咔唑-9-乙氧基碳酰肼柱前衍生中性糖的高效液相色谱分析  

Analysis of Neutral Saccharides by High Performance Liquid Chromatography after Pre-column Derivatization with 2-(9-Carbazole)-ethoxycarbonyl Hydrazide

作　　者：张琳[1] 张曦[1] 尤进茂[2] 段继成[1] 张维冰[1] 阎超[1] 张玉奎[1] 

机构地区：[1]中国科学院大连化学物理研究所,大连116011 [2]曲阜师范大学化学系,曲阜273165

出　　处：《分析化学》2004年第8期1002-1005,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目 (No .2 0 3 75 0 40 ;2 0 175 0 3 9;2 0 0 75 0 16)

摘　　要：采用一种新型紫外、荧光衍生试剂咔唑 9 乙氧基碳酰肼 (CEOC Hydrazide)对 5种中性糖 (乳糖 ,甘露糖 ,葡萄糖 ,鼠李糖和山梨糖 )进行柱前衍生 ,并通过紫外、荧光检测的方法进行高效液相色谱 (HPLC)分析。结果表明 :反应温度 6 5℃ ,时间 6 .5h ,醋酸含量为 3.5 % (V/V )的条件下 ,衍生产率可达最大。衍生物的激发和发射波长为λex/λem=2 93/36 0nm ,紫外检测波长 2 5 4nm。检出限范围 1 5～ 6 0fmol。该方法具有检测灵敏度高 ,衍生化反应简单 。2-(9-Carbazole)-ethoxycarbonyl hydrazide (CEOC-Hydrazide), a novel pre-column ultraviolet and fluorescence derivatization reagent, has been developed for the analysis of 5 neutral saccharides (lactose, mannose, glucose, rhamnose, sorbose) by high performance liquid chromatography with fluorescence detection and ultraviolet detection. Derivatizing conditions have been investigated. The results indicate that the maximum yields of this derivativation reaction could be obtained within 6.5 h in the presence of 3.5 % (V/V) acetic acid at 65degreesC. The derivatives are detected with fluorescence detection (lambda(ex)/lambda(em) = 293/360 nm) and ultraviolet detection (254 nm). The range of detection limits is from 15 to 60 fmol. It has been proved that this method has excellent sensitivity and the derivatizing reaction of saccharides is easy and operable. The method is suitable for the analysis of saccharides.

关 键 词：咔唑-9-乙氧基碳酰肼 柱前衍生 中性糖 高效液相色谱 

分 类 号：O657.7[理学—分析化学]