DEVELOPMENT AND VALIDATION OF AN ANALYTICAL METHOD FOR THE DETERMINATION OF RESIDUAL SOLVENTS IN OXACILLIN SODIUM BY HEADSPACE GAS CHROMATOGRAPHY

Habibur Rahman, Elaref Ratemi, S. K. Manirul Haque,* and Prem Shanker

ABSTRACT

A validated simple and sensitive headspace gas chromatographic (HSGC) method was developed for simultaneous determination of methanol, ethyl acetate and toluene in oxacillin sodium. The separation was achieved using a 30 m long Elite - 5 fused silica capillary column with 0.32 mm internal diameter. The developed gas chromatographic method offers a symmetric peak shape, good resolution and reasonable retention time for all the solvents. Beer’s law was obeyed in the concentration ranges of 100 – 1500, 100 – 800 and 100 – 500 ppm for methanol, ethyl acetate, and toluene, respectively for oxacillin sodium. The method was validated according to the international conference on harmonization (ICH) guidelines. The degrees of linearity of the calibration curves, the percent recoveries, relative standard deviation for the method were also determined. The correlation coefficient for methanol, ethyl acetate and toluene were found to be 0.9997, 0.9998 and 0.9996, respectively for oxacillin sodium.

Keywords: Oxacillin sodium, residual solvents, headspace gas chromatography, ICH.