【摘要】 研究了利用1-苯基-3-甲基-5-吡唑啉酮(PMP)对糖类物质柱前衍生化的方法,优化了反应时间、衍生试剂PMP用量等衍生化条件,最终确立了衍生化的最佳条件为:底物与衍生化试剂加入体积比为1∶3,反应时间120min,反应后样品稀释5倍。采用硅胶柱层析并结合薄层层析,最佳的分离条件为:硅胶柱的柱高为25cm(干硅胶的质量约为24.13g),80mL的洗脱液,加样量为1mL标准液,流速11～12d/min。三糖分离时间约为4.5h,四糖分离时间约为7h,五糖分离时间约为10h。更多还原

【Abstract】 The precolumn derivazation method was introduced using 1-Phenyl-3-Methyl-5-Pyrazolone as derivazation reagent. The derivazation reaction was optimized,including reacting time,PMP consumption and dilution of samples. The ratio of reactant and PMP was 1∶3,the time of reaction was 120min and the production was diluted 5 times. In addition,the silica gel column chromatography and the thin layer chromatographic were used to separate the compound of galactooligo -saccharide. The feasible conditions of separate were confirmed by the experimentation. The altitude of silica gel column was 25cm(the mass of dry silica gel was 24.13g),the volume of eluent was 80mL,the volume of sample was 1mL which was height 2 times,and the velocity of flow was 11~12d/min naturally. In this condition,the time of separating trisaccharides was about 4.5h,the time of tetrasaccharides was about 7h,and the time of separating pentasaccharides was about 10h.更多还原