CAJ | 학술논문

采用甲基丙烯酸缩水甘油酯原位聚合物基质,将磺丁基醚-β-环糊精修饰到毛细管内壁,制得了一种毛细管电色谱手性柱(SECDP),并通过红外光谱(IR)和扫描电子显微镜(SEM)表征了其结构.磺酸基可提供足够稳定的正向电渗流(EOF),基于磺丁基醚-β-环糊精在固定相和流动相中的协同作用,通过优化手性添加剂浓度、 pH 值、施加电压、温度及有机调节剂含量等条件,利用该开管电色谱柱拆分了氨氯地平、尼莫地平和尼卡地平等10种地平类手性药物对映体.优化的流动相组成为20 mmol/ L NaH2 PO4(pH =4.0),含4.0 mmol/ L 磺丁基醚-β-环糊精,乙腈的体积分数为10%~25%,施加电压15~25 kV,温度为15℃,电动进样2 kV×5 s,检测波长为236 nm.在上述条件下,分离度(RS )可达3.62,柱效达61011块/ m,分析时间一般为6~15 min.基于色谱分离数据,探讨了相关的手性分离机理.
채용갑기병희산축수감유지원위취합물기질,장광정기미-β-배호정수식도모세관내벽,제득료일충모세관전색보수성주(SECDP),병통과홍외광보(IR)화소묘전자현미경(SEM)표정료기결구.광산기가제공족구은정적정향전삼류(EOF),기우광정기미-β-배호정재고정상화류동상중적협동작용,통과우화수성첨가제농도、 pH 치、시가전압、온도급유궤조절제함량등조건,이용해개관전색보주탁분료안록지평、니막지평화니잡지평등10충지평류수성약물대영체.우화적류동상조성위20 mmol/ L NaH2 PO4(pH =4.0),함4.0 mmol/ L 광정기미-β-배호정,을정적체적분수위10%~25%,시가전압15~25 kV,온도위15℃,전동진양2 kV×5 s,검측파장위236 nm.재상술조건하,분리도(RS )가체3.62,주효체61011괴/ m,분석시간일반위6~15 min.기우색보분리수거,탐토료상관적수성분리궤리.
A novel sulfobutyl ether-β-cyclodextrin ( SBE-β-CD) capillary electrochromatographic column (SECDP) was prepared by glycidyl methacrylate polymer matrix in situ and its modification. Its basic struc-ture was characterized by infrared spectroscopy(IR) and scanning electron microscopy(SEM). The sulfonic acid group could provide a enough and stable positive electroosmotic flow(EOF). Enantioseparations of 10 kinds of chiral dihydropyridine drugs including amlodipine, nimodipine, nicardipine and so on were achieved by synergistic effects of SBE-β-CD in the stationary and mobile phases. Some effect factors such as the chiral additive concentration, pH value, the applied voltage, temperature and organic modifier content were opti-mized. The optimal separation conditions were as follows: the mobile phase consisting of 20 mmol/ L NaH2 PO4 (pH=4. 0), containing 4. 0 mmol/ L of SBE-β-CD, acetonitrile volume content of 10% to 25% , an applied voltage of 15-25 kV, the temperature at 15 ℃, electrokinetic injection 2 kV×5 s and the detection wave-length at 236 nm. Under the above conditions, the separation resolutions(Rs ) of dihydropyridine enantiomers were up to 3. 62, the column efficiency were about 61011 / m, and the analysis time were generally between 6-15 min. Based on the data of chromatographic separations, the related chiral separation mechanism was also discussed. The preparation method of SECDP and chiral separation method were rapid, simple, reprodu-cible and suitable for fast enantioseparations and montoring of chiral dihydropyridine drugs.