基于氨基酸的金属—有机骨架材料用作高效液相色谱手性固定相研究
发布时间：2019-02-16 11:08
【摘要】：基于多样空间结构、手性孔道环境和易于功能化等特性,手性金属-有机骨架材料(Chirality Metal-Organic Frameworks,CMOFs)作为一种新型多孔材料,在手性拆分领域备受关注。然而,目前我们未见到以氨基酸手性配体为起始原料的CMOFs材料用于手性拆分的研究报道。因此,本论文旨在研究并发展该类CMOFs在液相色谱分离中的应用。论文主要工作内容如下:1)合成了{[Co(L-trp)(bpe)(H_2O)]·H_2O·NO_3}n,对其用作HPLC手性固定相进行了研究。高压匀浆法制成了Co-Trp-CMOF新柱用于多种手性化合物的拆分,考察了流动相组成、流速、进样量以及柱温对色谱拆分的影响。实验结果表明,该手性柱对11种外消旋化合物和3种位置异构体表现出较好的拆分能力。证明了Co-Trp-CMOF作为一种新型的液相色谱固定相的可行性,为手性分离材料的探索提供了新的依据。2)合成了[Zn(L-tyr)]n(L-tyr Zn)、[Zn_4(btc)_2(Hbtc)(L-His)_2(H_2O)_4]·1.5H_2O和{[Zn_2(L-trp)_2(bpe)_2(H_2O)_2]·2H_2O·2NO_3}n三种手性晶体,分别将它们用作HPLC固定相进行了研究。制成了三种液相色谱柱用于常见的外消旋化合物和位置异构体的分离,有多种手性化合物在三种Zn-CMOFs柱上都获得了不用程度的拆分。表明了此类Zn-CMOFs材料在手性分离领域具有一定的应用前景。3)合成了[Co_2(L-Trp)(INT)_2(H_2O)_2(Cl O4)]、[Co_2(sdba)(L-Trp)_2]和Co(L-Glu)(H_2O)·H_2O]_∞三种手性晶体,分别将它们用作HPLC手性固定相进行了研究。分别考察了三种色谱固定相对常见的外消旋化合物和位置异构体的拆分,三种Co-CMOFs柱对多种手性化合物都具有一定的识别能力。说明了该类Co-CMOFs材料对于拓展CMOFs在色谱分离领域的应用具有较好的现实意义。
[Abstract]:As a new porous material, chiral metal-organic skeleton material (Chirality Metal-Organic Frameworks,CMOFs) has attracted much attention in the field of chiral resolution because of its diverse spatial structure, chiral pore environment and easy functionalization. However, we have not seen any studies on the chiral resolution of CMOFs with amino acid chiral ligand as the starting material. Therefore, the purpose of this thesis is to study and develop the application of CMOFs in liquid chromatographic separation. The main contents of this thesis are as follows: 1) {[Co (L-trp) (bpe) (H _ 2O)] H _ 2O NO_3} n has been synthesized and used as a chiral stationary phase for HPLC. A new Co-Trp-CMOF column was prepared for the separation of chiral compounds by high pressure homogenization. The effects of mobile phase composition, flow rate, sample injection amount and column temperature on the separation of chiral compounds were investigated. The experimental results show that the chiral column has good resolution ability for 11 racemic compounds and 3 position isomers. The feasibility of Co-Trp-CMOF as a new stationary phase in liquid chromatography was proved. 2) the synthesis of [Zn (L-tyr)] n (L-tyr Zn),) was carried out. [Zn_4 (btc) _ 2 (Hbtc) (L-His) _ 2 (H _ 2O) _ 4] 1.5H_2O and {[Zn_2 (L-trp) _ 2( bpe) _ 2 (H _ 2O) _ 2] 2H_2O 2NO_3} n chiral crystals, They were used as HPLC stationary phase respectively. Three kinds of liquid chromatographic columns were prepared for the separation of common racemic compounds and position isomers. It is indicated that this kind of Zn-CMOFs material has a certain application prospect in chiral separation. 3) Co_2 (L-Trp) (INT) _ 2 (H _ 2O) _ 2 (Cl O _ 4)] has been synthesized. Three chiral crystals, [Co_2 (sdba) (L-Trp] _ 2] and Co (L-Glu) (H _ 2O) H _ 2O] _ 鈭，
本文编号：2424382
[Abstract]:As a new porous material, chiral metal-organic skeleton material (Chirality Metal-Organic Frameworks,CMOFs) has attracted much attention in the field of chiral resolution because of its diverse spatial structure, chiral pore environment and easy functionalization. However, we have not seen any studies on the chiral resolution of CMOFs with amino acid chiral ligand as the starting material. Therefore, the purpose of this thesis is to study and develop the application of CMOFs in liquid chromatographic separation. The main contents of this thesis are as follows: 1) {[Co (L-trp) (bpe) (H _ 2O)] H _ 2O NO_3} n has been synthesized and used as a chiral stationary phase for HPLC. A new Co-Trp-CMOF column was prepared for the separation of chiral compounds by high pressure homogenization. The effects of mobile phase composition, flow rate, sample injection amount and column temperature on the separation of chiral compounds were investigated. The experimental results show that the chiral column has good resolution ability for 11 racemic compounds and 3 position isomers. The feasibility of Co-Trp-CMOF as a new stationary phase in liquid chromatography was proved. 2) the synthesis of [Zn (L-tyr)] n (L-tyr Zn),) was carried out. [Zn_4 (btc) _ 2 (Hbtc) (L-His) _ 2 (H _ 2O) _ 4] 1.5H_2O and {[Zn_2 (L-trp) _ 2( bpe) _ 2 (H _ 2O) _ 2] 2H_2O 2NO_3} n chiral crystals, They were used as HPLC stationary phase respectively. Three kinds of liquid chromatographic columns were prepared for the separation of common racemic compounds and position isomers. It is indicated that this kind of Zn-CMOFs material has a certain application prospect in chiral separation. 3) Co_2 (L-Trp) (INT) _ 2 (H _ 2O) _ 2 (Cl O _ 4)] has been synthesized. Three chiral crystals, [Co_2 (sdba) (L-Trp] _ 2] and Co (L-Glu) (H _ 2O) H _ 2O] _ 鈭，
本文编号：2424382
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