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Application of atmospheric pressure chemical ionisation mass spectrometry in the analysis of barbiturates by high‐speed analytical countercurrent chromatography
Author(s) -
Jones Jonathan J.,
Kidwell Huw,
Games David E.
Publication year - 2003
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1086
Subject(s) - chemistry , chromatography , mass spectrometry , countercurrent chromatography , analytical chemistry (journal) , high performance liquid chromatography , electrospray , electrospray ionization , atmospheric pressure chemical ionization , atmospheric pressure , ionization , chemical ionization , organic chemistry , ion , oceanography , geology
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. Copyright © 2003 John Wiley & Sons, Ltd.