二维金属-有机框架纳米片用作高效液相色谱手性固定相研究  

Two-dimensional Metal-Organic Framework Nanosheets Used as Chiral Stationary Phase in HPLC

作　　者：李毅洁 蒋雪菲 王雪萍 杨梅芳 龙怡幸 袁黎明[1] LI Yi-jie;JIANG Xue-fei;WANG Xue-ping;YANG Mei-fang;LONG Yi-xing;YUAN Li-ming(Department of Chemistry and Chemical Engineering,Yunnan Normal University,Kunming 650500,China)

机构地区：[1]云南师范大学化学化工学院,云南昆明650500

出　　处：《分析测试学报》2024年第12期1902-1910,共9页Journal of Instrumental Analysis

基　　金：国家自然科学基金(22174125)。

摘　　要：采用溶剂热法合成出一种二维金属-有机框架纳米片Co-NH_(2)-BDC,将(1S)-(+)-10-樟脑磺酰氯衍生到Co-NH_(2)-BDC上,制备了手性材料Co-NH_(2)-BDC-(1S)-(+)-10-樟脑磺酰氯,并对Co-NH_(2)-BDC和手性材料Co-NH_(2)-BDC-(1S)-(+)-10-樟脑磺酰氯进行了表征。通过“网包法”制备了手性固定相,用于高效液相色谱(HPLC)对其拆分能力进行考察。Co-NH_(2)-BDC-(1S)-(+)-10-樟脑磺酰氯色谱柱共拆分了26种外消旋体和5种苯系位置异构体,且大部分手性化合物的分离效果较好,达到基线分离。该色谱柱在不同进样量和柱温下具有良好的分离能力和较好的重复性,说明Co-NH_(2)-BDC-(1S)-(+)-10-樟脑磺酰氯所制备的HPLC手性固定相分离效果良好,具有较好的应用前景。The stationary phase is an important part of chromatographic columns and has a huge impact on the resolution performance of chiral compounds.Therefore,in order to improve the efficiency of chromatographic separations,it is necessary to develop new chromatographic stationary phases that are more efficient.In this paper,the two-dimensional metal-organic framework(2D-MOF) nanosheet Co-NH_(2)-BDC was synthesized by solvothermal method,and then(1S)-(+)-10-camphor sulfonyl chloride was derivatized onto Co-NH_(2)-BDC to prepare the chiral material Co-NH_(2)-BDC-(1S)-(+)-10-camphor sulfonyl chloride.A series of characterizations like XRD,FT-IR,CD,BET,SEM were carried out on Co-NH_(2)-BDC and the chiral material Co-NH_(2)-BDC-(1S)-(+)-10-camphor sulfonyl chloride.The chiral stationary phase was prepared by the "net-wrap method",and its separation performance was investigated by high performance liquid chromatography(HPLC).26racemates such as alcohols,ketones,esters,ethers,amines,and 5 benzene positional isomers were separated on the Co-NH_(2)-BDC-(1S)-(+)-10-camphor sulfonyl chloride column in normalphase HPLC(NPC) and reversed-phase HPLC(RPC),and most chiral compounds were separated effectively,achieving baseline resolution.The column still has good separation ability at different injection volumes and column temperatures and has good reproducibility.It was demonstrated that the HPLC chira stationary phase prepared from Co-NH_(2)-BDC-(1S)-(+)-10-camphor sulfonic chloride exhibits good separation efficiency and has certain practical value.

关 键 词：二维金属-有机框架纳米片 高效液相色谱 手性分离 手性固定相 

分 类 号：O657.7[理学—分析化学]