酶法合成海藻糖芥酸酯的分离纯化与结构鉴定
首发时间:2010-05-19
摘要:采用薄层层析 (TLC)、硅胶柱层析和高效液相色谱 (HPLC) 分离纯化海藻糖芥酸酯,红外光谱(IR)、液质连用 (HPLC-MS) 和核磁共振 (NMR) 鉴定纯化组分,为6’-O-海藻糖芥酸酯和6,6’-O-海藻糖芥酸二酯。TLC分离的最佳条件:点样量2 μL,氯仿/甲醇 (4:1, V/V) 为展开剂,5%硫酸乙醇溶液喷雾,120℃显色20 min。硅胶柱层析分离的最佳条件: 12 mm × 600 mm 硅胶 (100~200目) 层析柱,分离量5 mL,流动相为氯仿/甲醇 (4:1, V/V)。
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Enzymatic Synthesis, Separation and Identification of Erucoyl Trehaloses
Abstract:Erucoyl trehaloses were separated and purified by the thin layer chromatography (TLC), HPLC and silica gel column chromatography, then the purified products were identified by IR, HPLC-MS, and NMR to be 6’-O-erucoyl trehaloses and 6,6’-O- erucoyl trehaloses. The optimum conditions for TLC were confirmed: 2μl of the reaction mixture were applied to silica gel G plates, developed by chloroformmethanol (4:1, V/V), and then detected by spraying with 5% of sulfuric acid in ethanol and heated at 120 ℃ for 20 min. The optimum conditions for silica gel column chromatography were: 5 ml of the reaction mixture was applied to 12 mm × 600 mm silica gel column (100~200 mesh) and chloroform-methanol (4:1, V/V) was used as mobile phase.
Keywords: erucic acid erucoyl trehaloses TLC silica gel chromatography
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