title: Application of atmospheric pressure chemical ionisation mass spectrometry in the analysis of barbiturates by high-speed analytical countercurrent chromatography.
abstract: Four barbiturates (barbital, allobarbital, phenobarbital and butalbital) were analysed using high-speed analytical countercurrent chromatography (HSACCC) and high-performance liquid chromatography (HPLC) interfaced with mass spectrometry, using negative mode atmospheric pressure chemical ionisation (APCI). The polar biphasic solvent system of butyronitrile/acetonitrile/water (1:1:1) was used, in the upper-stationary, lower-mobile mode of operation, at a flow rate of 1 mL/min and a rotational speed of 1200 rpm, equating to an applied "g"-field of 177 g. The fractional stationary phase retention (S(F)) was 0.58. Representative mass spectral data are presented from the HPLC and the HSACCC analyses. Structural information was obtained using source-induced fragmentation at increased source block voltages. The effect of increasing g-field on chromatographic resolution is illustrated using the binary base system of butyronitrile/water (1:1), under electrospray ionisation.
authors.affiliation: Mass Spectrometry Research Unit, University of Wales Swansea, Grove Building, Singleton Park, Swansea SA2 8PP, Wales, UK. 147437@swan.ac.uk
authors.forename: Jonathan J
authors.initials: JJ
authors.lastname: Jones
authors.forename: Huw
authors.initials: H
authors.lastname: Kidwell
authors.forename: David E
authors.initials: DE
authors.lastname: Games
mesh_terms: D000465:Algorithms; D001463:Barbiturates / Q000032:analysis*; D003377:Countercurrent Distribution; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D012995:Solubility; D012997:Solvents
chemical_list: D001463:Barbiturates; D007202:Indicators and Reagents; D012997:Solvents