Use of ionic liquids as headspace gas chromatography diluents for the analysis of residual solvents in pharmaceuticals

Journal of Pharmaceutical and Biomedical Analysis
Omprakash NachamGregory K Webster

Abstract

In this study, two ionic liquids (ILs), 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide ([BMIM][NTf2]) and trihexyltetradecylphosphonium bis[(trifluoromethyl)sulfonyl]imide ([P66614][NTf2]) were examined as contemporary diluents for residual solvent analysis using static headspace gas chromatography (SHS-GC) coupled with flame ionization detection (FID). ILs are a class of non-molecular solvents featuring negligible vapor pressure and high thermal stabilities. Owing to these favorable properties, ILs have potential to enable superior sensitivity and reduced interference, compared to conventional organic diluents, at high headspace incubation temperatures. By employing the [BMIM][NTf2] IL as a diluent, a 25-fold improvement in limit of detection (LOD) was observed with respect to traditional HS-GC diluents, such as N-methylpyrrolidone (NMP). The established IL-based method demonstrated LODs ranging from 5.8 parts-per-million (ppm) to 20ppm of residual solvents in drug substances. The optimization of headspace extraction conditions was performed prior to method validation. An incubation temperature of 140°C and a 15min incubation time provided the best sensitivity for the analysis. Under optimized experimental con...Continue Reading

Citations

Jan 31, 2018·Analytical and Bioanalytical Chemistry·Rahul A PatilDaniel W Armstrong
Oct 6, 2018·Journal of Separation Science·Adissu Alemayehu AsfawErwin Adams
Sep 20, 2017·Journal of Separation Science·Kevin D ClarkJared L Anderson
Dec 29, 2018·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Xiaowen HeLantong Zhang

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