9-(2-羟乙基)-吖啶酮柱前衍生胆汁酸高效液相色谱分析  

Analysis of Bile Acids by High Performance Liquid Chromatography after Pre-column Derivatization with 9-(2-Hydroxyethyl)-Acridone

作　　者：张琳[1] 尤进茂[2] 张曦[1] 田燕[1] 段继诚[1] 梁振[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9期1131-1134,共4页Chinese Journal of Analytical Chemistry

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

摘　　要：采用一种新型紫外、荧光衍生试剂 9 ( 2 羟乙基 ) 吖啶酮 (HEA) ,在缩合剂 1 乙基 3 ( 3 二甲氨丙基 ) 碳酰二亚胺 (EDC·HCl)及碱性催化剂 4 二甲氨基吡啶 (DMAP)的存在下 ,对 1 0种胆汁酸进行柱前衍生 ,并通过荧光检测的方法进行高效液相色谱 (HPLC)分析。在HypersilBDSC18柱上 ,采用梯度洗脱 ,1 0种胆汁酸衍生物获得了基线分离 ,衍生物的激发和发射波长为λex/λem=40 4/44 0nm。衍生产物稳定性好 ,检测灵敏度高 ,按信噪比S/N =3∶1 ,平均检出限可达 8.3fmol。9-(2-hydroethyl) -acridone (HEA), a novel ultraviolet and fluorescence labelling reagent, has been utilized as pre-column derivatization reagent for the analysis of 10 bile acids by high performance liquid chromatography ( HPLC) with fluorescence detection. HEA reacts with bile acids in the presence of the coupling agent 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride ( EDC . HCl) and the base catalyst 4-dimethylaminopyridine ( DMAP) to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 404 nm and an emission maximum at lambda(em) 440 nm. The labeled derivatives exhibit high stability under reversed-phase conditions. The method, in conjunction with a gradient elution, offers a baseline resolution of the 10 bile acids derivatives on a reversed-phase Hypersil BDS C-18 column. The average detection limit ( at a signal-to-noise ratio of 3) for per injection is 8.3 fmol.

关 键 词：9-(2-羟乙基)-吖啶酮 柱前衍生 胆汁酸 高效液相色谱 血清 含量测定 

分 类 号：O657.7[理学—分析化学]