Abstract

METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF RESIDUAL SOLVENTS IN OXFENDAZOLE API BY USING HEAD SPACE GAS CHROMATOGRAPHY

N. H. Eswara Prasad, Dr. K. Basavaiah*, Dr. B. M. Rao, N. V. N. B. Srinivasa Rao, Y. V. Sunil Kumar and D. Rama Devi

ABSTRACT

Residual solvents in pharmaceutical samples are monitored using gas chromatography with head space. Based on the good manufacturing practices, measuring residual solvents is mandatory for the release testing of all active pharmaceutical ingredients (API). The analysis of residual organic solvents (methanol, acetone and toluene) in Oxfendazole veterinary API was carried out. Oxfendazole is a broad spectrum benzimidazole anthelmintic used as a veterinary drug. Its main use is for protecting livestock against roundworm, strongyles and pinworms.[1] Oxfendazole is the sulfoxide metabolite of fenbendazole. The residual organic solvents (methanol, acetone and toluene) in Oxfendazole was determined using the DB WAX column (30 m length, 0.32 mm internal diameter, and 0.5 μm film thickness) Nitrogen was used as carrier gas. Split ratio was 1:30, detector temperature was 230 °C, Oven temperature was initially kept 50 °C, held for 2 minutes, raised to 100°C by 10°C/min, raised to 220°C by 20°C/min , 2 minutes hold. Headspace injector oven equilibrium was at 85 °C. Needle temperature was 90 °C. Transfer line temperature was 95 °C. Oven/vial equilibration time was 20 min and pressurization time was 3 min. N, N-dimethyl formamide was selected as a diluent. The method was validated according to ICH guidelines and found to be specific, linear i.e., correlation coefficient is 0.999, precise and % RSD of each analyte is less than 15%, sensitive, rugged and showed excellent recovery. The Present developed & validated method are run successfully for Oxfendazole residual solvents determination by Gas chromatography with head space in active pharmaceutical ingredient manufacturing.

Keywords: Headspace-gas chromatography, Omeprazole, Method validation, Residual solvents.