Magnetic graphene oxide modified with choline chloride-based deep eutectic solvent for the solid-phase extraction of protein

Four kinds of green deep eutectic solvents (DESs) based on choline chloride (ChCl) have been synthesized and coated on the surface of magnetic graphene oxide (Fe₃O₄@GO) to form Fe₃O₄@GO-DES for the magnetic solid-phase extraction of protein. X-ray diffraction (XRD), vibrating sample magnetometer (VSM), Fourier transform infrared spectrometry (FTIR), field emission scanning electron microscopy (FESEM) and thermal gravimetric analysis (TGA) were employed to characterize Fe₃O₄@GO-DES, and the results indicated the successful preparation of Fe₃O₄@GO-DES. The UV–vis spectrophotometer was used to measure the concentration of protein after extraction. Single factor experiments proved that the extraction amount was influenced by the types of DESs, solution temperature, solution ionic strength, extraction time, protein concentration and the amount of Fe₃O₄@GO-DES. Comparison of Fe₃O₄@GO and Fe₃O₄@GO-DES was carried out by extracting bovine serum albumin, ovalbumin, bovine hemoglobin and lysozyme. The experimental results showed that the proposed Fe₃O₄@GO-DES performs better than Fe₃O₄@GO in the extraction of acidic protein. Desorption of protein was carried out by eluting the solid extractant with 0.005 mol L⁻¹ Na₂HPO₄ contained 1 mol L⁻¹ NaCl. The obtained elution efficiency was about 90.9%. Attributed to the convenient magnetic separation, the solid extractant could be easily recycled.     

Three-dimensional roselike α-Ni(OH)2 assembled from nanosheet building blocks for non-enzymatic glucose detection

Glucose detection plays very important roles in diagnostics and management of diabetes. The search for novel catalytic materials with appropriate architectures is the key step in the fabrication of highly sensitive glucose sensors. In this work, α-Ni(OH)₂ roselike structures (Ni(OH)₂-RS) assembled from nanosheet building blocks were successfully synthesized by a hydrothermal method through the hydrolysis of nickel chloride in the mixed solvents of water and ethanol with the assistance of polyethylene glycol (PEG). The structure and morphology of the roselike α-Ni(OH)₂ were characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD) and N₂ adsorption–desorption isotherm measurement. TEM and FE-SEM images showed that the synthesized Ni(OH)₂ was roselike and the size of the leaf-shaped nanosheet was about 5 nm in thickness, which leads to larger active surface areas and faster electron transfer for the detection of glucose. Compared with the bare GCE and bulk Ni(OH)₂/GCE, the Ni(OH)₂-RS/GCE had higher catalytic activity toward the oxidation of glucose. Under the optimal conditions, the Ni(OH)₂-RS/GCE offers a variety of merits, such as a wide linear response window for glucose concentrations ranging from 0.87 μM to 10.53 mM, short response time (3 s), a lower detection limit of 0.08 μM (S/N = 3), as well as long term stability and repeatability.     

Propane σ‐Complexes on PdO(101): Spectroscopic Evidence of the Selective Coordination and Activation of Primary C?H Bonds

Achieving selective C H bond cleavage is critical for developing catalytic processes that transform small alkanes to value‐added products. The present study clarifies the molecular‐level origin for an exceptionally strong preference for propane to dissociate on the crystalline PdO(101) surface via primary C H bond cleavage. Using reflection absorption infrared spectroscopy (RAIRS) and density functional theory (DFT) calculations, we show that adsorbed propane σ‐complexes preferentially adopt geometries on PdO(101) in which only primary C H bonds datively interact with the surface Pd atoms at low propane coverages and are thus activated under typical catalytic reaction conditions. We show that a propane molecule achieves maximum stability on PdO(101) by adopting a bidentate geometry in which a H Pd dative bond forms at each CH₃ group. These results demonstrate that structural registry between the molecule and surface can strongly influence the selectivity of a metal oxide surface in activating alkane C H bonds.     

镥晶体的绝热量热法测试和热力学函数

文章合成了Lu(NO₃)₃(C₂H₅O₂N)_4.H₂O,用红外和元素分析对其进行了表征。用高精度全自动绝热量热仪,测定了该配合物80-382 K温区的热容, 利用实验热容数据, 根据热容与焓、熵的热力学关系, 求出了配合物85-350 K温区内每隔5 K相对于298.15K的标准热力学函数(HT - H298.15)m和(ST - S298.15)m.在80-350 K温度区间内,配合物的热容随温度升高而增大,没有相转移点和热力学吸收峰的出现,该配合物在此温度区间内是稳定存在的。     

C3对称性含膦三足体衍生物及其Eu(Ⅲ)配合物的合成以及与DNA相互作用的研究

设计合成了一种新的C3对称性含膦三足体衍生物N',N',N'-三(亚磷酸三乙酯)缩氨三乙酸(L)及其Eu(Ⅲ)配合物.用1H NMR、13C NMR、红外光谱、元素分析、差热-热重及紫外光谱对其组成和结构进行分析和表征.结果表明,三足体衍生物与稀土苦味酸盐(Eu(pic)3·6H2O)形成了1:1配合物Eu(pic)3L.综合运用紫外-可见吸收光谱法、荧光光谱法和循环伏安法研究了Eu(pic)3L与小牛胸腺DNA之间的结合模式,结果表明,配合物Eu(pic)3L与DNA之间以嵌插形式发生相互作用.将该配合物作为杂交探针,对其在DNA电化学传感器方面的应用进行了探讨.结果发现,该配合物在修饰单链DNA的电极检测作用下,无明显的电化学信号响应,而当将其用于检测杂交双链DNA时,出现了明显信号,并且该配合物的DNA传感器对互补序列、错配序列及非互补序列都有良好的选择作用.     

Single‐Crystal‐to‐Single‐Crystal Transition in an Enantiopure [7]Helquat Salt: The First Observation of a Reversible Phase Transition in a Helicene‐Like Compound

Here it is reported that crystals of an enantiopure [7]helquat salt undergo reversible thermal solid–solid phase transition at 404 K. Differential scanning calorimetry (DSC), capillary electrophoresis (CE), and X‐ray diffraction analysis were used to unravel the mechanistic details of this process. The single‐crystal‐to‐single‐crystal course enabled direct monitoring of the structural changes by in situ variable‐temperature X‐ray diffraction, thus providing the first direct evidence of a solid phase transition in a helicene‐like compound.     

Recent Progress towards Transition‐Metal‐Catalyzed Synthesis of Fluorenes

Fluorenes are a commonly encountered structural motif in materials science, pharmaceutical chemistry, and organic synthesis. Among various strategies towards the synthesis of this unique structure, transition metal‐catalyzed functionalization has emerged as one of the most efficient methods. This Minireview presents an overview of the recent advances in this emerging area by highlighting the reactions’ specificity and applicability and, where possible, provides a mechanistic rationale.     

无机固态材料中气体元素分析的现状与进展

本文介绍了气体元素分析样品表面处理的最新研究成果,综述了热导法、红外吸收法、库仑滴定法、飞行时间质谱法和火花源原子发射光谱法等分析方法在无机固态材料气体分析中的应用现状,分析了各自的特点及存在的问题,并展望了气体分析的发展方向(引用文献85篇)。