新型高效液相色谱固定相的制备与应用研究

【作者】 许志刚；

【导师】 艾萍； 袁黎明；

【作者基本信息】 云南师范大学 ， 环境科学， 2005， 硕士

【摘要】 本论文分为五个部分: 1.综述了纤维素类色谱固定相、全衍生化β-环糊精类色谱固定相的研究进展,并简要介绍了分子印记技术和膜分离技术。 2.制备了纤维素三(3,5-二甲基苯基氨基甲酸酯)色谱柱,对包括醇类、羧酸类、胺类、氨基酸类及药物类的18种手性化合物进行了拆分,结果有15种手性化合物得到了分离。结果表明:该柱不仅有良好的手性拆分能力,而且有广泛的适用性。 3.制备了醋酸纤维素柱,对包括醇类、羧酸类、胺类、氨基酸类及药物类的18种手性化合物进行了拆分,结果有7种手性化合物得到了分离。然后分别筛选(+)-二-O,O′-对甲苯甲酰基-D-酒石酸、(+)-1-苯基-1,2-乙二醇和(+)-苯乙醇酸三种手性化合物作为致孔剂,混合醋酸纤维素涂渍修饰硅胶,致孔剂由乙醇洗脱,得到手性色谱柱,对包括醇类、羧酸类、胺类、氨基酸类及药物类的18种手性化合物进行了拆分。结果这些色谱柱除了能拆分各自致孔剂的外消旋体外,还能拆分结构类似的手性化合物。 4.制备了苯基氨基甲酸酯全衍生化β-环糊精键合硅胶手性柱,对包括醇类、羧酸类、胺类、氨基酸类及药物类的18种手性化合物进行了拆分,结果有11种手性化合物得到了分离,结果令人满意。 5.使用自制高效液相色谱柱:纤维素三(3,5-二甲基苯基氨基甲酸酯)和醋酸纤维素色谱柱,分别对水源水中的芳香族含氮化合物、多环芳烃及其衍生物、芳香族含卤化合物进行了分离。结果表明:自制柱有良好的分离能力,具有操作简便、分析速度快等优点。更多还原

【Abstract】 The thesis includes five sections:1. The cellulose and perderivative β-cyclodextrin chiral stationary phase was reviewed. The molecular imprinting and membrane technology was introduced.2. Cellulose tris(3,5-dimethylphenylcarbamate), which is the best chiral stationary phase of polysaccharide, was synthesized. In the normal phase of high performance liquid chromatography, eighteen chiral compounds, including alcohols, acids, amines, amino acids and drugs, had been resolved on this column. Our experimental results also show that cellulose tris(3,5-dimethylphenylcarbamate) stationary phase possesses the excellent chiral resolution ability.3. Cellulose triacetate was coated on silica gel as stationary phase for HPLC and the pores of membrane were created by chiral additive (+)-di-O,O’-p-toluyl-D-tartarric acid, (+)-l-phenyl-l,2-ethanediol and (+)-L-mandelic acid, respectively. The results show that those stationary phases not only can separate extensively racemates, but also can resolve the chiral additive. This is a report, for the first time, that the chiral additive was used in formation of chiral stationary phase of optically active polymer.4. Mono-6-ethylendiamine-β-cyclodextrin was coupled to silica modified by 3-aminopropyltriethoxylsilane via the spacer of chloromethyloxirane. The rest hydroxyls of β-cyclodextrin were derivatized by phenyl isocyanate. The bonded stationary phase was attained and packed into column 250 mm x4.6 mm i.d. under the pressure of 40 Mpa. Fifteen chiral compounds, including alcohols, acids, amines, amino acids and drugs, were resolved on the column in the normal phase of high performance liquid chromatography. Among the 18 racemates, 11 chiral compounds could be separated on the column.5. Some aromatic compounds were separated on the cellulose tris(3,5-dimethylphenylcarbamate) and cellulose triacetate columns.更多还原