新型靛红衍生化β-环糊精键合SBA-15液相色谱固定相的制备与表征

利用靛红的羰基与β-环糊精单取代乙二胺的缩合反应,合成得到种靛红衍生化β-环糊精Schiff碱类化合物。以3-异氰酸丙基三乙氧基硅烷为偶联剂,将其键合到自制的有序介孔二氧化硅材料SBA-15表面,制得种新型的靛红衍生化β-环糊精键合SBA-15液相色谱固定相(ISCDP)。分别对β-环糊精衍生物、SBA-15及固定相进行必要的结构表征。在反相色谱条件下,以卤代尿嘧啶类极性化合物和二取代苯位置异构体为探针,评价新固定相的基本色谱性能。在极性有机溶剂和反相模式下,将新固定相分别用于β-受体阻滞剂药物和丹磺酰化氨基酸对映体的拆分,探讨了相关色谱分离机理。实验表明,靛红吲哚环的引入,增强了环糊精类固定相对卤代尿嘧啶的反相色谱分离能力,分析时间小于7 min。固定相分离硝基苯胺、氨基苯酚和苯二酚的位置异构体时也表现出较高的立体选择性,其中对位异构体均后被洗脱,这与包结作用相关;靛红衍生化β-环糊精配体也提高了固定相的手性分离能力,除疏水作用外,靛红衍生化β-环糊精配体还能提供偶极、氢键、π-π和包结等作用,多种协同作用力有利于提高新固定相的手性和非手性分离的选择性。SBA-15作为键合基质,其有序的孔结构有利于保持色谱柱的良好渗透性和小的传质阻力,在快速高效分离分析中具有应用潜能。     

Synthesis of binuclear palladium complexes with a rigid phenylene bridge linker

The complexes [PdX₂Py]₂(di-NHC) (X = Br or Cl) in which di-NHC represents a di-N-heterocyclic carbene, featuring a rigid phenylene spacer between the carbene units, have been prepared from reactions of the corresponding diimidazolium halide salts with PdCl₂ in pyridine. The molecular structures of three of the complexes were determined by X-ray diffraction studies. The influences of different substitutions and of the halide ligand (Br or Cl) on the structure and reactivity of the complexes have been studied. The catalytic activity of the binuclear palladium complexes was tested in the Mizoroki–Heck reaction of styrene with bromobenzene.     

6-氯-N,N-二甲基嘧啶-4-胺的晶体结构研究

X-射线单晶衍射结果表明,所合成的6-氯-N,N-二甲基嘧啶-4-胺的晶体结构属正交晶系,Pbca空间群,晶胞参数为a=10.922(2),b=7.386(3),c=17.861(6)。由于在其晶格内存在着潜在的C—H…N和C—H…Cl两类分子间弱相互作用力,形成了二维网络结构,化合物变得更加稳定。     

玉米醇溶蛋白高分子材料的制备与应用进展

作为一种天然高分子,玉米醇溶蛋白(Zein)具有疏水性、可降解性、抗菌性等特点。本文在介绍Zein结构、组成及性质的基础上,首先介绍了Zein的提取与脱色方法;然后,总结了通过小分子与高分子改性制备Zein基高分子材料的方法;最后,综述了基于Zein的高分子材料在食品、生物医药、纤维、粘合剂以及其他行业的应用研究进展。作为一类生物相容与生物可降解的天然高分子材料,Zein基材料在药物载体、食品包装、粘合剂等领域将具有更广泛的发展前景。     

Synthesis and characterization of novel blue emitting Na2CaSiO4:Ce3+ phosphor

The blue phosphors Na_(2?x)Ca_(1?x)SiO₄:xCe³⁺ were synthesized by the sol–gel method and their luminescence characteristics were investigated for the first time. Structural information about prepared samples is obtained by analyzing the XRD patterns and SEM micrographs. The photoluminescence (PL) excitation spectra indicate that the Na_(2?x)Ca_(1?x)SiO₄:xCe³⁺ phosphors can be effectively excited by ultraviolet (360 nm) light. The PL emission spectra exhibit tunable blue broadband emission with the dominant wavelength of 427–447 nm under excitation of 360 nm by controlling the doping concentration of Ce³⁺. The concentration quenching effect for Ce³⁺ was found at the optimum doping concentration of 4 mol%. The Commission Internationale de l’Eclairage 1931 chromaticity coordinates of Na_1.96Ca_0.96SiO₄:0.04Ce³⁺ are (0.1447, 0.0787), which are better color purity compared to the commercial Eu²⁺-doped BaMgAl₁₀O₁₇ phosphor. Na_1.96Ca_0.96SiO₄:0.04Ce³⁺ composition shows intense blue emission (peak wavelength, 439 nm) with relative intensity versus commercial BaMgAl₁₀O₁₇:Eu²⁺ blue phosphor (Nichia) 65 and 158 % under 254 and 365 nm excitation, respectively. All the results indicate that Na_(2?x)Ca_(1?x)SiO₄:xCe³⁺ phosphors are potential candidate as a blue emitting phosphor for UV-converting white light-emitting diodes.     

超高效液相色谱法测定餐饮油烟中的十五种醛酮

采用在流动相中添加四氢呋喃的方法来改善丙烯醛-2,4-二硝基苯肼(DNPH)和丙酮-DNPH的分离,然后优化流动相比例和梯度,确定了UPLC分析醛酮-DNPH的色谱条件。有机溶剂消耗量和分析时间分别是传统方法的1/20~1/10和12%~30%;工作曲线线性相关系数、方法检出限和测定下限均满足HJ683-2014的规定;UPLC法测定醛酮的2,4-二硝基苯肼衍生物的平均回收率为91.5%~101%。基于常规的超高效反向C18色谱柱,在40℃条件下建立了高效分离醛酮混标的UPLC方法,方法已用于测定餐饮油烟中醛酮类化合物。     

高β相聚偏氟乙烯基复合体系的制备及压电性能

为了提高聚偏氟乙烯(PVDF)的压电性能,需要寻找有效的途径来提高PVDF的电活性相(β相)含量。 通过水热法成功合成了Ag、ZnO以及二者复合(Ag-ZnO)的3种类型纳米粒子,并与PVDF共混形成PVDF复合薄膜。 通过表征PVDF复合材料的形貌,结晶性能和压电性能,可以发现Ag-ZnO复合纳米粒子的协同作用可以有效提高PVDF的结晶性能和压电性能。 此外,通过单轴拉伸可以使得所有PVDF膜的β相含量得到进一步提高,其中拉伸后的PVDF/Ag-ZnO纳米颗粒(P-C)的β相物质的量分数最高,达到70.0％,最佳的压电系数(d₃₃)达到了31.0 pC/N。     

现场侦检装备在应对化学威胁中的应用与发展

近年来,国内外不断发生的化学恐怖袭击和化学事故仍然是当今人类生存、国家安全所面临的重大威胁。化学侦检是防化应急处置与救援的眼睛,熟练掌握和正确使用侦检装备是应对化学威胁、降低损失和伤亡的关键因素。基于化学传感等技术的侦检装备具有响应快速、智能便携的特点,并且在远程监测和实时值守等方面具有优势。该文针对涵盖电化学传感器、质量敏感型传感器、红外传感器、拉曼传感器、离子迁移谱仪、火焰光度检测器、光致电离检测器、远程遥测传感装备等在内的现场侦检装备,从原理、性能、优势和不足等方面进行了概述,重点阐述了侦检装备在应对化学威胁方面的最新进展,并对其发展趋势、应用前景进行了展望,以期为化学侦检装备在应对化学威胁中的深入研究与应用提供参考。     

CRISPR-Cas System for RNA Detection and Imaging

The system of clustered regularly interspaced short palindromic repeats(CRISPR)and CRISPR-associated endonucleases(Cas)have been widely used in gene editing,disease treatment,molecular diagnosis and chromosome imaging.On account of the programmable target recognition of CRISPR-Cas system and the specific targeting function toward RNA of type Ⅵ class Ⅱ Cas proteins,CRISPR-Cas system has been deployed as RNA recognition and detection tools,exhibiting promising application potentials in the field of RNA detection and imaging.In this review,we summarize the latest research progresses as well as development prospects of CRISPR-Cas system in RNA diagnosis and live cell RNA imaging.     

Designing a 0D/2D S‐Scheme Heterojunction over Polymeric Carbon Nitride for Visible‐Light Photocatalytic Inactivation of Bacteria

Constructing heterojunctions between two semiconductors with matched band structure is an effective strategy to acquire high‐efficiency photocatalysts. The S‐scheme heterojunction system has shown great potential in facilitating separation and transfer of photogenerated carriers, as well as acquiring strong photoredox ability. Herein, a 0D/2D S‐Scheme heterojunction material involving CeO₂ quantum dots and polymeric carbon nitride (CeO₂/PCN) is designed and constructed by in situ wet chemistry with subsequent heat treatment. This S‐scheme heterojunction material shows high‐efficiency photocatalytic sterilization rate (88.1 %) towards Staphylococcus aureus (S. aureus) under visible‐light irradiation (λ≥420 nm), which is 2.7 and 8.2 times that of pure CeO₂ (32.2 %) and PCN (10.7 %), respectively. Strong evidence of S‐scheme charge transfer path is verified by theoretical calculations, in situ irradiated X‐ray photoelectron spectroscopy, and electron paramagnetic resonance.