Identification and deconvolution of carbohydrates with gas chromatography-vacuum ultraviolet spectroscopy
Autor: | Jonathan Smuts, Nicola L. B. Pohl, Kevin A. Schug, Jamie Schenk, Allegra Leghissa, Gabe Nagy |
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Rok vydání: | 2017 |
Předmět: |
Analyte
Anomer Vacuum Carbohydrates 010402 general chemistry Mass spectrometry Methylation 01 natural sciences Biochemistry Gas Chromatography-Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Fragmentation (mass spectrometry) Oximes Derivatization chemistry.chemical_classification Chromatography 010401 analytical chemistry Organic Chemistry General Medicine Silanes Furanose 0104 chemical sciences Pharmaceutical Preparations chemistry Pyranose Spectrophotometry Ultraviolet Gas chromatography |
Zdroj: | Journal of Chromatography A. 1513:210-221 |
ISSN: | 0021-9673 |
Popis: | Methodology for qualitative and quantitative determination of carbohydrates with gas chromatography coupled to vacuum ultraviolet detection (GC-VUV) is presented. Saccharides have been intently studied and are commonly analyzed by gas chromatography-mass spectrometry (GC-MS), but not always effectively. This can be attributed to their high degree of structural complexity: α/β anomers from their axial/equatorial hydroxyl group positioning at the C1-OH and flexible ring structures that lead to the open chain, five-membered ring furanose, and six-membered ring pyranose configurations. This complexity can result in convoluted chromatograms, ambiguous fragmentation patterns and, ultimately, analyte misidentification. In this study, mono-, di, and tri-saccharides were derivatized by two different methods-permethylation and oximation/pertrimethylsilylation-and analyzed by GC-VUV. These two derivatization methods were then compared for their efficiency, ease of use, and robustness. Permethylation proved to be a useful technique for the analysis of ketopentoses and pharmaceuticals soluble in dimethyl sulfoxide (DMSO), while the oximation/pertrimethylsilylation method prevailed as the more promising, overall, derivatization method. VUV spectra have been shown to be distinct and allow for efficient differentiation of isomeric species such as ketopentoses and reducing versus non-reducing sugars. In addition to identification, pharmaceutical samples containing several compounds were derivatized and analyzed for their sugar content with the GC-VUV technique to provide data for qualitative analysis. |
Databáze: | OpenAIRE |
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