稀土铕双功能螯合剂的合成  

Synthesis and Characterization of 2,6-{N,N',N,N'-[bis(2,2'-bipyridine-6,6'-dimethyl)bis(aminomethyl)]-pyridine}-4-carboxylic ester-Eu^(3+)

作　　者：赵啟含 常宇[2] 马玉芹[1] 潘利华[2] ZHAO Qihan;CHANG Yu;MA Yuqin;PAN Lihua(School of Chemistry and Environmental Engineering,Changchun University of Science and Technology,Changchun 130022;Changchun Institute of Applied Chemistry Chinese Academy of Sciences,Changchun 130022)

机构地区：[1]长春理工大学化学与环境工程学院,长春130022 [2]中国科学院长春应用化学研究所,长春130022

出　　处：《长春理工大学学报（自然科学版）》2018年第5期127-131,136,共6页Journal of Changchun University of Science and Technology(Natural Science Edition)

基　　金：吉林省重点科技攻关项目(20170204038GX)

摘　　要：均相时间荧光免疫分析(HTRF)是一种快速、简便的分析方法,它将荧光共振能量转移与时间分辨荧光相结合,以稳定的穴状稀土螯合剂为荧光标记物进行检测分析。为了满足HTRF的分析要求,以2,6-二甲基吡啶-4-羧酸甲酯为原料,经N-溴代琥珀酰亚胺(NBS)溴化、水解等化学反应制备得到Eu^(3+)-双功能螯合剂2,6-{N,N',N,N'-[二(2,2’-联吡啶-6,6’-二甲基)]二氨甲基}-吡啶-4-羧酸-Eu^(3+),通过IR、MS等表征方法证明各化合物结构的准确性。对螯合剂荧光性质进行研究。螯合剂的最大激发波长为320nm;最大发射波长为597nm (~5D_0-~7F_2),Stokes位移达到277nm;荧光寿命828μs;荧光量子产率Y_f=0.233。其荧光性质可以满足HTRF的分析要求。Homogeneous-Time Fluorescence Immunoassay(HTRF)was a simple,rapid analysis method being combined fluorescence resonance energy transfer with time-resolved fluorescence,and a stable cryptate rare earth chelator was used as a fluorescent marker.In order to meet the requirements of HTRF,the 2,6-bis methyl pyridine-4-carboxylic ester as starting material via NBS bromination,Eu3+bi-functional chelator2,6-{N,N',N,N'-[bis(2,2'–bi-pyridine-6,6'-dimethyl)bis(aminomethyl)]-pyridine}-4-carboxylic ester-Eu3+was finally prepared by hydrolysis reaction and other chemical reactions.The structure and purity of compounds was confirmed by IR,MS and other characterization methods.The fluorescence properties of the chelating agent showed that the maximum excitation wavelength was 320nm,the maximum emission wavelength was 597nm(5D0-7F2),the Stokes displacement was 277nm,the fluorescence lifetime was 828μs,and the fluorescence quantum yield Yf=0.233.Its fluorescence properties can meet the analysis requirements of HTRF.

关 键 词：中间体 双功能螯合剂 均相时间分辨荧光免疫分析 合成 

分 类 号：O626.3[理学—有机化学]