A new RP-HPLC method for separation and determination of process related impurities in Pioglitazone Hydrochloride API

Abstract

The objective of the study was to develop a validated, specific and stability-indicating gradient reverse phase liquid chromatographic method for determination of Pioglitazone Hydrochloride along with its impurities in bulk samples. <span style="mso-bidi-font-style:italic">Drug substance was subjected to stress conditions of hydrolysis (acid and base), oxidation, photolytic, humidity and thermal degradation as per International Conference on Harmonization (ICH) to show the stability-indicating power of the method. Significant degradation was observed with alkali and hydrogen peroxide. <span style="mso-bidi-font-style:italic">The impurities were characterized using spectral techniques like IR, ¹H NMR and MS<span style="mso-bidi-font-style:italic">. Successful separation of impurities was achieved on C18 ODS (150x4.6 mm) <span style="mso-bidi-font-weight:bold">3.5 µ column using mobile phase consisting of Solvent A: Ammonium acetate buffer and Acetonitrile in the ratio (57:43 v/v) for 0-7 min and Solvent B: Ammonium acetate buffer and Acetonitrile in the ratio (20:80 v/v) at a flow rate of 1.0 ml/min from 7-20 min followed by Solvent A from 20-21 min. The retention times of impurity A, impurity B, impurity C and Pioglitazone were 3.44, 10.65, 17.95 and 8.32 min respectively. The detection wavelength was set at 254 nm with column temperature at<span style="mso-bidi-font-weight:bold"> 45 ºC. Finally<span style="mso-bidi-font-style:italic"> developed method was validated as per ICH guidelines for specificity, linearity, precision and accuracy.<span style="mso-bidi-font-style:italic">

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