European Journal of Biomedical and Pharmaceutical Sciences

A NEW CHROMATOGRAPHIC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS DETERMINATION OF DOXYLAMINE SUCCINATE, PYRIDOXINE HYDROCHLORIDE AND RELATED IMPURITIES

N. Nagaraju*, P. Sanjeeva, P. Venkata Ramana

ABSTRACT

The combination of Doxylamine Succinate and pyridoxine Hydrochloride wasrecognized for the treatment of nausea and vomiting in pregnancy women. The present investigation illustrates a new rapid, precise, accurate, stability indicating reverse phase high performance liquidchromatographic separation methodology was developed for highly resolved separation and determination of Doxylamine Succinate, Pyridoxine Hydrochloride and related nineteen impurities in Pharmaceutical dosage forms among them 14 impurities are degraded quantified  4 process related impurities were separated and unknown impurity was separated but not quantified. Chromatographic separation is achieved on an ACE Excel 5 AR 150 x 3.0 mm C-18 column using gradient elution. Mixture of Di ammonium hydrogen phosphate-n-pentane sulfonic acid buffer (PH=4.00±0.05), Methanol and n-propanol in a ratio of 400: 525: 75v/v/v respectively was used as mobile phase. The eluted compounds were monitored at 268 nm; the flow rate was 0.7 ml/min and column oven temperature maintained at 25±2°C. Resolution of determination of doxylamine succinate and pyridoxine hydrochloride and impurities(potential, bi-products and degradation) is greater than 2.0 for all pair of components. The high correlation coefficient (r2> 0.999) values indicated good correlations. The repeatability and intermediate precision, expressed by the RSD was less than 1.5%. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness and robustness. Stress studies and Peak purity studies were carried out according to ICH guidelines. All the degradation product (s) arose by induced degradation were well separated from the drug peaks. The degradation peaks observed due to various extreme conditions (such as acidic, alkaline, oxidation, hydrolysis, photolytic, thermal, etc.) are completely resolved from main drug peak. Hence the method found to be stability indicating. The proposed method is practical and valuable for its routine application in quality control laboratories for estimation of Doxylamine Succinate, Pyridoxine Hydrochloride and related nineteen impurities in Pharmaceutical dosage forms.

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