ABSTRACT
A rapid static headspace-gas chromatographic (SHS-GC) method was developed and validated for the quantitation of residual solvents in pharmaceutical gel extrusion module (GEM) tablet formulations. A static headspace sampling technique was utilized to overcome the difficulties imposed by direct injection methods. A Rtx-1701 megabore capillary column was selected to achieve optimal resolution among organic volatile chemicals used commonly in the manufacturing of GEM tablets, residual solvents in the active ingredient and excipients, and other formulation matrix artifacts. A 50-mM pH 3.0 sodium phosphate buffer was used as a sample diluent to minimize matrix effects. The instrumental parameters of the SHS-GC method were optimized for sensitivity and precision. Quantitation was performed by external standard analysis. The SHS-GC method was validated according to regulatory requirements and produced acceptable results with respect to specificity, linearity, range, detection and quantitation limits, precision, and accuracy.
