FAST AND SENSITIVE DERIVATIZATION METHOD TO DETERMINE THE RESIDUAL HYDRAZINE AS ACETONE AZINE IN DRUG SUBSTANCES BY USING GAS CHROMATOGRAPHY

摘要

A sensitive gas chromatographic method was developed and validated for the determination of carcinogenic free hydrazine in drug substance by using the derivatization with acetone. The critical experimental parameters, such as, derivatization time, reaction temperatures were studied and optimized. The method was validated as per guidelines in terms of detection limit (DL), quantitation limit (QL), linearity, precision, accuracy, specificity and robustness. A linear range from 0.1 to 1.5 mcg/mL was obtained with the coefficient of determination (r2) 0.9988. The DL and QL of hydrazine 0.05 mcg/mL and 0.10 mcg/mL respectively. The mean recovery was 104.57% with a relative standard deviation of 0.93% for hydrazine. Also, the specificity of the method was proved through gas chromatography mass spectrometry (GC-MS).