【摘要】：分子印跡是合成分子識別材料的新興技術(shù),整體柱是新型的色譜固定相技術(shù),分子印跡聚合物與整體柱技術(shù)相結(jié)合是一種非常具有應(yīng)用潛力的色譜固定相,發(fā)展新型具有良好識別性能及高柱效的印跡整體柱是當前研究領(lǐng)域的重要挑戰(zhàn)。本文以不同方法合成了分子印跡整體柱,并對其制備條件、色譜條件和物理特性等方面進行了考察研究,結(jié)果如下： 1本文以酮洛芬(KET)為模板分子,引入丙烯酰胺(AAm)和2-丙烯酰胺-2-甲基丙磺酸(AMPS)作為功能單體,選擇原位熱引發(fā)聚合法,首次合成了溫控熱敏型酮洛芬印跡整體柱。系統(tǒng)考察了整體柱制備條件,如模板分子與功能單體的比例,功能單體之間的比例等,結(jié)合掃描電鏡形貌分析和高效液相色譜實驗,優(yōu)化了柱制備條件。結(jié)果顯示,溫度變化對于酮洛芬及結(jié)構(gòu)類似物的保留及識別性能有較大的影響,其中在溫度為35度時模板的保留因子(k=0.242)明顯大于常溫時的保留因子,其印跡因子為5.38。 2首次用低共熔溶劑氯化膽堿溶于乙二醇作為致孔劑合成了具有識別能力的分子印跡液相整體柱。該整體柱以西替利嗪為模板,以4-VP為功能單體,以EDMA為交聯(lián)劑,加入橋接劑乙酸鈷,DMF、離子液體和氯化膽堿-乙二醇為致孔劑在不銹鋼管柱中合成整體柱。對聚合過程中一些重要的參數(shù),如模板與功能單體的比例,功能單體與交聯(lián)劑的比例和氯化膽堿與乙二醇的比例等進行了系統(tǒng)考察。結(jié)果顯示,單體與交聯(lián)劑比例為1：3的整體柱上西替利嗪具有良好的容量因子(k=30.2)和高的印跡因子(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，

本文編號：2414318