β-环糊精/硅基杂化多功能手性固定相的制备及其色谱性能研究

Chiral stationary phase is the core and key component in the chiral resolution of HPLC. The development of the new organic-inorganic hybrid materials promotes the research progress of chiral stationary phase of HPLC and the establishment of many kinds of the separation modes of HPLC. The research and development of multifunctional chiral stationary phase with many kinds of the separation modes is one of the emphases and hotspots at the field of the separation materials. The development of preparation methods of the organic-inorganic hybrid materials provides theories and technologies for the development of new multifunctional chiral stationary phases.The project is to build and develop the synthesis and preparation technology for new β-cyclodextrin-silica hybrid organosilica spheres with the different functional groups in the pore space and wall. The materials as the HPLC stationary phases may be used to separate a wide range of organic compounds including chiral molecules under normal or reverse phase mode on a single chromatographic column arising from the multiple interactions provided by organic functional groups in the pore walls and the channel space. The new technologies and methods of the multifunctional separation were established for β-cyclodextrin-silica hybrid chiral stationary phase. The influence of the load of the β-cyclodextrin, the linker length of β-cyclodextrin, the groups of the pore walls and pore diameter on separation behaves of HPLC were systematically investigated, chromatographic separation mechanism with multiple separation function was revealed. A kind of the broad spectrum chiral stationary phase were developed under the normal and reverse phase conditions, which broke the boundaries for the traditional chromatography stationary phase, and the foundation was established for the research and development of new chromatography stationary phase.

手性固定相是高效液相色谱手性分离的核心和关键，研制和开发新型多功能手性固定相是当前高效液相色谱分离材料研究的重要方向之一。有机-无机杂化材料制备技术的发展为新型多功能手性固定相的研制提供了理论基础和技术支持。本项研究结合有机-无机杂化材料功能基团可调控的特点，设计制备孔道与孔壁骨架中含有不同功能基团的新型β-环糊精/硅基杂化手性固定相；系统考察β-环糊精/硅基杂化手性固定相的对映体拆分与非手性化合物分离性能；建立β-环糊精/硅基杂化手性固定相的多功能色谱分离新方法；阐明环糊精负载量、环糊精连接臂、孔壁功能基团以及孔径对色谱性能的影响；结合功能基团提供的多种作用模式，揭示色谱分离机制；开发一类在正/反相模式下具有多种分离功能的广谱型手性固定相，突破传统色谱固定相使用的界限，发展集多种功能于一体的色谱固定相，为新型色谱分离材料的研究与开发奠定了基础。

手性固定相是高效液相色谱手性分离的核心和关键，研制和开发新型多功能手性固定相是当前高效液相色谱分离材料研究的重要方向之一。有机-无机杂化材料制备技术的发展为新型多功能手性固定相的研制提供了理论基础和技术支持。本项研究结合了有机-无机杂化材料功能基团可调控的特点，以表面活性剂为模板， 以β-环糊精硅基衍生物与有机硅试剂为混合硅源，设计制备了粒径在3-10µm，孔道和孔壁骨架中含有不同功能基团的新型β-环糊精/硅基杂化介孔硅球作为高效液相色谱手性固定相；在正相和反相模式下，系统评价了杂化介孔硅球对映体拆分与非手性化合物的色谱分离性能，建立了β-环糊精/硅基杂化手性固定相的多功能色谱分离新方法；阐明了环糊精负载量、环糊精连接臂、孔壁功能基团以及孔径对色谱性能的影响；结合功能基团提供的多种作用模式，揭示了色谱分离机制，研发了一类制备过程简单、多作用模式，在正/反相模式下具有多种色谱分离功能的广谱型手性固定相，突破传统色谱固定相使用的界限，发展了集多种功能于一体的色谱固定相，为新型色谱分离材料的研究与开发奠定了基础。此外，结合高效液相色谱固定相研究中新型色谱固定相的制备技术方法的应用以及手性固定相的研究发展动态，以构建多功能和高分离效能的高效液相色谱固定相为目标，初步开展了石墨烯量子点键合硅胶固定相的制备与多模式色谱分离性能研究以及桥联多环糊精键合型或杂化型手性固定相的制备与手性拆分性能研究，取得了良好的阶段性研究成果。