Spectrophotometric method for the determination of ketoconazole based on amplification reactions / 药物分析学报

This paper describes a sensitive spectrophotometric method developed for determination of Ketoconazole (KC) in tablets based on amplification reactions.Ketoconazole was oxidized with periodate,resulting in formation of KC2+ and iodate ions.After masking the excess periodate with molybdate,the iodate was treated with iodide to release iodine.The liberated iodine was transformed to ICl2ˉspecies and extracted as ion-pair with rhodamine 6G into toluene for spectrophotometric measurement at 535nm.A linear calibration graph was obtained between 0.2136μg/mL and 1.7088 μg/mL of Ketoconazole with a molar absorptivity of 5 × 105 mol.L-1 cmˉ 1.The procedure was successfully applied for the determination of ketoconazole in tablet formulation.

Development and validation of RP-HPLC and RP-UPLC methods for quantification of parathyroid hormones (1-34) in medicinal product formulated with meta-cresol / 药物分析学报

Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for of parathyroid hormone (PTH)in presence of meta-cresol as a stabilizer in a pharmaceutical formulation.Chromatography was performed with phase containing 0.1％ Trifluoroacetic acid (TFA) in MilliQ water and 0.1％ TFA in acetonitrile with gradient and flow rate at 0.3 mL/min for HPLC and 0.4 mL/min for UPLC.Quantification was accomplished with internal reference standard (qualified against innovator product and National for for Biological Standards and Control (NIBSC) standard).The methods were validated for linearity (correlation coefficient=0.99),range,accuracy,precision and robustness.Robustness was confirmed by considering three factors; mobile phase composition,column temperature and flow rate/age of mobile phase.Intermediate precision was confirmed on different equipments,different columns and on different days.The relative standard deviation (RSD) (＜2％ for RP-HPLC and ＜1％ for UPLC n=30) indicated a good precision.Retention time was found about 17min and 2min by HPLC and UPLC methods,respectively.Both methods are simple,highly sensitive,precise and accurate and have the potential of being useful for routine quality control.