| 摘要 |
<p>The method having a purpose of reducing analysis time, increasing reliability via higher resolution with very high pressure due to smaller particles, sensitivity and selectivity as well as economical method by reducing solvent consumption, Reverse Phase-Ultra performance Liquid Chromatography (RP-UPLC) is most promising advancement in a world of chromatography. Being a patented drug, Prenoxdiazine HC1 has not any published analytical background. In this novel research work, a new gradient reverse phase UPLC method was developed for the same in bulk form. Forced degradation study was carried out as per International Conference on Harmonization (ICH) guideline and a newly developed method is applicable to degradation analysis of drug. A chromatographic separation of drug as well as its degradants was achieved using Waters acquity CSH, 2.1 x 100mm, 1.7μm C18 column with gradient of phosphate buffer pH 7.0 and acetonitrile. Drug and degradants were monitored at detection wavelength of 220 nm, the flow rate was 0.4 ml/min, injection volume was 5 μl and temperature of column and auto sampler compartments were ambient. Retention time of drug was about 2.9 mins and relative retention time of common degradant in all stressed conditions is 0.92. The resolution of drug and degradant was greater than 1.7 in all cases. At higher stressed conditions, drug degrades into more fragments as compare to one degradant n optimized stressed condition. Drug shows different solution stability in two different diluents that are acetonitrile and methanol. A developed method was validated as per ICH guideline using validation parameters like precision, linearity and range, specificity, robustness, solution stability and filter compatibility. Results of validation were found satisfactorily within specified acceptance criteria. Forced degradation studies demonstrated the stability indicating power of the UPLC method.</p> |
