Analytical Method Development and Validation of Glucosamine Sulphate and Its Impurities by Using AQbD Approach

Background: Pharmaceutical firms are confronting issues with pharmaceutical quality control. The classic OFAT approach required testing final products. It is time-consuming and expensive. Instead, the new AQbD strategy seeks to instill quality in the product throughout the manufacturing process, reducing the likelihood of product failure. A high-performance liquid chromatography (HPLC) method was devised to detect glucosamine sulphate impurities in bulk and solid dose formulations. There are many methods developed for the same but by using new DoE tools we can develop more robust method. Materials and Methods: The HPLC separation was achieved on Phenomenex 100-5 C-18 column (5 µm 100Å, 250 mm X 4.6 mm) using a mobile phase Acetonitrile: Potassium dihydrogen ortho phosphate buffer (80:20 v/v pH 3.0) at a flow rate of 1.0 ml/min and UV detection at 210 nm. The method was validated for specificity, linearity, solution stability, accuracy, precision, limit of detection, and limit of quantitation. CPP were selected by risk assessment Programme. Results: The detector response for glucosamine sulphate was linear over the selected concentration range from 100 to 500 ug/ml with a correlation coefficient 0.9997. The accuracy was between 97.40 – 100.37%. The precision (R.S.D.) amongst five sample preparations was 0.029(intraday) & 0.879(interday). The limit of detection and the limit of quantitation are 3.307 and 10.023 ug/ml, respectively. Conclusion: Forced degradation study of glucosamine was carried out under acidic, alkaline, oxidative, thermal, and neural conditions. It was found that glucosamine was stable in all conditions except in oxidative degradation. The amount estimated in oxidative degradation by HPLC and HPTLC was found to be 95.28 and 95.33 respectively.