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  • Column liquid chromatography  (2)
  • Atmospheric pressure ionization  (1)
  • Column liquid chromatography/mass spectrometry  (1)
  • Semisynthetic alkaloid  (1)
  • Thin-layer chromatography  (1)
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  • 1
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Atmospheric pressure chemical ionization-mass spectrometry ; Dried yeast ; Thiamine ; Ion-pair extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary High-performance liquid chromatography (HPLC) and high-performance liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (HPLC/APCI-MS) have been applied to the analysis of thiamine in dried yeast. Thiamine was extracted from dried yeast with isobutanol containing sodium 1-octanesulfonate as an ion-pairing agent and determined by HPLC on a reversed phase ODS column with UV detection at 254 nm. Response was linear in the range 25–300 μg/g of thiamine in dried yeast with a coefficient of variation in the reproducibility of 8.0%. Thiamine was recovered in good yield (109.2%, n=5). Identification of the thiamine peak was obtained by the mass spectrum using the HPLC/APCI-MS system. The utility of the selected ion monitoring technique using the HPLC/APCI-MS was also investigated. The results obtained by this method are in good agreement with those obtained by the thiochrome method [1].
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography/mass spectrometry ; Atmospheric pressure ionization ; Selective ion monitoring ; Nicergoline ; Semisynthetic alkaloids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary This study demonstrated the utility of high-performance liquid chromatography/atmospheric pressure ionization mass spectrometry (HPLC/API-MS) in the investigation of 10α-methoxy-1,6-dimethylergoline-8β-methanol 5-bromonicotinic acid ester (Nicergoline) and its related substances. The analysis was performed by using an ODS column with ammonium acetate and methanol mixture as the mobile phase. Nicergoline and its related compounds could be characterized by HPLC/API-MS in terms of their molecular weight. The use of multiple ion detection techniques for the quantitation of these compounds was also investigated. The detection limits of nicergoline and its related substances were 5 to 10 ng each at a signal-to-noise ratio of 4. The method was also applied to the study of the decomposition products of nicergoline in simulated gastric and intestinal fluids.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 32 (1991), S. 179-181 
    ISSN: 1612-1112
    Schlagwort(e): Thin-layer chromatography ; Secondary ion mass spectrometry ; Nicergoline ; Semisynthetic alkaloid
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A direct combination of thin-layer chromatography with secondary ion mass spectrometry (TLC/SIMS) provides a method for the quantitative analysis of thermally unstable compounds or compounds of low volatility such as nicergoline. The method is very simple and has excellent precision. The analysis was performed by using an aluminium TLC plate and a mixture of methylene chloride, acetone, and distilled water as a developing solvent. After development the portion of the plate with the nicergoline and the internal standard spots was cut off the TLC plate, and was attached to the SIMS holder directly. The amount of nicergoline was determined from the ratio of the fragment ion intensity of the nicergoline to the internal standard. The calibration curve was linear, and the detection limit was 10 ng at a signal-to-noise ratio of 5. This method should be considered for application to the determination of drugs in biological samples and also for the determination of possible impurities and decomposition products in drugs.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 4
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Aldehydes, aliphatic ; 1,3-Cyclohexanedione (CHD) ; Fluorimetric detection ; Plasma analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A simple and sensitive method is proposed for the measurement of aldehydes in plasma. The plasma samples are treated with 1,3-cyclohexanedione (CHD) and after addition of the internal standard (the CHD derivative of octaldehyde) are analysed by reversed-phase high-performance liquid chromatography with an acetonitrile-water gradient as the mobile phase. Detection is by fluorimetry with excitation at 395 nm and emission at 457 nm. In plasma samples spiked with aldehydes, the calibration curves showed good linearity in the range 0–10 μg mL−1. The recoveries of aldehydes were quantitative; coefficients of within-day and between-day variation were less than 13% and 11%, respectively. Applications to human and some animal plasma samples are reported.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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