Development of stability-indicating UHPLC method for the quantitative determination of silodosin and its related substances.

ABSTRACT

A novel, specific and stability-indicating reversed-phase (RP) ultra-high-performance liquid chromatography (UHPLC) method, which is mass compatible, was developed and validated for the quantitative determination of silodosin and its related substances. Silodosin was subjected to stress conditions like hydrolysis (acid and basic), oxidation, photolysis and thermal degradation, as per the guidelines of the International Conference Harmonization, to show that the method is stability-indicating. The proposed UHPLC method has a resolution of greater than 2.0 between silodosin and its process-related impurities. The chromatographic separation was achieved on an Agilent Poroshell 120 EC-C18 column (50 × 4.6mm i.d.; particle size, 2.7 µm). The method employed a linear gradient elution using a mobile phase consisting of acetonitrile and 10 mM ammonium acetate buffer with 0.1% triethyl amine, with pH adjusted to 6.0, monitored at 273 nm. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness. The known process impurities were separated and their structure was confirmed by using liquid chromatography-mass spectrometry and direct mass analysis.