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  • 1990-1994  (2)
  • Fast atom bombardment mass spectrometry  (1)
  • Hexamethyldisilazane treated silica  (1)
  • 1
    ISSN: 1612-1112
    Keywords: Thin layer chromatography ; Fast atom bombardment mass spectrometry ; TLC/FABMS ; 3-Glycidoxypropyldimethylethoxysilane treated TLC plate ; Midazolam intoxication
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effectiveness of 3-glycidoxypropyl-treated thin layer chromatographic plates in the determination of midazolam intoxication has been studied by thin layer chromatography/fast atom bombardment mass spectrometry. Silica plates treated with 3-glycidoxypropyldimethylethoxysilane were used for the measurement of their physical composition and for chemical analysis. From elemental carbon analysis data, the maximum number of bonded 3-glycidoxypropyl surface groups per gram was calculated to be 0.417×1021. Midazolam in human serum from patients suffering from intoxication could be separated on a 3-glycidoxypropyl-treated thin layer chromatographic plate with chloroform as eluent. After applying the technique of diffused spot condensation on the 3-glycidoxypropyl-treated thin layer chromatographic plate, the established thin layer chromatography/fast atom bombardment mass spectrometry method was used for the identification of midazolam intoxication, and improved the detection limit for midazolam in the serum of an intoxication patient by 30 times.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Octadecyl modified silica ; Hexamethyldisilazane treated silica ; Calcination ; Heat-treated silica
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of silanol groups on three types of octadecylmodified column gels using heat-treated silicas by calcination has been studied by high-performance liquid chromatography. After heat-treating at 180°C, 500°C and 950°C, the silicas treated with octadecyldimethylchlorosilane were used for the measurement of physical and chemical analysis. From elemental carbon analysis data, the reactive silanol group concentrations, αOH(s), were determined to be 2.0 in the 180°C treated silica, 2.1 in the 500°C treated silica and 1.6 in the 950°C treated silica, respectively (original silica: mean pore diameter 116 Å, specific surface area 298 m2/g, pore volume 1.22 ml/g, particle size 5.0 μm). The separation factors, α, of pyridine versus phenol were measured to be 0.79 on 180°C treated silica, 0.91 on 500°C treated silica and 1.98 on 950°C treated silica, using acetonitrile-water mixtures as the eluent. And then, on the basis of the physico-chemical and chromatographic data, the three types of octadecyl modified column gels using heat-treated silicas by calcination have been compared.
    Type of Medium: Electronic Resource
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