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将乙二胺衍生化β-环糊精与有序介孔材料SBA-15相结合,得到新型的含稳定脲键的手性固定相(EACDP),匀浆法填充制备毛细管电色谱柱。采用红外光谱、元素分析、质谱、热重分析、电子扫描显微镜表征固定相的结构和形貌。首先测定其孔隙率和电渗流(EOF),发现新的β-环糊精类键合SBA-15柱有良好的通透性,并能产生足够稳定的电渗流。以电渗流为驱动力,在极性有机模式下,发展了拆分β-受体阻滞剂手性药物对映体的电色谱方法。考察了运行电压、温度、有机调节剂以及三乙胺和冰乙酸的含量对手性选择性和分离度的影响,实现了盐酸普萘洛尔、美托洛尔等10种β-受体阻滞剂对映体的拆分。以盐酸普萘洛尔为例,优化的流动相组成为乙腈/甲醇/三乙胺/冰乙酸(85/15/2/2,V/V/V/V),电动进样2 kV×5 s,温度15℃,运行电压15 kV,检测波长214nm,分离度和柱效分别达到1.96和38941块/m,单次分离只需20 min,日内和日间保留时间的RSD分别小于1.2%和2.4%。将方法用于盐酸普萘洛尔片剂的测定,在9.8~250.0μg/mL范围内线性关系良好,对映体加标回收率范围为98.2%~103.2%。
The novel ethylenediamine-derivatized β-cyclodextrin was combined with the ordered mesoporous material SBA-15 to obtain novel stable urea bond-containing chiral stationary phase (EACDP). The structure and morphology of the stationary phase were characterized by FTIR, elemental analysis, mass spectrometry, thermogravimetric analysis and scanning electron microscopy. First, the porosity and the electroosmotic flow (EOF) were measured. The new β-cyclodextrin-bonded SBA-15 column was found to have good permeability and generate a sufficiently stable electroosmotic flow. Using electroosmotic flow as the driving force, the electrochromatographic method for the resolution of chiral drug enantiomers of β-blockers has been developed in polar organic mode. The effects of operating voltage, temperature, organic regulators and the content of triethylamine and glacial acetic acid on the chiral selectivity and resolution were investigated. Ten kinds of β-receptor blockers such as propranolol hydrochloride and metoprolol were achieved Resolution of the enantiomers. Taking propranolol hydrochloride as an example, the optimized mobile phase consisted of acetonitrile / methanol / triethylamine / glacial acetic acid (85/15/2/2, V / V / V / s, temperature 15 ℃, operating voltage 15 kV, detection wavelength 214 nm, resolution and efficiency of 1.96 and 38941 blocks / m, respectively. The single separation time was only 20 min. The RSD of intra- and inter-day retention time was less than 1.2% 2.4%. The method was applied to the determination of propranolol hydrochloride tablets in the range of 9.8 ~ 250.0μg / mL. The recoveries of enantiomers ranged from 98.2% to 103.2%.