DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING RP-HPLC METHOD FOR THE DETERMINATION OF XIPAMIDE IN PURE AND DOSAGE FORMS
Keywords:
Xipamide, Stability indicating RP-HPLC, stress degradation, pure form, dosage formsAbstract
Objective: A simple, selective, precise and stability-indicating RP-HPLC-method was developed and validated for the determination of xipamide (XIP).
Methods: Stability tests were done through exposure of the analyte solution to thermal, photolytic, hydrolytic and oxidative stress conditions. The chromatographic separation was carried out in less than five min on a RP stainless-steel C-18 analytical column (150 mm ×4.6 mm ID, 5 µm) with an isocratic elution system of 0.023 M orthophosphoric acid of pH 2.6 and acetonitrile as the mobile phase in the ratio of 60: 40 at 1.5 ml/min flow rate at room temperature. A diode array UV was used at 220 nm for detection.
Results: The degradation products were well separated from the pure drug. The elution time of XIP was found to be 4.561±0.024 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ) and robustness. Good linearity was found in the concentration range of 1–100 µg/ml with a correlation coefficient of 0.9999. Intraday and interday precision were within 1.4%. LOD and LOQ were 0.088 μg/ml and 0.267 μg/ml, respectively and percentage recovery of XIP was found to be 99.92±1.02 %.
Conclusion: The proposed method was successfully applied to the determination of XIP in pure form and in its pharmaceutical preparation without interference from its degradation products.
Keywords: Xipamide, Stability indicating RP-HPLC, Stress degradation, Pure form, Dosage forms
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