原子转移自由基聚合制备新型接枝聚α-D-吡喃半乳糖苷色谱固定相及其性能  

Preparation of New Poly (α-D-galactopyranose) Chain-grafted Silica Chromatographic Stationary Phase by Atom Transfer Radical Polymerization and Its Chromatographic Properties

作　　者：王富强[1] 郝俊霞[1] 戴小军[1] 龚波林[1] 

机构地区：[1]宁夏大学能源化工重点实验室,银川750021

出　　处：《高等学校化学学报》2011年第12期2757-2762,共6页Chemical Journal of Chinese Universities

基　　金：科技部重大基础研究前期专项(批准号:2009CB626608);国家自然科学基金(批准号:201065008);宁夏自然科学基金项目(批准号:NZ0838)资助

摘　　要：以2-溴异丁酰溴为引发剂,CuCl/CuCl2/Me6TREN为催化体系,在室温条件下采用原子转移自由基聚合(ATRP)法将单体6-O-甲基丙烯酰基-1,2,3,4-双-O-亚异丙基-α-D-吡喃半乳糖苷(6-O-methacryloyl-1,2,3,4-di-O-isopropylidene-α-D-galactopyranose,MAIPGal)接枝到5μm大孔硅胶表面上,得到了新型接枝聚合物(pMAIPGal)色谱固定相.考察了单体的合成过程、分离性能以及乙腈、甲醇对溶质保留行为的影响,并采用红外光谱和元素分析对固定相进行了表征.经元素分析测得该聚合物填料的接枝链密度达0.818 mg/m2.在反相色谱模式下,该固定相可基线分离7种酚类化合物和4种胺类化合物.与C18反相柱相比,该合成柱的分离时间较短且分离效果较好.同时,流动相中有机溶剂的含量对酚类和胺类化合物的保留行为有较大的影响,随着流动相中有机溶剂含量的增加,该类化合物的保留减弱.实验结果表明,该填料具有良好的色谱性能.Atom transfer radical polymerization（ATRP） of α-D-galactopyranose was conducted on the surface of 5 μm silicas at ambient temperature using 2-bromoisobutryl bromide as the initiator and CuCl/CuCl2/tris[2-（dimethylamino）ethyl]amine（Me6TREN） as the catalytic system,a novel pMAIPGal chromatographic stationary phase was obtained.The synthesized stationary phase was evaluated in detail to determine its separa-bility,monomer synthetical process,effect of acetonitrile（ACN） and methanol on the retention of solutes.The stationary phase was characterized by means of element analysis and FTIR spectroscopy.The amount of monomer was calculated to be 0.818 mg/m2 on the surface of silica,and the stationary phase can effectively separated seven hydroxybenzene compounds and four amine compounds in reverse phase liquid chromatography（RPLC） mode.Compared with C18 column for separation of these compounds under the same chromatographic conditions,the separation efficiency was better,and the analysis time was shortened.The organic solvent content in the mobile phase has the largest influence on the retention of hydroxybenzene and amine compounds,the retention factor decreased along with increasing the organic solvent content in the mobile phase.The results show that the synthesized stationary phase has satisfactory chromatographic properties.

关 键 词：原子转移自由基聚合 聚α-D-吡喃半乳糖苷 色谱固定相 酚类和胺类化合物分离 色谱性能 

分 类 号：O657[理学—分析化学]