阳离子交换毛细管整体柱的制备及其在毛细管离子色谱中的应用  

Preparation and Application of Cation-exchange Capillary Monolithic Column in Capillary Ion Chromatography

作　　者：李晶[1,2] 朱岩[3] 

机构地区：[1]云南烟草科学研究院,昆明650106 [2]工业控制技术国家重点实验室,浙江大学智能系统与控制研究所,杭州310058 [3]浙江大学化学系,杭州310028

出　　处：《分析化学》2013年第3期400-405,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.20775070,J0830413);浙江省自然科学基金(No.Y4090268)资助项目

摘　　要：以甲基丙烯酸缩水甘油酯(GMA)为功能单体,亚乙基二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为自由基引发剂,在三元致孔剂(正丙醇,1,4-丁二醇,水)的存在下,在320!m内径的弹性石英毛细管柱内制备得到带有环氧功能基团的聚合物整体柱基质;利用Na2SO3对其改性,制备得到磺酸基型阳离子交换毛细管整体柱。采用微流泵、毛细管检测池和紫外检测器构建了毛细管离子色谱系统,并对所制备的整体柱的流体力学参数、色谱性能参数进行评价;采用流速梯度洗脱的方式实现9种常见阳离子(Li+,Na+,NH4+,K+,Cs+,Mg2+,Ca2+,Sr2+,Ba2+)的分离分析;此色谱系统还可应用于牛奶中阳离子和三聚氰胺的分离检测。Polymer-based cation exchange capillary monolithic column was prepared for capillary ion chromatography （CIC） by radical polymerization in a 320%tm-i. d. fused-silica capillary tube, taking glycidyl methacrylate （GMA） as the functional monomer, ethylene dimethacrylate （EDMA） as the cross-linking agent and in the presence of 1,4-butanediol, 1-propanol and water as the porogen solvents and azobisisobutyronitrile （AIBN） as a suitable initiator. Introduction of cation exchange sites was achieved by reacting with Na2SO3. Coupled with the prepared cation exchange capillary monolithic column, a capillary ion chromatography system was constructed with a pump （in ~tlMmin level）, a capillary detection cell and a UV detector, on which more chromatographic characteristics were further studied. With the CIC system, 9 common univalent and divalent cations （Li^＋, Na^＋, NH^4＋, K^＋, Cs^＋, Mg^2＋, Ca^2＋, Sr^2＋, Ba^2＋） were successfully separated and determined by flow rate gradient. Another interesting separation of cations and melamine was also tested on the prepared column.

关 键 词：阳离子交换 毛细管整体柱 毛细管离子色谱 阳离子分析 三聚氰胺 

分 类 号：O657.8[理学—分析化学]