Comprehensive Profiling by Non-targeted Stable Isotope Tracing Capillary Electrophoresis-Mass Spectrometry: A New Tool Complementing Metabolomic Analyses of Polar Metabolites

Mass spectrometry (MS) driven metabolomics is a frequently used tool in various areas of life sciences; however, the analysis of polar metabolites is less commonly included. In general, metabolomic analyses lead to the detection of the total amount of all covered metabolites. This is currently a major limitation with respect to metabolites showing high turnover rates, but no changes in their concentration. Such metabolites and pathways could be crucial metabolic nodes (e.g., potential drug targets in cancer metabolism). A stable-isotope tracing capillary electrophoresis–mass spectrometry (CE-MS) metabolomic approach was developed to cover both polar metabolites and isotopologues in a non-targeted way. An in-house developed software enables high throughput processing of complex multidimensional data. The practicability is demonstrated analyzing [U-¹³C]-glucose exposed prostate cancer and non-cancer cells. This CE-MS-driven analytical strategy complements polar metabolite profiles through isotopologue labeling patterns, thereby improving not only the metabolomic coverage, but also the understanding of metabolism.     

Deposition of Hydrogen-Free Silicon Nitride Thin Films by Microwave ECR plasma Enhanced Magnetron Sputtering at Room Temperature

Hydrogen-free silicon nitride （SiNx） films were deposited at room temperature by microwave electron cyclotron resonance （MW-ECR） plasma enhanced unbalance magnetron sputtering system. Both Fourier-transform infrared spectroscopy and x-ray photoelectron spectroscopy are used to study the bonding type and the change of bonding structures of the silicon nitride films. The results indicate that the chemical structure and composition of SiNx films deposited by this technique depend strongly on the N2 flow rates, the stoichiometric SiNx film, which has the highest hardness of 22.9 GPa, could be obtained at lower N2 flow rate of 4 sccm.     

A note on the critical points of equilibrium paths in imperfect structures

In a recent work (Int. J. Solids Struct. 37 (2000) 1561) by one of the authors, an extended system for calculating critical points of equilibrium paths in imperfect structures was presented. However, the extremum nature of these points was not analyzed explicitly in that paper. In this note, we will fill in the gap and establish a sufficient condition for determining the buckling strength of imperfect structures.     

1-烃基-1-硅杂环丁烷的合成及其Si—H键伸缩振动频率与结构关系的研究

硅杂环丁烷在有机硅化学中是一类非常重要的小分子环系化合物。由于硅杂环丁烷和环丁烷的环张力相似,因而显示出较高的反应活性。例如能与某些试剂作用,生成开环产物;在光解或热解条件下,产生具有Si=C结构的高活性中间体,可用以合成多种有机硅化合物。     

Flow injection system with in-line Winkler's procedure using 16-way valve and spectrofluorimetric determination of dissolved oxygen in environmental waters

Flow injection spectrofluorimetry with in-line Winklers procedure was developed for the dissolved oxygen (DO) determination. 2-Thionaphthol reacted with iodine produced by Winkler’s method to form fluorescence inactive disulfide compound. To automate the process completely, a 5-channel flow system with a newly designed 16-way valve was assembled. The system consisted of a dispersion coil (DC), a precipitate formation coil (PFC), a precipitate dissolving coil (PDC), and extraction coil (EC). A calibration can be constructed by using a standard iodine solution for dissolved oxygen. The calibration graph was linear over the range 1.2×10⁻⁴∼6.0×10⁻⁴ mol l⁻¹ iodine (1.96∼9.80 mg O l⁻¹)). The relative standard deviation (n=6) was below 0.3% for the 4×10⁻⁴ mol l⁻¹ iodine (6.27 mg O l⁻¹) determination. The sample throughput was 12/h.     

Simultaneous hydrogen and peroxide production by photocatalytic water splitting

Photocatalytic oxidation of water is a promising method to realize large-scale H₂O₂ production without a hazardous and energy-intensive process. In this study, we introduce a Pt/TiO₂(anatase) photocatalyst to construct a simple and environmentally friendly system to achieve simultaneous H₂ and H₂O₂ production. Both H₂ and H₂O₂ are high-value chemicals, and their separation is automatic. Even without the assistance of a sacrificial agent, the system can reach an efficiency of 7410 and 5096 μmol g^–1 h^–1 (first 1 h) for H₂ and H₂O₂, respectively, which is much higher than that of a commercial Pt/TiO₂(anatase) system that has a similar morphology. This exceptional activity is attributed to the more favorable two-electron oxidation of water to H₂O₂, compared with the four-electron oxidation of water to O₂.     

Indium-mediated one-pot reductive conversion of nitroarenes to N-arylacetamides

N-Arylacetamides were prepared in excellent yields from nitroarenes in the presence of acetic anhydride, acetic acid and indium by a one-pot procedure.     

小角激光光散射法测定聚甲基丙烯酸-6-磺己基钠特性粘数-分子量关系

<正> 聚甲基丙烯酸己磺酸钠(PSSHMA)是我们最近合成的,具有较好的抗凝血性能。对于带磺酸基聚合物抗凝血性能的研究,文献报道还不多。我们用羟基己磺酸钠与甲基丙烯酸反应制备了甲基丙烯酸己磺酸钠(SSHMA)新单体,在此异相酯化反应中,使用了四丁基硫酸氢铵(TBAB)作为催化剂,使反应较顺利的进行,得纯单体。经复钙时     

3D Uranyl Organic Frameworks Supported by Rigid Octadentate Carboxylate Ligand: Synthesis,Structure Diversity,and Luminescence Properties

Seven three dimensional (3D) uranyl organic frameworks (UOFs), formulated as [NH₄][(UO₂)₃(HTTDS)(H₂O)] ( 1 ), [(UO₂)₄(HTTDS)₂](HIM)₆ ( 2 , IM=imidazole), [(UO₂)₄(TTDS)(H₂O)₂(Phen)₂] ( 3 , Phen=1,10-phenanthroline), [Zn(H₂O)₄]_0.5[(UO₂)₃(HTTDS)(H₂O)₄] ( 4 ), and {(UO₂)₂[Zn(H₂O)₃]₂(TTDS)} ( 5 ), {Zn(UO₂)₂(H₂O)(Dib)_0.5(HDib)(HTTDS)} ( 6 , Dib=1,4-di(1H-imidazol-1-yl)benzene) and [Na]{(UO₂)₄[Cu₃(u₃-OH)(H₂O)₇](TTDS)₂} ( 7 ) have been hydrothermally prepared using a rigid octadentate carboxylate ligand, tetrakis(3,5-dicarboxyphenyl)silicon(H₈TTDS). These UOFs have different 3D self-assembled structures as a function of co-ligands, structure-directing agents and transition metals. The structure of 1 has an infinite ribbon formed by the UO₇ pentagonal bipyramid bridged by carboxylate groups. With further introduction of auxiliary N-donor ligands, different structure of 2 and 3 are formed, in 2 the imidazole serves as space filler, while in 3 the Phen are bound to [UO₂]²⁺ units as co-ligands. The second metal centers were introduced in the syntheses of 4–7 , and in all cases, they are part of the final structures, either as a counterion ( 4 ) or as a component of framework ( 5 − 7 ). Interesting, in 7 , a rare polyoxometalate [Cu₃(μ₃-OH)O₇(O₂CR)₄] cluster was found in the structure. It acts as an inorganic building unit together with the dimer [(UO₂)₂(O₂CR)₄] unit. Those uranyl carboxylates were sufficiently determined by single crystal X-ray diffraction, and their topological structures and luminescence properties were analyzed in detail.     

Large electro‐optic activity and enhanced temporal stability of methacrylate‐based crosslinking hyperbranched nonlinear optical polymer

A methacrylate‐based crosslinking hyperbranced polymers have been synthesized through initiator‐fragment incorporation radical polymerization and used for the temperature stable electro‐optic (EO) polymer application. This polymer consists of methyl methacrylate, 2‐metacryloxyethyl isocyanate, and ethylene glycol dimethacrylate (EGDMA) monomers. The use of EGDMA as a bifunctional unit resulted in the solvent‐soluble crosslinking hyperbranched chain, so that the EO polymer enhanced glass transition temperatures. A phenyl vinylene thiophene vinylene bridge nonlinear optical chromophore was attached to the polymer backbone as the side‐chain by a post‐functionalization reaction. The loading concentration of the chromophore was varied between 30 and 50 wt % by simply changing the mixing ratio of the precursor polymer to the chromophore. The synthesized EO polymers produced optical quality films with a light propagation loss of 0.61 dB/cm in a slab waveguide at 1.31 μm. The electrically poled film had an EO coefficient (r₃₃) of 139 pm/V at 1.31 μm. The EO crosslinking hyperbranced polymer had a high‐glass transition temperature of 170 °C, and exhibited excellent temporal stability of the EO activity at 85 °C for 500 h. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012