多糖和联萘酚衍生的手性固定相的制备及手性识别机理研究-分析化学专业论文.docxVIP

多糖和联萘酚衍生的手性固定相的制备及手性识别机理研究-分析化学专业论文.docx

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多糖和联萘酚衍生的手性固定相的制备及手性识别机理研究-分析化学专业论文

PAGE PAGE IV III III 相。联萘酚环醚,(9S,10S)-9,10-二氢菲,氢化安息香,萘普生等化合物在自制 柱上都有较好的分离效果。 4、合成了葡萄糖和联萘酚键合型手性固定相,并对其进行了元素分析、热重分 析等表征。手性柱对萘乙醇及联萘酚环醚等化合物有拆分的迹象,分离效果不太理 想,键合量还有待提高,还需进一步进行酯化等衍生化反应。 关键词:高效液相色谱;手性固定相;对映体分离;手性识别;洗脱顺序反转 Abstract Chiral is one of the fundamental properties of nature. It comes from the Greek word, “cheir”, which means “hands”. The two enantiomers of chiral drug may have different effect on living organisms. In this context, the preparation of individual enantiomers has become more and more important. Chromatographic enantioseparation on chiral stationary phases (CSPs) represents one of the most direct and facile approaches for the determination of enantiomeric purity and the preparation of pure enantiomeric drugs. So, the study of chiral recognition mechanism and the synthesis of CSPs are very important. This article mainly discussed the enantioseparations of 1,1-bi-2-naphthol (BINOL) on two polysaccharide-based CSPs, including Chiralpak IA and Chiralcel OD-H. And three chiral stationary phases were synthesized, including coated cellulose tris-cinnamate CSP, bonded binaphthol and glucose CSPs. In Chapter l, the importance and the methods of chiral separation were briefly introduced. The literatures of two kinds of CSPs, polysaccharide derivative and Pirkle type CSPs, were briefly reviewed. And the chromatographic parameters and chiral separation theory were introduced. The enantioseparations of 1,1-bi-2-naphthol (BINOL) were performed on polysaccharide-based chiral stationary phases, Chiralpak IA and Chiralcel OD-H, under normal-phase mode. The effects of polar modifier in the mobile phase on the retention, enantioseparation and elution order were investigated in detail. On the immobilized polysaccharide-based chiral stationary phase, Chiralpak IA, temperature-induced inversion of elution order for BINOL was observed directly. When n-hexane/2-propanol (92/8, v/v) was used as mobile phase, temperature-induced inversion of elution order was observed distinc

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