温敏型及基于低共熔溶剂印迹整体柱的制备及评价
发布时间：2019-01-24 08:45
【摘要】：分子印迹是合成分子识别材料的新兴技术,整体柱是新型的色谱固定相技术,分子印迹聚合物与整体柱技术相结合是一种非常具有应用潜力的色谱固定相,发展新型具有良好识别性能及高柱效的印迹整体柱是当前研究领域的重要挑战。本文以不同方法合成了分子印迹整体柱,并对其制备条件、色谱条件和物理特性等方面进行了考察研究,结果如下： 1本文以酮洛芬(KET)为模板分子,引入丙烯酰胺(AAm)和2-丙烯酰胺-2-甲基丙磺酸(AMPS)作为功能单体,选择原位热引发聚合法,首次合成了温控热敏型酮洛芬印迹整体柱。系统考察了整体柱制备条件,如模板分子与功能单体的比例,功能单体之间的比例等,结合扫描电镜形貌分析和高效液相色谱实验,优化了柱制备条件。结果显示,温度变化对于酮洛芬及结构类似物的保留及识别性能有较大的影响,其中在温度为35度时模板的保留因子(k=0.242)明显大于常温时的保留因子,其印迹因子为5.38。 2首次用低共熔溶剂氯化胆碱溶于乙二醇作为致孔剂合成了具有识别能力的分子印迹液相整体柱。该整体柱以西替利嗪为模板,以4-VP为功能单体,以EDMA为交联剂,加入桥接剂乙酸钴,DMF、离子液体和氯化胆碱-乙二醇为致孔剂在不锈钢管柱中合成整体柱。对聚合过程中一些重要的参数,如模板与功能单体的比例,功能单体与交联剂的比例和氯化胆碱与乙二醇的比例等进行了系统考察。结果显示,单体与交联剂比例为1：3的整体柱上西替利嗪具有良好的容量因子(k=30.2)和高的印迹因子(IF=31.5)。
[Abstract]:Molecular imprinting is a new technology for the synthesis of molecular recognition materials. Monolithic column is a new chromatographic stationary phase technology. The combination of molecularly imprinted polymer and monolithic column technology is a very potential chromatographic stationary phase. Developing new imprinted monolithic columns with good recognition performance and high column efficiency is an important challenge in current research fields. In this paper, molecular imprinted monolithic columns were synthesized by different methods, and their preparation conditions, chromatographic conditions and physical properties were investigated. The results are as follows: 1 in this paper, ketoprofen (KET) was used as template molecule. Using acrylamide (AAm) and 2-acrylamide 2-methylpropanesulfonic acid (AMPS) as functional monomers, the thermally controlled ketoprofen imprinted monolithic column was synthesized by in situ thermal initiation polymerization. The preparation conditions of monolithic column, such as the ratio of template molecule to functional monomer, the proportion of functional monomer and so on, were systematically investigated. The preparation conditions of the column were optimized by SEM morphology analysis and HPLC experiment. The results showed that the retention and recognition properties of ketoprofen and its structural analogues were greatly affected by temperature change. The retention factor (KG 0.242) of the template at 35 鈩，
本文编号：2414318
[Abstract]:Molecular imprinting is a new technology for the synthesis of molecular recognition materials. Monolithic column is a new chromatographic stationary phase technology. The combination of molecularly imprinted polymer and monolithic column technology is a very potential chromatographic stationary phase. Developing new imprinted monolithic columns with good recognition performance and high column efficiency is an important challenge in current research fields. In this paper, molecular imprinted monolithic columns were synthesized by different methods, and their preparation conditions, chromatographic conditions and physical properties were investigated. The results are as follows: 1 in this paper, ketoprofen (KET) was used as template molecule. Using acrylamide (AAm) and 2-acrylamide 2-methylpropanesulfonic acid (AMPS) as functional monomers, the thermally controlled ketoprofen imprinted monolithic column was synthesized by in situ thermal initiation polymerization. The preparation conditions of monolithic column, such as the ratio of template molecule to functional monomer, the proportion of functional monomer and so on, were systematically investigated. The preparation conditions of the column were optimized by SEM morphology analysis and HPLC experiment. The results showed that the retention and recognition properties of ketoprofen and its structural analogues were greatly affected by temperature change. The retention factor (KG 0.242) of the template at 35 鈩，
本文编号：2414318
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