Abstract
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 Anemarrhena asphodeloides roots and determination of monosaccharides in Glossy ganoderma polysaccharides.
Highlights
Carbohydrates from plants, especially oligosaccharides and polysaccharides, have attracted more attention in recent decades because of their biological functions, as well as their roles as structural materials and energy sources [1,2]
A precolumn derivatization based on trimethylsilyl-dithioacetal (TMSD) derivatives has been established, employing GC-MS for a simultaneous analysis of multiple classes of carbohydrates
Some studies have described the optimized derivatization reactions on the formation of TMSDs, these derivatization parameters were only focused on aldoses and uronic acids [4,10]
Summary
Carbohydrates from plants, especially oligosaccharides and polysaccharides, have attracted more attention in recent decades because of their biological functions, as well as their roles as structural materials and energy sources [1,2]. High-performance GC-MS procedure is the technique for carbohydrate analysis, because of the high-resolution separation and sensitivity of detection [3,4] It is well-known that many GC-MS methods have been applied to analyze carbohydrates such as methyl ethers [5], acetates [6], trifluoroacetates [7], trimethylsilyl ethers (TMS) [8], TMS oximes [9], and diethyl dithioacetal [10]. A precolumn derivatization based on trimethylsilyl-dithioacetal (TMSD) derivatives has been established, employing GC-MS for a simultaneous analysis of multiple classes of carbohydrates These carbohydrates were characterized by the simultaneous presence of seven aldoses, one ketose, two uronic acids and three amino sugars. The chromatographic system can provide retention data which serve as complementary information for the positive identification
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