నైరూప్య

A validated specific stability-indicating RP-HPLC method for altretamine and its process related impurities

M.B.V.Narayana, K.B.Chandrasekhar

AValidated Specific Stability indicating Reversed-phase Liquid chromatographic method was developed for the quantitative determination of Altretamine and its related substances in bulk samples, pharmaceutical dosage forms in presence of degradation products. Forced degradation studies were performed on bulk sample of Altretamine as per ICH prescribed stress conditions using acid, base, oxidative, water hydrolysis, thermal stress and photolytic degradation to show the stability indicating power of the LC method. Significant degradation in oxidative hydrolysis was observed and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies and the impurity spiked solution. Good resolution between the process related impurities and degradation products from the analyte was achieved on Zorbax SB-C18 column using the mobile phase consists a mixture of 10mMammoniumcarbonate in water pH adjusted to 8.0 with ammoniumhydroxide solution andMethanol in the ratio of 35:65 v/v at detection of 227 nmwavelength. The limit of detection and the limit of quantitation for Altretamine and its process related impurities were established. The stressed test solutions were assayed against the qualified standard ofAltretamine and the mass balance in each case was in between 98.7%-99.8%indicating that the developed LCmethod was Stability-indicating. Validation of the developed LC method was carried out as per ICH requirements. The developed method was found to be suitable to check the quality of bulk samples of Altretamine at the time of batch release and also during its storage and stability studies.