A reversed-phase high-performance liquid chromatography (HPLC) method with beta-cyclodextrin (beta-CD) derivatized as chiral stationary phase is used to directly separate oxazepam (Oxa) and lorazepam (Lor) enantiomers. The effect of temperature on the direct HPLC separation of Oxa and Lor enantiomers is studied for the commercially available beta-CD derivatized bonded chiral stationary phase. Chromatographic peak coalescence, appearing as a plateau between the resolved peaks, is observed at column temperatures of above 13 degrees C. Peak coalescence on the beta-CD derivatized bonded column is attributable to racemization of the Oxa enantiomer. By reducing the column temperature to 13 degrees C, the enantiomeric composition of Oxa and Lor could be determined on the chiral column. This method is expected to be useful for the resolution of 3-hydroxybenzodiazepines. At the same time, the separation mechanism is studied by calculating the thermodynamic parameters. The results reveal that the separation of Oxa and Lor enantiomer is a case of enthalpy-controlled separation, inclusion mechanism does not control the separation. The interaction between Oxa and beta-CD is an additionally strong pi-pi interaction or hydrogen bonding, but that between Lor or beta-CD derivatized is a weak pi-pi interaction or hydrogen bonding. 相似文献
Core-shell surface molecular imprinting technology represents a rather new trend in analytical sciences. In this kind of material, the imprinting sites are located on the surface of the cores or shells of nanoparticles (NPs). This material can improve the capability of recognizing target molecules (analytes), reduce nonspecific adsorption, increase the relative adsorption capacity and selectivity, and accelerate the rate of mass transfer. This review (with 158 references) focuses on recent trends in core-shell MIPs. Following an introduction into the field, a first main section covers common core-materials including silica, magnetic NPs, quantum dots (including semiconductor quantum dots and carbon dots), gold and silver nanoclusters, and up-conversion materials. A further section covers the materials and reagents required for preparing MIPs (with subsections on templates, functional monomers, cross-linkers, initiators, and effects of solvent). A next main section covers synthetic approaches such as precipitation polymerization, emulsion polymerization, and grafting approach. A final section gives examples for applications of core-shell MIPs in analytical assays and in sensing.
Graphical abstract This review (with 158 references) focuses on recent trends in core-shell nanoparticles coated with molecularly imprinted polymers (core-shell MIPs). Three significant synthesis methods are introduced: precipitation, emulsion and grafting approach. Applications of core-shell MIPs concentrate on solid phase extraction, fluorescent probe, surface-enhanced Raman scattering-based sensors and electrochemical sensors.
A poly(vinyl chloride) (PVC) main chain was grafted with poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) containing a quaternary amine group using atom transfer radical polymerization. The successful synthesis of a PVC-g-PDMAEMA graft copolymer was confirmed by Fourier transform infrared, nuclear magnetic resonance, thermogravimetric analysis, and transmission electron microscopy. The PVC-g-PDMAEMA graft copolymer was used as a structure-directing agent (SDA) for the fabrication of a mesoporous thin film containing a titanium dioxide (TiO2) layer. To control the porosity of the resultant inorganic layer, the ratio of SDA to TTIP as well as the concentration of the sol?Cgel was varied. The structure and porosity of the mesoporous film were characterized by XRD and SEM analysis. The mesoporous TiO2 film fabricated on the FTO surface was used as a photoanode for the dye-sensitized solar cell (DSSC). DSSC performance was the greatest when using TiO2 film with a higher porosity and lower interfacial resistance. The highest energy conversion efficiency reached 3.2?% at 100?mW/cm2, which was one of the highest reported values for a quasi-solid-state DSSC with 600-nm-thick TiO2 film. 相似文献
We introduce the p-adic weighted multilinear Hardy-Cesàro operator. We also obtain the necessary and sufficient conditions on weight functions to ensure the boundedness of that operator on the product of Lebesgue spaces, Morrey spaces, and central bounded mean oscillation spaces. In each case, we obtain the corresponding operator norms. We also characterize the good weights for the boundedness of the commutator of weighted multilinear Hardy-Cesàro operator on the product of central Morrey spaces with symbols in central bounded mean oscillation spaces. 相似文献