validated for the determination of almotriptan malate and its process-related impurities. Separation was achieved with a Phenomenex, Gemini, C-18 column and sodium phosphate buffer (pH adjusted to 7.6): acetonitrile (80:20, v/v) as eluent, at a flow rate of 1.5 mL/min. UV detection was performed at 227 nm. The method is simple, rapid, selective, accurate and stability indicating. The described method is linear over a range of LOQ, 1.5 ug/mL (150% of the specification limit) for all the process-related impurities. The method precision for the determination of related compounds was below 1.0% R.S.D. The accuracy of the method demonstrated at 4 levels in the range of 25-150% of the specification limit and the recovery of impurities were found to be in the range of 96-102%. The method is useful in the quality control of bulk manufacturing.
