A rapid assay for angiotensin‐converting enzyme activity using ultra‐performance liquid chromatography–mass spectrometry

Angiotensin‐converting enzyme (ACE) plays an important role in the renin–angiotensin system and ACE activity is usually assayed in vitro by monitoring the transformation from a substrate to the product catalyzed by ACE. A rapid and sensitive analysis method or ACE activity by quantifying simultaneously the substrate hippuryl–histidyl–leucine and its product hippuric acid using an ultra‐performance liquid chromatography coupled with electrospray ionization‐mass spectrometry (UPLC‐MS) was first developed and applied to assay the inhibitory activities against ACE of several natural phenolic compounds. The established UPLC‐MS method showed obvious advantages over the conventional HPLC analysis in shortened running time (3.5 min), lower limit of detection (5 pg) and limit of quantification (18 pg), and high selectivity aided by MS detection in selected ion monitoring (SIM) mode. Among the six natural products screened, five compounds, caffeic acid, caffeoyl acetate, ferulic acid, chlorogenic acid and resveratrol indicated potent in vitro ACE inhibitory activity with IC₅₀ values of 2.527 ± 0.032, 3.129 ± 0.016, 10.898 ± 0.430, 15.076 ± 1.211 and 6.359 ± 0.086 mm , respectively. A structure–activity relationship estimation suggested that the number and the situation of the hydroxyls on the benzene rings and the acrylic acid groups may play the most predominant role in their ACE inhibitory activity. Copyright © 2009 John Wiley & Sons, Ltd.     

Electrochemical performance of a nonaqueous rechargeable lithium-air battery

Nonaqueous rechargeable lithium-air battery has so high specific capacity and specific energy that it is being widely researched by academia, corporation, and different research institutes. When used in dried air and absorbing oxygen form the air, this battery is called lithium-air battery, and its specific capacity based on cathode active material (oxygen) is infinite. However, its cycle performance is very limited as reported by the state-of-the-art researches. This cycle problem is mainly caused by instability of electrolyte. Based on electroanalysis of materials’ electrochemical property, a stable electrolyte solvent (sulfolane) and a lithium salt LiBF₄ are selected as electrolytes in this work. Coupled with other eligible battery materials and careful assembly, the lithium-air battery exhibits favorable cycle performance. Above all, this lithium-air system is evaluated objectively in this paper.     

Preparation and performance of sulfur–carbon composite based on hollow carbon nanofiber for lithium-sulfur batteries

A unique structured hollow carbon nanofiber–sulfur composite material (HCF–S) was fabricated and characterized in lithium-sulfur batteries. It is found that a part of spherical sulfur particles are located in the voids formed by the intertwined fibers and the others are confined in hollow channel of the HCF. The high conductive and porous HCF favors the construction of stable three-dimensional conducting network and convenient infiltration of the electrolytes into the cathode. The HCF–S cathode exhibits excellent electrochemical performance in the electrolyte with LiNO₃. By contrast, the ionic liquid electrolyte provides insufficient shuttle suppression and weakens ion transport, which leads to poor cycle and rate capability.     

Kinetic Study of the Degradation of PAC-1 and Identification of a Degradation Product in Alkaline Condition

A selective and validated stability-indicating LC method was developed for the kinetic study of the degradation of PAC-1, which was carried out in aqueous solutions at 37, 60, 80 and 100 °C with pH 1.5–9.0. Separation was performed on a Kromasil C₁₈ column with acetonitrile–water–fomic acid (30:70:0.1, v/v/v) as mobile phase with a flow rate of 1.0 mL min⁻¹ at 281 nm. The degradation rate obtained indicated a first-order reaction law and the activation energy (E _a) was calculated. The results showed that temperature and pH values were significant factors affecting the degradation of PAC-1. An unknown degradation product in alkaline condition was isolated using a reverse-phase semi-preparative LC system. The structure of the degradation product is identified as 2-hydroxy-3-(2-propenyl)-[[2-hydroxy-3-(2-propenyl)phenyl]methylene]hydrazone utilizing the ¹H NMR, ¹³C NMR, IR and Q-TOF-MS techniques.

     

Copper oxide nanoarray based on the substrate of Cu applied for the chemical sensor of hydrazine detection

This communication reports on a novel amperometric hydrazine sensor of CuO nanoarray based on a Cu substrate. Copper oxide nanoarray was directly grown on Cu substrates using a one-step facile hydrothermal method and was characterized using scanning electron microscopy and X-ray powder diffraction. The electrochemical study has shown that the CuO nanoarray exhibits higher catalytic effect on the hydrazine than the normal CuO nanoparticles. This may be attributed to the special structure of the nanomaterials esp. the substrate of the electric Cu. And the amperometric response showed that the CuO nanoarray modified glassy carbon electrode has a low detection and a high sensitivity for hydrazine.     

Improved microhardness and microtribological properties of bismaleimide nanocomposites obtained by enhancing interfacial interaction through carbon nanotube functionalization

Through the functionalization of multiwalled carbon nanotubes (MWCNTs) by 0,0′‐diallylbisphenol A (DBA), the interface situation between MWCNTs and bismaleimide (BMI) was improved, as detected by scanning electron microscope (SEM) and dynamic mechanical analysis (DMA). The improved interface situation was considered to be the main reason for the huge increased microhardness value and greatly improved the microtribological property of MWCNTs/BMI composites. Besides, the wear mechanism for the composite was also believed to be related to the interfacial situation. The rough wavelike worn surface of pure BMI resin is attributed to its poor load capacity. The smoother waterfall‐shape worn surface of MWCNTs/BMI is related to the interface formed by the addition of MWCNTs while the ultrasmooth worn surface of DBA modified MWCNTs/BMI is due to the greatly improved interfacial interaction of the composite. Copyright © 2008 John Wiley & Sons, Ltd.     

Feasibility-Solvability Theorem for a Generalized System

In this paper, we consider a generalized system in the framework of the formulation proposed by Blum and Oettli. The concepts of feasibility and strict feasibility are introduced for a generalized system and a feasibility-solvability theorem is obtained. This work was supported by the Foundation for Young Teacher in Sichuan University (07069), the National Natural Science Foundation of China (10826064, 10671135) and the Specialized Research Fund for the Doctoral Program of Higher Education (20060610005). The authors thank Professor L.D. Muu (Hanoi) and the referee for valuable comments and suggestions which lead to improvements of this paper.     

Experimental and computational studies of the macrocyclic effect of an auxiliary ligand on electron and proton transfers within ternary copper(II)-Histidine complexes

The dissociation of [Cu^II(L)His]^•2+ complexes [L=diethylenetriamine (dien) or 1,4,7-triazacyclononane (9-aneN₃)] bears a strong resemblance to the previously reported behavior of [Cu^II(L)GGH]^•2+ complexes. We have used low-energy collision-induced dissociation experiments and density functional theory (DFT) calculations at the B3LYP/6-31+G(d) level to study the macrocyclic effect of the auxiliary ligands on the formation of His^•+ from prototypical [Cu^II(L)His]^•2+ systems. DFT revealed that the relative energy barriers of the same electron-transfer (ET) dissociation pathways of [Cu^II(9-aneN₃)His]^•2+ and [Cu^II(dien)His]^•2+ are very similar, with the ET reactions of [Cu^II(9-aneN₃)His]^•2+ leading to the generation of two distinct His^•+ species; in contrast, the proton transfer (PT) dissociation pathways of [Cu^II(9-aneN₃)His]^•2+ and [Cu^II(dien)His]^•2+ differ considerably. The PT reactions of [Cu^II(9-aneN₃)His]^•2+ are associated with substantially higher barriers (>13 kcal/mol) than those of [Cu^II(dien)His]^•2+. Thus, the sterically encumbered auxiliary 9-aneN₃ ligand facilitates ET reactions while moderating PT reactions, allowing the formation of hitherto nonobservable histidine radical cations.