【摘要】：基于多樣空間結(jié)構(gòu)、手性孔道環(huán)境和易于功能化等特性,手性金屬-有機骨架材料(Chirality Metal-Organic Frameworks,CMOFs)作為一種新型多孔材料,在手性拆分領(lǐng)域備受關(guān)注。然而,目前我們未見到以氨基酸手性配體為起始原料的CMOFs材料用于手性拆分的研究報道。因此,本論文旨在研究并發(fā)展該類CMOFs在液相色譜分離中的應(yīng)用。論文主要工作內(nèi)容如下:1)合成了{(lán)[Co(L-trp)(bpe)(H_2O)]·H_2O·NO_3}n,對其用作HPLC手性固定相進(jìn)行了研究。高壓勻漿法制成了Co-Trp-CMOF新柱用于多種手性化合物的拆分,考察了流動相組成、流速、進(jìn)樣量以及柱溫對色譜拆分的影響。實驗結(jié)果表明,該手性柱對11種外消旋化合物和3種位置異構(gòu)體表現(xiàn)出較好的拆分能力。證明了Co-Trp-CMOF作為一種新型的液相色譜固定相的可行性,為手性分離材料的探索提供了新的依據(jù)。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三種手性晶體,分別將它們用作HPLC固定相進(jìn)行了研究。制成了三種液相色譜柱用于常見的外消旋化合物和位置異構(gòu)體的分離,有多種手性化合物在三種Zn-CMOFs柱上都獲得了不用程度的拆分。表明了此類Zn-CMOFs材料在手性分離領(lǐng)域具有一定的應(yīng)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]_∞三種手性晶體,分別將它們用作HPLC手性固定相進(jìn)行了研究。分別考察了三種色譜固定相對常見的外消旋化合物和位置異構(gòu)體的拆分,三種Co-CMOFs柱對多種手性化合物都具有一定的識別能力。說明了該類Co-CMOFs材料對于拓展CMOFs在色譜分離領(lǐng)域的應(yīng)用具有較好的現(xiàn)實意義。
[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，

本文編號：2424382