A simple, easy and economical approach for the preparation of a hybrid carbon/silica monolithic capillary column was described for the first time by using silica monolith as framework in combination with hydrothermal carbonization at 180°C. During the preparation process, formamide was introduced to the reaction solutions to reduce the dissolution rate of monolithic silica skeleton and its optimal concentration was 1.5 M. Fourier transform infrared spectrometry, scanning electron microscopy, energy dispersive X‐ray spectrometry, and inverse size exclusion chromatography were carried out to characterize the as‐prepared column. The results demonstrated that carbon spheres ranging from 150 to 1000 nm were successfully attached to the surface of silica skeleton. The prepared hybrid carbon/silica column had a permeability of 4.4 × 10?14 m2. Chromatographic performance of the column was evaluated by separation of various compounds including alkylbenzenes, nucleosides and bases, and aromatic acids. The column exhibited an efficiency of 75 000 plates/m for butylbenzene at the optimal linear velocity of 0.23 mm/s. The successful separation of these compounds and the study on mechanism indicated that the column can be applied in mixed‐mode chromatography. 相似文献
Pyrrolizidine alkaloids are highly hepatotoxic natural chemicals that produce irreversible chronic and acute hepatotoxic effects on human beings. Purification of large amounts of pyrrolizidine alkaloids is necessary for toxicity studies. In this study, an efficient method for targeted analysis and purification of pyrrolizidine alkaloid cis/trans isomers from herbal materials was developed for the first time. Targeted analysis of the hepatotoxic pyrrolizidine alkaloids was performed by liquid chromatography with tandem mass spectrometry (precursor ion scan and daughter ion scan), and the purification of pyrrolizidine alkaloids was achieved with a mass‐directed auto purification system. The extraction and preparative liquid chromatography conditions were optimized. The developed method was applied to analysis of Gynura japonica (Thunb.) Juel., a herbal medicine traditionally used for detumescence and relieving pain but is potentially hepatotoxic as it contains pyrrolizidine alkaloids. Twelve pyrrolizidine alkaloids (six cis/trans isomer pairs) were identified with reference compounds or characterized by liquid chromatography with tandem mass spectrometry, and five individual pyrrolizidine alkaloids, including (E)‐seneciphylline, seneciphylline, integerrimine, senecionine, and seneciphyllinine, were prepared from G. japonica roots with high efficiency. The results of this work provide a new technique for the preparation of large amounts of pyrrolizidine alkaloid reference substances, which will also benefit toxicological studies of pyrrolizidine alkaloids and treatments for pyrrolizidine alkaloid‐induced toxicity. 相似文献
The PPh3‐catalyzed ring‐expansion reaction of sulfamate‐derived cyclic imines with acetylenedicarboxylates has been developed. The reaction works quite efficiently under very mild conditions to afford benzo[g][1,2,3]oxathiazocine‐4,5‐dicarboxylate 2,2‐dioxide derivatives in high yields. 相似文献
Recent advances in direct‐use plasmonic‐metal nanoparticles (NPs) as photocatalysts to drive organic synthesis reactions under visible‐light irradiation have attracted great interest. Plasmonic‐metal NPs are characterized by their strong interaction with visible light through excitation of the localized surface plasmon resonance (LSPR). Herein, we review recent developments in direct photocatalysis using plasmonic‐metal NPs and their applications. We focus on the role played by the LSPR of the metal NPs in catalyzing organic transformations and, more broadly, the role that light irradiation plays in catalyzing the reactions. Through this, the reaction mechanisms that these light‐excited energetic electrons promote will be highlighted. This review will be of particular interest to researchers who are designing and fabricating new plasmonic‐metal NP photocatalysts by identifying important reaction mechanisms that occur through light irradiation. 相似文献
A new tetranuclear organotin carboxylate {[(n‐Bu2SnO)2L]2}n (complex 1 ) was synthesized by the reaction of di‐n‐butyltin oxide with (p‐carboxymethoxy‐phenoxy) acetic acid (LH2) and characterized by elemental analyses: IR, UV–visible, 1H, 13C, 119Sn NMR spectroscopy and single crystal X‐ray study. X‐ray crystallography diffraction data revealed that the complex 1 was polymeric fashion with a chain structure containing a ladder‐like tetranuclear organo‐oxotin cluster. In the complex 1 , the ligand LH2 is coordinated to the central tin(IV) atoms via the carboxylato‐O atoms. The tetranuclear tin system is formed by the bridges through the carbonyl oxygen atom of the carboxylate moieties and making the tin atom of pentacoordinated in distorted trigonal bipyramidal geometry. Single crystal X‐ray data indicate that the complex 1 crystallized in the cubic system with the space group C2/c. 相似文献
The feasibility of realizing a photonic Floquet topological insulator (PFTI) in an atomic ensemble is demonstrated. The interference of three coupling fields will split energy levels periodically, to form a periodic refractive index structure with honeycomb profile that can be adjusted by different frequency detunings and intensities of the coupling fields. This in turn will affect the appearance of Dirac cones in momentum space. When the honeycomb lattice sites are helically ordered along the propagation direction, gaps open at Dirac points, and one obtains a PFTI in an atomic vapor. An obliquely incident beam will be able to move along the zigzag edge of the lattice without scattering energy into the PFTI, due to the confinement of edge states. The appearance of Dirac cones and the formation of a photonic Floquet topological insulator can be shut down by the third‐order nonlinear susceptibility and opened up by the fifth‐order one.