CAJ | 학술논문

合成了一种新型6-单硝基苯胺衍生化β-环糊精配体,将该手性配体键合到 SBA-15有序介孔材料表面,制备了手性液相色谱固定相(NCDSP),采用红外光谱、元素分析、热重分析、质谱、扫描电子显微镜、透射电子显微镜和 X 射线衍射分析对其结构进行了表征.评价了新固定相的基本色谱性能,并将其用于β-受体阻滞剂和二氢黄烷酮类手性药物对映体的拆分.结果表明,14种β-受体阻滞剂和6种二氢黄烷酮类药物在 NCDSP 上均可实现手性分离,其中美托洛尔的分离度达到1.75,2′-羟基黄烷酮的分离度达到5.21,并且分析时间一般不超过20 min.通过与苯胺衍生化β-环糊精固定相(PCDSP)进行对比研究,探讨了新固定相的手性分离机理.
합성료일충신형6-단초기분알연생화β-배호정배체,장해수성배체건합도 SBA-15유서개공재료표면,제비료수성액상색보고정상(NCDSP),채용홍외광보、원소분석、열중분석、질보、소묘전자현미경、투사전자현미경화 X 사선연사분석대기결구진행료표정.평개료신고정상적기본색보성능,병장기용우β-수체조체제화이경황완동류수성약물대영체적탁분.결과표명,14충β-수체조체제화6충이경황완동류약물재 NCDSP 상균가실현수성분리,기중미탁락이적분리도체도1.75,2′-간기황완동적분리도체도5.21,병차분석시간일반불초과20 min.통과여분알연생화β-배호정고정상(PCDSP)진행대비연구,탐토료신고정상적수성분리궤리.
A mono-nitrophenylamino-β-cyclodextrin was synthesized and bonded to the surface of ordered me-soporous SBA-15 for high performance liquid chromatography(HPLC), which obtained a novel 6-mono-nitro-phenylamino-β-cyclodextrin bonded SBA-15 chiral stationary phase( NCDSP). Its structure and morphology were characterized by infrared spectroscopy, elemental analysis, thermal gravimetric analysis, mass spectrome-try, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The basic chroma-tographic property of new NCDSP was evaluated and used for enantioseparations of chiral drugs such asβ-blockers and dihydroflavanones. The fourteen kinds of β-blockers and six kinds of dihydroflavanones chiral drugs can be separated on NCDSP. The resolutions of metoprolol enantiomers and 2′-hydroxy flavanone enantiomers reached 1. 75 and 5. 21 within 20 min, respectively. By comparative study with PCDSP, some enantio-separation mechanisms of the new stationary phase were also discussed.