title: Application of acetone acetals as water scavengers and derivatization agents prior to the gas chromatographic analysis of polar residual solvents in aqueous samples.
abstract: The sensitivity of gas chromatography (GC) combined with the full evaporation technique (FET) for the analysis of aqueous samples is limited due to the maximum tolerable sample volume in a headspace vial. Using an acetone acetal as water scavenger prior to FET-GC analysis proved to be a useful and versatile tool for the analysis of high boiling analytes in aqueous samples. 2,2-Dimethoxypropane (DMP) was used in this case resulting in methanol and acetone as reaction products with water. These solvents are relatively volatile and were easily removed by evaporation enabling sample enrichment leading to 10-fold improvement in sensitivity compared to the standard 10μL FET sample volumes for a selection of typical high boiling polar residual solvents in water. This could be improved even further if more sample is used. The method was applied for the determination of residual NMP in an aqueous solution of a cefotaxime analogue and proved to be considerably better than conventional static headspace (sHS) and the standard FET approach. The methodology was also applied to determine trace amounts of ethylene glycol (EG) in aqueous samples like contact lens fluids, where scavenging of the water would avoid laborious extraction prior to derivatization. During this experiment it was revealed that DMP reacts quantitatively with EG to form 2,2-dimethyl-1,3-dioxolane (2,2-DD) under the proposed reaction conditions. The relatively high volatility (bp 93°C) of 2,2-DD makes it possible to perform analysis of EG using the sHS methodology making additional derivatization reactions superfluous.
authors.affiliation: KU Leuven, University of Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB 923, Leuven 3000, Belgium.
authors.forename: Niels
authors.initials: N
authors.lastname: van Boxtel
authors.affiliation: KU Leuven, University of Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB 923, Leuven 3000, Belgium.
authors.forename: Kris
authors.initials: K
authors.lastname: Wolfs
authors.affiliation: KU Leuven, University of Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB 923, Leuven 3000, Belgium.
authors.forename: Ann
authors.initials: A
authors.lastname: Van Schepdael
authors.affiliation: KU Leuven, University of Leuven, Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, Herestraat 49, O&N2, PB 923, Leuven 3000, Belgium. Electronic address: Erwin.Adams@pharm.kuleuven.be.
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D000080:Acetals / Q000737:chemistry*; D000096:Acetone / Q000031:analogs & derivatives* / Q000737:chemistry*; D000900:Anti-Bacterial Agents / Q000032:analysis; D002439:Cefotaxime / Q000031:analogs & derivatives / Q000032:analysis; D002849:Chromatography, Gas / Q000379:methods; D004148:Dioxolanes / Q000737:chemistry; D007202:Indicators and Reagents; D011760:Pyrrolidinones / Q000032:analysis; D012997:Solvents; D014835:Volatilization; D014867:Water / Q000737:chemistry*
chemical_list: D000080:Acetals; D000900:Anti-Bacterial Agents; D004148:Dioxolanes; D007202:Indicators and Reagents; D011760:Pyrrolidinones; D012997:Solvents; D014867:Water; D000096:Acetone; C038678:N-methylpyrrolidone; D002439:Cefotaxime
keywords: 2,2-Dimethoxypropane; Dehydration; Full evaporation technique; Static headspace