Preparation of a butyl–silica hybrid monolithic column with a “one-pot” process for bioseparation by capillary liquid chromatography

A butyl–silica hybrid monolithic column for bioseparation by capillary liquid chromatography (cLC) was prepared with butyl methacrylate and alkoxysilanes through a “one-pot” process. The effects of polycondensation temperature, volume percentage of N,N′-dimethylformamide, and content of cetyltrimethylammonium bromide and butyl methacrylate on the morphologies of the hybrid monolithic columns prepared were investigated in detail. Baseline separations of proteins and small peptides on the hybrid monolithic column were achieved by cLC with gradient elution. In addition, the resulting hybrid column was also applied for analysis of tryptic digests of bovine serum albumin by cLC coupled with tandem mass spectrometry. The results demonstrate its potential application in separation of complex biological samples.     

Polyhedral oligomeric silsesquioxanes as functional monomer to prepare hybrid monolithic columns for capillary electrochromatography and capillary liquid chromatography

A simple approach to fabricate hybrid monolithic column within the confines of fused-silica capillaries (75 μm i.d.) was introduced. A polyhedral oligomeric silsesquioxanes (POSS) reagent containing a methacrylate group was selected as functional monomer, and copolymerized with bisphenol A dimethacrylate (BPADMA) or ethylene dimethacrylate (EDMA) in the presence of porogenic solvents via thermally initiated free radical polymerization. After optimization of the preparation conditions, two POSS-containing hybrid monoliths were successfully prepared and exhibited good permeability and stability. By comparison of the separation efficiencies of the resulting poly(POSS-co-BPADMA) and poly(POSS-co-EDMA) monoliths in capillary electrochromatography (CEC) and capillary liquid chromatography (cLC), it was indicated the former has better column efficiencies for alkylbenzenes, phenols, anilines and PAHs in CEC and cLC than the latter. Particularly, the hybrid poly(POSS-co-BPADMA) monolith is more suitable for separation of PAHs due to π–π interaction between the analytes and aromatic rings in the surface of monolithic stationary phase.     

Hierarchical Fe3O4@TiO2 Yolk–Shell Microspheres with Enhanced Microwave‐Absorption Properties

A facile and efficient strategy for the synthesis of hierarchical yolk–shell microspheres with magnetic Fe₃O₄ cores and dielectric TiO₂ shells has been developed. Various Fe₃O₄@TiO₂ yolk–shell microspheres with different core sizes, interstitial void volumes, and shell thicknesses have been successfully synthesized by controlling the synthetic parameters. Moreover, the microwave absorption properties of these yolk–shell microspheres, such as the complex permittivity and permeability, were investigated. The electromagnetic data demonstrate that the as‐synthesized Fe₃O₄@TiO₂ yolk–shell microspheres exhibit significantly enhanced microwave absorption properties compared with pure Fe₃O₄ and our previously reported Fe₃O₄@TiO₂ core–shell microspheres, which may result from the unique yolk–shell structure with a large surface area and high porosity, as well as synergistic effects between the functional Fe₃O₄ cores and TiO₂ shells.     

磷杂菲改性腰果酚多元醇的合成及阻燃聚氨酯硬泡性能

采用生物质原料腰果酚和9,10-二氢-9-氧杂-10-膦杂菲-10-氧化物(DOPO)为原料, 合成了一种磷杂菲改性腰果酚多元醇(P-Cardanol-Polyol), 并利用核磁共振氢谱和磷谱对其结构进行了表征. 利用P-Cardanol-Polyol对聚氨酯硬泡(RPUF)进行阻燃改性, 得到一系列阻燃聚氨酯硬泡. 考察了P-Cardanol-Polyol的用量对阻燃聚氨酯硬泡的形貌、 密度、 热导率、 压缩性能、 热稳定性以及阻燃性能的影响. 研究结果表明, P-Cardanol-Polyol对聚氨酯硬泡的密度影响可以忽略不计; 随着P-Cardanol-Polyol的加入, 阻燃聚氨酯硬泡的平均孔径逐渐减小, 热导率也逐渐降低. 未改性聚氨酯硬泡的最大热释放速率和总放热量分别为390 kW/m²和31.9 MJ/m², 阻燃聚氨酯硬泡则降低至340 kW/m²和24.6 MJ/m². 此外, 阻燃聚氨酯硬泡的压缩强度比未改性聚氨酯硬泡提升了约13%. 炭层分析结果表明, P-Cardanol-Polyol能够促进聚氨酯硬泡形成连续致密且具有良好抗热氧化性能的炭层, 有利于减少燃烧过程中可燃性气体的逸出, 从而提升阻燃性能.     

High-performance liquid chromatography quantitative analysis of ephedrine alkaloids in Ephedrae Herba on a perfluorooctyl stationary phase

Ephedrae Herba is one of the most commonly used herbal medicines, and it has been shown that most of the clinical efficacy for cold and asthma is exerted by its alkaloidal components. A simple and sensitive high-performance liquid chromatography method was developed using a perfluorooctyl column for the simultaneous determination of five alkaloids (norephedrine, norpseudoephedrine, ephedrine, pseudoephedrine, and methylephedrine) in Ephedrae Herba. The mobile phase comprising acetonitrile and 15 mM ammonium trifluoroacetate was used to elute the targets in isocratic elution mode. The method was validated for linearity (R² > 0.999), repeatability, intraday and interday precision, recoveries with trueness (93.87–110.99%), limits of detection (5.35–5.76 µg/mL), and limits of quantification (20 µg/mL). The quantitative results revealed that the developed method was precise and accurate. Then it was successfully applied to determine the difference in the contents of three batches of Ephedrae Herba from three pharmaceutical companies.     

pH-responsive pseudorotaxane between comblike PEO-grafted triblock polymer and α-cyclodextrin

The pH-responsive inclusion complexation of comblike triblock polymer, P2VP-b-PPEOMA-b-P2VP, with α-cyclodextrin (α-CD) was studied. The triblock polymer was prepared by reversible addition–fragmentation chain transfer polymerization (RAFT) and formed inclusion complexes (ICs) after selective threading of the PEO segment of the triblock polymer through the cavities of α-CD units. For comparison, PPEOMA homopolymer was prepared, and the inclusion complexation with α-CD was also studied. The formed ICs were characterized by XRD and ¹H NMR. The results revealed that P2VP-b-PPEOMA-b-P2VP can form ICs with α-CD even when forming micelles, and the introduction of P2VP had a great influence on the solution property and the stoichiometry of EO to CD of the inclusion complexes depending on the concentration and the pH of the solution.     

α-Al_2O_3比表面积标准物质的研制

选择市售α-Al2O3粉体作为比表面积标准物质候选材料,采用交叉缩分方法对标准物质样品进行分装。检验结果表明α-Al2O3标准物质样品具有良好的均匀性和稳定性(18个月)。采用国际公认的氮气物理吸附BET方法,联合测量能力经过确认的8家实验室对α-Al2O3标准物质样品进行定值,标准值比表面积为5.47 m2/g,不确定度为0.22 m2/g(k=2)。