键合型聚丙烯酰胺衍生物手性固定相的制备与手性识别性能

发布时间：2018-05-14 02:26

本文选题：高效液相色谱 + 手性固定相　；参考：《色谱》2016年01期

【摘要】：高效液相色谱(HPLC)被广泛认为是分离制备光学纯单一对映体的最有效方法。在高效液相色谱手性拆分中,手性固定相(CSP)的性能直接影响到色谱柱的手性分离能力。在众多手性固定相中,键合型手性固定相具有溶剂耐受性好,分离模式灵活等优点,已经发展成为一类重要的手性固定相。本文通过两步化学反应合成了新型的光学活性丙烯酰胺衍生物——(S)-1-丙烯酰-2-(N-苯基甲酰胺基)吡咯烷((S)-APACP),采用核磁共振氢谱表征了(S)-APACP的化学结构;通过3步化学反应制备了键合型聚丙烯酰胺衍生物手性固定相,采用热重分析法表征了聚合物的键合量,采用HPLC评价了键合型手性固定相的识别能力,分析了影响其手性识别能力的因素。研究结果表明,APACP聚合物成功地键合到硅胶表面制备了具有良好溶剂耐受性的键合型手性固定相,其聚合物键合量为10.2%~11.8%,该键合型手性固定相对若干种对映体显示了较好的手性识别能力。
[Abstract]:High performance liquid chromatography (HPLC) is widely regarded as the most effective method for the separation and preparation of optical pure enantiomers. In high performance liquid chromatography (HPLC) chiral resolution, the performance of chiral stationary phase (CSP) has a direct impact on the chiral separation ability of the column. Among the many chiral stationary phases, the bonded chiral stationary phase has been developed into an important chiral stationary phase because of its good solvent tolerance and flexible separation mode. In this paper, a new type of acrylamide derivative, Szoc-1-acrylyl-2-N-phenylformamide, was synthesized by two-step chemical reaction. The chemical structure of Sn-APACP was characterized by nuclear magnetic resonance spectroscopy (NMR). The chiral stationary phase of bonded polyacrylamide derivatives was prepared by three steps chemical reaction. The amount of polymer was characterized by thermogravimetric analysis and the recognition ability of bonded chiral stationary phase was evaluated by HPLC. The factors affecting chiral recognition ability were analyzed. The results show that APACP polymers have been successfully bonded to silica gel surface to prepare a good solvent-tolerant bonded chiral stationary phase. The amount of polymer bonding is 10.2 and 11.8.The chiral fixation of the bonding type shows good chiral recognition ability relative to several enantiomers.
【作者单位】：哈尔滨工程大学材料科学与化学工程学院;日本名古屋大学;
【基金】：国家自然科学基金项目(51103030) 黑龙江省自然科学基金项目(E201419) 哈尔滨市科技创新人才研究专项(2013RFLXJ027) 日本大赛璐公司合作研究基金~~
【分类号】：O652.63

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