Krishna R Gupta

  In the present work the approach of forced degradation study was successfully applied for the development of stability-indicating assay method for determination of Thiocolchicoside in the presence of its degradation products.  The RP-HPLC separation was carried out on Shimadzu® -HPLC 1100 series using a Phenomenex ODS 5µ C18 column (250×4.6mm) with mobile phase comprising of Acetonitrile: Phosphate Buffer (70:30) pH 3.5 v/v at flow rate of 1.0mL/min and UV detection at 260.0 nm. In stress testing a drug substance or the drug product is exposed to an environment vigorous than the normal i.e. at high temperature, high humidity over the period of time called accelerated stability conditions. The drug was subjected to Solid state analysis which includes Humidity studies (40°C/75% RH), photochemical studies (UV light and sunlight exposure) and Thermal studies to apply stress conditions. The method was validated as per ICH guidelines for accuracy, precision, linearity and range, ruggedness and robustness. The linearity of the proposed method was investigated in the range of 80-120% of label claim; the correlation coefficient for Thiocolchicoside was found to be 0.999. The proposed method was found to be simple, specific, linear and rugged and can be used for routine quality control.

  The present work describes the development of stability indicating assay method for Diacerein and Aceclofenac in their combined dosage form that would provide helpful information to the manufacturers. Stress studies were conducted on the drug substance and product under the ICH prescribed stress conditions viz. hydrolysis, oxidation, humidity, photolysis, thermal stress. The separation of the drug from its degradation products, trials were made by taking acetonitrile: water, acetonitrile: phosphate buffer, acetonitrile: phosphoric acid in various blends. Separation was achieved using C-18 column and a mobile phase comprising of Acetonitrile: Phosphoric acid 0.1 M (61: 39) at a flow rate of 1.5 mL/min. The detection wavelength was 260 nm. The drug showed sufficient decomposition under alkaline hydrolysis (0.05 N NaOH), acidic hydrolysis (0.05 N HCl), neutral hydrolysis (distilled water), and oxidative hydrolysis (6% H2O2). The drug was found to be moderately sensitive to humidity studies (75 % RH), photochemical studies (UV 254 nm), and thermal studies (600C). Recovery studies were also carried out for both the drugs and the mean percent recovery were found to be 100.69 for diacerein and 99.15 for aceclofenac. Mean percent estimation in marketed formulation gave 99.63% for diacerein and 100.04% for aceclofenac. The above method was validated for accuracy, precision, ruggedness, limit of detection, limit of quantitation and was found to be satisfactory for routine analysis of diacerein and aceclofenac in their combined dosage form in the presence of their degradation products.   Key words: Aceclofenac, Diacerein, Stress Degradation, Stability Indicating, Validation