title: Water determination in active pharmaceutical ingredients using ionic liquid headspace gas chromatography and two different detection protocols.
abstract: A rapid, accurate, precise and versatile analytical method was developed for the detection and quantification of water in solid active pharmaceutical ingredients (APIs). The headspace gas chromatography (HSGC) method utilized an ionic liquid (IL) based open tubular capillary GC column to increase sensitivity and ruggedness of this method. ILs are also utilized as the headspace solvent because of their low vapor pressure, unique physiochemical properties and high thermal stability. This method is not affected by side reactions and solubility problems which are common with Karl Fischer Titration (KFT) methods. Nor is it as limited as weight loss on drying approaches. The ability to use either/both modern thermal conductivity or barrier ion discharge GC detection provides flexibility, different dynamic ranges and sensitivity. The developed method also was shown to be broadly applicable.
authors.affiliation: Department of Chemistry and Biochemistry, University of Texas at Arlington, TX, USA.
authors.forename: Lillian A
authors.initials: LA
authors.lastname: Frink
authors.affiliation: Department of Chemistry and Biochemistry, University of Texas at Arlington, TX, USA.
authors.forename: Choyce A
authors.initials: CA
authors.lastname: Weatherly
authors.affiliation: Department of Chemistry and Biochemistry, University of Texas at Arlington, TX, USA. Electronic address: sec4dwa@uta.edu.
authors.forename: Daniel W
authors.initials: DW
authors.lastname: Armstrong
mesh_terms: D002849:Chromatography, Gas / Q000379:methods; D004355:Drug Stability; D052578:Ionic Liquids / Q000737:chemistry*; D007477:Ions / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D012680:Sensitivity and Specificity; D012995:Solubility; D013696:Temperature; D013814:Thermal Conductivity; D014867:Water / Q000737:chemistry*
chemical_list: D052578:Ionic Liquids; D007477:Ions; D004364:Pharmaceutical Preparations; D014867:Water
keywords: Ionic liquid; Karl Fischer; Pharmaceuticals