Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education, Harbin 150040, Heilongjiang, China.
Molecules. 2018 May 27;23(6):1284. doi: 10.3390/molecules23061284.
A modified GC-MS analytical procedure based on trimethylsilyl-dithioacetal (TMSD) derivatization has been established for a simultaneous determination of thirteen carbohydrates. Different from previous approaches, the current GC-MS method was featured by a powerful practicability for simultaneous detection of aldoses, uronic acids, ketoses, and amino sugars; simplifying GC-MS chromatograms and producing a single peak for each derivatized sugar, as well as high resolution, sensitivity, and repeatability. An additional liquid-liquid extraction from derivatization mixtures was performed not only to increase the detection sensitivity of amino sugars but also to decrease the by-products of derivatization. Contrarily, three amino sugars were detected at a very low intensity or not detected at all. The effect of time on monosaccharide- mercaptalated reaction was systematically investigated. The effect of trimethylsilylation on the formation of TMSD was also optimized. The established GC-MS based on TMSD derivatization was suitable for complex carbohydrate analysis and has been successfully applied for the detection of free carbohydrates in water extracts of roots and determination of monosaccharides in polysaccharides.
建立了一种基于三甲基硅基二硫代乙酸酯（TMSD）衍生化的改良 GC-MS 分析方法，用于同时测定 13 种碳水化合物。与以前的方法不同，当前的 GC-MS 方法具有很强的实用性，可同时检测醛糖、糖醛酸、酮糖和氨基糖；简化 GC-MS 图谱，使每个衍生化糖产生单个峰，以及高分辨率、灵敏度和可重复性。从衍生化混合物中进行额外的液-液萃取不仅可以提高氨基糖的检测灵敏度，还可以减少衍生化的副产物。相反，三种氨基糖的检测强度非常低或根本无法检测到。系统研究了时间对单糖-巯基反应的影响。还优化了三甲基硅化对 TMSD 形成的影响。基于 TMSD 衍生化的建立 GC-MS 适用于复杂碳水化合物分析，并已成功应用于检测根水提取物中的游离碳水化合物和多糖中单糖的测定。
