Fast capillary GC using a low thermal mass column oven for the determination of residual solvents in pharmaceuticals

Abstract

A low thermal mass column oven was used for fast capillary GC analysis (high throughput) of residual solvents in pharmaceutical products. A dedicated capillary column, 20 m L x 180 microm ID x 1 microm DB-624 was programmed from 35 degrees C (30 s) to 150 degrees C at 100 degrees C/min and to 250 degrees C (30 s) at 200 degrees C/min, resulting in a total GC cycle time of less than 4 min. Complete separation of a target 20-component mixture was achieved, while method performance in terms of repeatability, sensitivity, and linearity was maintained in comparison to the generic method currently applied in our laboratories.

Determination of residual solvents in isobutylboronic acid: Masking derivatization improves stability of GC column

“…The static headspace GC is a conventional and powerful analytical technique that has been adopted and recommended by the European Pharmacopoeia and the United States Pharmacopoeia for the determination of residual solvents within quality control of pharmaceutical products . Relative simplicity of sample preparation, sensitivity and elimination of GC system contamination by unwanted non‐volatile substances belong to the main benefits of the headspace technique . However, analysis of some specific matrices for the RS content requires a special sample pretreatment.…”

Recent developments in the determination of residual solvents in pharmaceutical products by microextraction methods

“…8 Among them, the most commonly used technique for the analysis of residual solvents is conventional gas chromatography (GC). 9,10 In order to analyze trace amounts of such analytes in pharmaceuticals, an appropriate sample preparation step is necessary prior to GC. 11,12 The traditional technique for residual solvent determination is direct injection; in which the drug substance or the formulation is dissolved in or extracted with a high boiling point solvent.…”