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TpBD(NH2)2的D-葡萄糖衍生物高效液相色谱固定相研究
Study on High Performance Liquid Chromatography Stationary Phase of 1,3,5-Trimethylaldehyde Phloroglucinol-3,3′-dini-trobenzidine D Glucose Derivative
【摘要】 使用1,3,5-三甲醛间苯三酚(Tp)、单体3,3′-二硝基联苯胺(DNB)合成了TpBD(NH2)2,并采用后合成修饰策略对该材料进行手性修饰,网包法将其固载到球型硅胶上,得到手性衍生物固定相材料。利用X射线衍射、红外光谱、圆二色谱、热重分析、氮吸附-脱附和扫描电镜对该材料进行表征。实验结果表明材料空间结构和热稳定性良好。使用该材料的手性固定相制备的色谱柱已成功拆分二苯基乙醇酮、华法林、N-(3,5-二硝基苯甲酰)-L-亮氨酸、1-苯乙醇、2-甲基戊酸甲酯、2-乙基己酸、1,2-环氧丁烷、环氧溴丙烷、3-氯-2-丁酮、2-甲基戊醛、3-羟基丁酸乙酯、异丙基缩水甘油醚、乳酸乙酯、1-(1-萘基)乙胺、γ-辛内酯。根据对拆分温度的探究,得到了该色谱柱的最佳拆分温度。选用华法林作为分析对象,评价色谱柱的性能,表明该柱具有良好的重复性,可用作高效液相色谱柱的固定相。
【Abstract】 TpBD(NH2)2 was synthesized using 1,3,5-trimethylaldehyde phloroglucinol(Tp) and the monomer 3,3′-dinitrobenzidine(DNB). This materials were chiral modified using a post synthesis modification strategy. The materials were immobilized on spherical silica gel by a mesh encapsulation method to obtain chiral derivative stationary phase materials. The material was characterized by X-ray diffraction, infrared spectroscopy, circular dichroism, thermogravimetric analysis, nitrogen adsorption desorption, and scanning electron microscopy. The experimental results show that the material has good spatial structure and thermal stability. A chromatographic column prepared using the chiral stationary phase of this material was used for the successful resolution of diphenylethanone, warfarin, N-(3,5-dinitrobenzoyl)-L-leucine, 1-phenylethanol, 2-methylpentanoate methyl ester, 2-ethylhexanoic acid, 1,2-epoxybutane, epoxybromopropane, 3-chloro-2-butanone, 2-methylpentaldehyde, 3-hydroxybutyrate ethyl ester, isopropyl glycidyl ether, ethyl lactate, 1-(1-naphthyl) ethylamine γ-caprolactone. Based on the investigation of resolution temperature, the optimal resolution temperature of the chromatographic column was obtained. Warfarin was selected as the analysis object to evaluate the performance of the chromatographic column, indicating that the column has good repeatability and can be used as a stationary phase for high performance liquid chromatography columns.
【Key words】 chiral stationary phase; chiral covalent organic framework material; high performance liquid chromatography; chiral separation;
- 【文献出处】 云南化工 ,Yunnan Chemical Technology , 编辑部邮箱 ,2023年07期
- 【分类号】O657.72
- 【下载频次】8