聚NIPAAm及C12整体柱的制备及其性能评价.pdfVIP

摘 要 摘 要 作为第四代分离介质，整体柱因其高的比表面积和优异的传质速率广泛应用于样品 分析。如何获得结构均匀、通透性良好的聚合物整体柱使其对复杂样品实现快速、高效、 高通量的分离分析依然是现在研究的热点。 本文首先以 N -异丙基丙烯酰胺 （NIPAAm）作为反应单体，1,6- 己二醇二丙烯酸酯 （HDDA ）和乙二醇二甲基丙烯酸酯（EDMA ）为交联剂，偶氮二异丁腈 （AIBN ）为引 发剂，采用自由基原位聚合方法制备了有机聚合物整体柱。考察了整体柱的渗透性，热 稳定性和机械性能。此外，通过改变流动相的比例和柱温考察了小分子化合物在目标整 体柱上的保留行为。最后，该整体柱对两组小分子化合物进行了成功分离。 其次，本文还制备了聚（十二碳烯-三羟甲基丙烷三丙烯酸酯- 乙二醇二甲基丙烯酸 酯）[poly(C12-co-TMPTA-co-EDMA)] 整体柱。通过红外光谱法、扫描电镜等方法对其 官能团、内部结构进行了表征。将该整体柱用作高效液相色谱（HPLC ）的固定相，对 4 三组小分子化合物进行了分离，柱效可高达到10 块/米。 关键词 高效液相色谱（HPLC ） 整体柱 制备评价 小分子化合物 I Abstract Abstract As the fourth generation of chromatography sorbents, monolithic column has been used in the field of sample analysis because of its high surface areas and excellent mass transfer properties. In order to achieve rapid, efficient and high throughput separation of complex samples, the preparation of polymeric monolith with uniform structure and good permeability is still a hot research focus. Firstly, a new monolithic column was prepared by in situ free-radical polymerization reaction using N - isopropylacrylamide (NIPAAm) as monomer, hexanediol dia crylate (HDDA) and ethylene dimethacrylate (EDMA) as crosslinking agent, 2, 2’-azobisisobutyronitrile (AIBN) as initiator. The permeability, thermal properties and mechanical strength o f monolithic column were investigated. Furthermore, the influence of the mobile phase composition and temperature on the separation of aromatic compounds was also investigated. Finally, the monolithic column was used to separate two kinds of small molecules