STABILITY INDICATING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF LABETALOL AND ITS DEGRADATION PRODUCTS IN TABLET DOSAGE FORMS

Abstract

<p>ABSTRACT<br />Objective: The objective of the present work is to develop a simple, efficient, and reproducible stability indicating reverse phase high-performance<br />liquid chromatographic method for simultaneous determination labetalol and its degradation products in tablet dosage forms.<br />Methods: The chromatographic separation of labetalol and its degradation products in tablets was carried out on Zorbax Eclipse Plus C-18<br />(100 × 4.6 mm, 3.5 µm) column using 0.1% trifluoroacetic acid (TFA) (v/v) in 1000 ml of water and 0.1% TFA (v/v) in 1000 ml of acetonitrile:<br />Methanol (1:1) by linear gradient program. Flow rate was 1.0 mL min<br /> with a column temperature of 35°C, and detection wavelength was carried out<br />at 230 nm. Known impurity is well resolved from the main active drug within 14 minutes run time.<br />−1<br />Results: The forced degradation studies were performed on labetalol tablets under acidic, basic, oxidation, thermal, humidity, and photolytic<br />conditions. No degradation products were observed from the forced degradation studies, and the known impurity is well resolved from the main<br />active drug. The method was validated in terms of specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, and<br />robustness as per the ICH guidelines. The method was found to be linear in the range of LOQ to 120% for all the known and unknown impurities.<br />The LOD and LOQ values of known impurity were found between 0.3593 and 0.7187 µg mL<br />, and the percentage recovery values were in the range<br />of 95.5-105.2% at different concentration levels. Relative standard deviation for precision and intermediate precision results were found to be <5%.<br />The correlation coefficient found for all compounds was not <0.99. The results obtained from the validation experiments prove that the developed<br />method is a stability indicating method.<br />−1<br />Conclusion: The developed method can be successfully applied for routine analysis, quality control analysis and also suitable for stability analysis of<br />the simultaneous determination of labetalol and its degradation products in tablet dosage forms as per the regulatory requirements.<br />Keywords: Labetalol, Development, Validation, Reverse phase high-performance liquid chromatography.</p>