Development and Validation of UPLC Method for the Determination ofDuloxetine Hydrochloride and Its Impurities in Active Pharmaceutical Ingredient

摘要

A suitable, rapid, sensitive and accurate ultra-performance liquid chromatography (UPLC) method was developed for the quantitative determination of Duloxetine hydrochloride and its impurities in active pharmaceutical ingredient. Chromatographic separation was achieved on shim-pack XR-ODS II (3.0 × 100 mm, 2.2 μm), and the gradient eluted within a period of time, that is, 15 minutes. The eluted compounds were monitored at 230 nm. The flow rate was 0.9 ml/min and the column oven temperature was maintained at 40oC. The resolution of Duloxetine hydrochloride and 12 impurities (potential impurity, process related impurity and degradation products) were greater than 1.3. The correlation coefficient (r2>0.99) values indicated clear correlations between the investigated compound concentrations and their peak areas within the quantitation limit to 200% level. The performance of the method was validated according to the present ICH guidelines for specificity, quantitation limit, detection limit, linearity, accuracy, precision, ruggedness and robustness. The recoveries obtained (93.28-102.41%) ensured the accuracy of the developed methods.