STABILITY INDICATING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF LABETALOL AND ITS DEGRADATION PRODUCTS IN TABLET DOSAGE FORMS
Objective: The objective of the present work is to develop a simple, efficient, and reproducible stability indicating reverse phase high-performance
liquid chromatographic method for simultaneous determination labetalol and its degradation products in tablet dosage forms.
Methods: The chromatographic separation of labetalol and its degradation products in tablets was carried out on Zorbax Eclipse Plus C-18
(100 Ã— 4.6 mm, 3.5 Âµm) 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:
Methanol (1:1) by linear gradient program. Flow rate was 1.0 mL min
with a column temperature of 35Â°C, and detection wavelength was carried out
at 230 nm. Known impurity is well resolved from the main active drug within 14 minutes run time.
Results: The forced degradation studies were performed on labetalol tablets under acidic, basic, oxidation, thermal, humidity, and photolytic
conditions. No degradation products were observed from the forced degradation studies, and the known impurity is well resolved from the main
active drug. The method was validated in terms of specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, and
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.
The LOD and LOQ values of known impurity were found between 0.3593 and 0.7187 Âµg mL
, and the percentage recovery values were in the range
of 95.5-105.2% at different concentration levels. Relative standard deviation for precision and intermediate precision results were found to be <5%.
The correlation coefficient found for all compounds was not <0.99. The results obtained from the validation experiments prove that the developed
method is a stability indicating method.
Conclusion: The developed method can be successfully applied for routine analysis, quality control analysis and also suitable for stability analysis of
the simultaneous determination of labetalol and its degradation products in tablet dosage forms as per the regulatory requirements.
Keywords: Labetalol, Development, Validation, Reverse phase high-performance liquid chromatography.
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