ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF CLASS-2 RESIDUAL SOLVENTS IN LULICONAZOLE BY HS-GCAbstract
A simple headspace gas chromatographic (HS-GC) method has been developed and validated for the simultaneous determination of residual solvents like methanol, methyl isobutyl ketone, cyclohexane and toluene in luliconazole by Flame ionization detector (FID). The separation was achieved on 30 m long DB-624 column, 0.53 mm in inner diameter, and 3.0 µm in film thickness. The headspace and chromatographic parameters like flow rate and oven temperature are optimized to enhance sensitivity and chromatographic resolution. Dimethyl sulfoxide is used as diluents, equilibration temperature of 80 °C for 5 min, programmed temperature in the range of 35 °C to 210 °C and nitrogen as the carrier gas was used. The developed headspace gas chromatographic method offers good symmetry and resolution for all the residual solvents. The proposed was found to be suitable for the determination of 4 different residual solvents. Validation results indicated that the method is specific, linear, precise, accurate, rugged, and robust, where recoveries ranged between 90-110%.
G. S. S. V. Madhulika and B. R. Kuber *
Sri Padmavati Mahila Visvavidyalayam, Institute of Pharmaceutical Technology (Women’s University), Tirupati, Andhra Pradesh, India.
30 July 2019
30 November 2019
18 April 2020
01 July 2020