Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing, PR China.
J Sep Sci. 2011 Sep;34(18):2523-7. doi: 10.1002/jssc.201100103. Epub 2011 Jul 27.
Monodisperse spherical periodic mesoporous organosilicas (PMOs) with ethane integrated in the framework were synthesized and their application as stationary phase for chromatographic separation is demonstrated. The ethane-PMOs were prepared by condensation of 1,2-bis(triethoxysilyl)ethane (BTSE) in basic condition using octadecyltrimethylammonium chloride (C(18)TMACl) as template and ethanol as co-solvent. The morphology and mesoporous structure of ethane-PMOs were controlled under different concentrations of sodium hydroxide (NaOH) and EtOH. The results of scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), nitrogen sorption measurement, Fourier transform infrared spectroscopy (FT-IR) and elemental analysis showed that ethane-PMOs have spherical morphology, uniform particle distribution, highly ordered pore structure, high surface area and narrow pore-size distribution. The column packed with these materials exhibits good permeability, high chemical stability and good selectivity of mixtures of aromatic hydrocarbons in normal phase high-performance liquid chromatography (HPLC).
合成了具有乙烷集成骨架的单分散球形周期性介孔有机硅(PMO),并证明其可用作色谱分离的固定相。乙烷-PMO 是通过在碱性条件下用十八烷基三甲基氯化铵(C(18)TMACl)作为模板和乙醇作为共溶剂缩合 1,2-双(三乙氧基硅基)乙烷(BTSE)制备的。在不同浓度的氢氧化钠(NaOH)和 EtOH 下控制乙烷-PMO 的形态和介孔结构。扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粉末 X 射线衍射(XRD)、氮气吸附测量、傅里叶变换红外光谱(FT-IR)和元素分析的结果表明,乙烷-PMO 具有球形形态、均匀的颗粒分布、高度有序的孔结构、高表面积和窄的孔径分布。用这些材料填充的色谱柱在正相高效液相色谱(HPLC)中显示出良好的渗透性、高化学稳定性和芳香烃混合物的良好选择性。