A highly sensitive and rapid assay for protein determination in human urine and penicillin using a Rayleigh light-scattering technique with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt.

A simple and sensitive method was conducted for the determination of trace amounts of proteins with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt (azophloxine, AP) using a Rayleigh light-scattering (RLS) technique. At pH 2.60 and in the presence of an emulsifier OP microemulsion, the RLS of AP can be greatly enhanced by proteins, owing to the interaction between AP and protein. The enhanced intensity is proportional to the concentration of proteins. Four proteins, including bovine serum albumin (BSA), human serum albumin (HSA), lysozyme (Lys) and gamma globulin (gamma-G) have been tested. For example, the linear range of BSA was 0 - 0.06 microg mL(-1) with detection limits of 2.38 ng mL(-1). The method was applied to the analysis of protein in human urine and penicillin samples with satisfactory results. The relative standard deviation was in all instances less than 4.0%, and the recovery was in the range of 97.5 - 104%.     

Novel photoswitching dithienylethenes with ferrocene units

Two novel dithienylethenes with ferrocene units were synthesized by Wittig reaction. The structure of 2a has been established by X‐ray diffraction studies. They could reversibly interconvert between two thermally stable forms, an open and a closed one, using light of different wavelengths as triggers. Copyright © 2006 John Wiley & Sons, Ltd.     

男性型秃发患者发中K,Na,Ca,Mg元素含量分析

采用火焰原子吸收法对３０例男性型秃发患者及３８例毛发健康男性对照者发中宏量元素Ｋ、Ｎａ、Ｃａ、Ｍｇ的含量进行了测定。结果表明，男性型秃发患者发Ｋ含量明显高于对照组，具有统计学上的显著差异（Ｐ〈０．０１）。发Ｎａ、Ｃａ、Ｍｇ含量在两组间未见显著差异（Ｐ〉０．０５）。本文提示，体内某些宏量元素变化对男性型秃发可能产生一定影响。     

Powering the analytical glow discharge

The glow discharge may be powered by direct current (dc), radio frequency (rf) and pulsed discharge sources. Each has specific advantages and special features that should be considered by analysts using the various forms of glow discharge spectroscopy. This paper reviews some of the factors that contribute to the selection of a power source for the glow discharge.     

The Baylis-Hillman condensation of alpha,beta-conjugate cycloketones with aldehydes using diethylaluminum iodide alone as the promoter

The Baylis-Hillman condensation of three types of alpha,beta-conjugate cycloketones with aldehydes was successfully performed by using diethylaluminum iodide as the Lewis acid promoter alone without the direct use of a Lewis base. The reaction proceeded to completion at 0 degree C in CH2Cl2 within 24 h to give modest to good yields (53-72%).     

The Studies of Lanthanide Shift Reagents in NMR Spectroscopy

The action of a series of lanthanide chelate complexes LnL₃, where Lu=La, Pr, Nd, Sm, Eu, Dy, Ho, Er and Yb; L= dbm (dibenzoylmethanato), dpm (dipivaloylmethanato), and acac acetylactonato), on nmr spectra of 2-butanol has been studied. The origin of shifting abilities and shifting sign of various lanthanide ions are explained by means of Bleaney's theory.     

Adsorption, desorption and activities of acid phosphatase on various colloidal particles from an Ultisol

Adsorption, desorption and activity of acid phosphatase on various soil colloidal particles and pure clay minerals were studied. Higher adsorption amounts and low percentage of desorption of acid phosphatase were found on fine soil clays (<0.2 μm). Electrostatic force and ligand exchange are the major driving forces that are involved in the adsorption of enzymes on soil clays. More enzyme molecules were adsorbed on soil clays in the presence of organic components. However, enzymes on organic clays were more easily released. One-third of the enzyme on goethite was adsorbed via ligand exchange process. Some other interactions, such as van der Waals force, hydrophobic force and hydrogen bonding may be more important in the adsorption of enzyme on kaolinite and the enzyme in this system cannot be easily removed. Coarse clays (0.2–2 μm) and inorganic soil clays had higher affinities for enzyme molecules than fine clays and organic clays, respectively. The activity of enzyme bound on soil clays was inhibited and the thermal stability was increased in the presence of organic matter. Data obtained in this study are helpful for a better understanding of the interactions of enzymes with inorganic and organic constituents in soil and associated environments.     

Simple synthesis of aminoquinoline/ethylaniline copolymer semiconducting nanoparticles

Pure copolymer nanoparticles from 8-aminoquinoline (AQ) and 2-ethylaniline (EA) were easily synthesized by a chemically oxidative polymerization in three different aqueous media. The potential and temperature of polymerization solution were used to successfully follow the polymerization progress. The molecular and morphological structures of the resulting AQ/EA copolymer particles were systematically characterized by IR, UV/Vis, NMR, gel permeation chromatography, laser particle-size analysis, atomic force and transmission electron microscopy. The oxidation potential of the monomers as well as the polymerization yield, structure, and properties of the particles were found to significantly depend on AQ/EA ratio, polymerization temperature and medium. It is surprisingly found that AQ homopolymerization and AQ/EA (50:50) copolymerization at 5 degrees C in HCl simply afford nano-ellipsoids with the major/minor axis diameters of 24/14 nm and 80/67 nm, respectively. A simple method of synthesizing semiconducting pure nanoparticles by introducing the AQ units with positively charged quaternary ammonium groups but in the absence of adscititious stabilizer or sulfonic substituent on the monomers is established first. Both the molecular weight and bulk electroconductivity of the copolymers exhibit a maximum at AQ content of 10 mol %. The solubility and film formability of the copolymers are good in highly polar solvents and reach the optimal at the AQ content of 20 and 10 mol %, respectively.     

Guest sorption and desorption in the metal-organic framework [Co(INA)(2)] (INA=isonicotinate)--evidence of intermediate phases during desorption

The metal-organic framework [Co(INA)(2)]x0.5EtOH (INA = isonicotinate, NC(5)H(4)-4-CO(2)(-)), was synthesised under solvothermal conditions. Its X-ray crystal structure shows channels containing ethanol guests which are hydrogen-bonded to carboxylate oxygens of the framework. The pyridyl rings of the framework alternate between 'open' and 'closed' positions along the channels resulting in large variation in the channel cross-sectional area from ca. 1.4 by 2.3 A at the narrowest point to 4.9 by 5.3 A at the widest. Despite the very small windows, the ethanol guests (of van der Waals diameter ca. 4.2-6.1 A) may be reversibly desorbed and sorbed into the structure quantitatively, as shown by in situ variable-temperture IR spectroscopy and XRPD. The single-crystal structure of the desolvated form [Co(INA)(2)] shows that there is no change in the overall connectivity on desolvation, but the rotational positions of the pyridine rings are altered. This suggests that pyridyl rotation may occur to allow guests to pass in and out. When the synthesis was conducted in 1-propanol solvent [Co(INA)(2)]x0.5Pr(n)OHxH(2)O, was obtained, and a single-crystal X-ray structure revealed the same overall connectivity as in but with pyridine rings disordered over closed and open positions. There was no evidence of included guests from X-ray crystallography, suggesting that they are also highly disordered. Variable-temperature XRPD performed on bulk samples showed peaks which were unsymmetrical and exhibited shoulders, suggesting that for each pattern obtained the material actually consisted of several closely-related phases. The movements of the peaks during desolvation showed the presence of intermediate phases before the final desolvated product was formed. The peak positions of the intermediate phases matched more closely with the calculated pattern for than with or, suggesting that they may have disordered structures similar to. The results also suggest that the intermediate phase represents an initial increase in volume before a larger decrease in volume occurs to give the final desolvated material.     

Structures, stabilities, and electronic and optical properties of c(58) fullerene isomers, ions, and metallofullerenes.

The 1205 classical isomers of fullerene C58, as well as one quasi-fullerene C58 isomer with a heptagonal ring (labeled as Cs:hept) have been investigated by the quantum chemical methods PM3, HCTH/3-21G, and B3LYP/6-31G(d). Isomer C3v:0001, which has the lowest number of adjacent pentagons, is predicted to be the most stable isomer, but the quasi-fullerene isomer Cs:hept is only 2.50 kcal mol-1 higher in energy. Systematic investigations of the electronic properties of C3v:0001 and Cs:hept find that the C3v:0001 isomer has high vertical electron affinity (3.19 eV). The nucleus-independent chemical shifts (NICS) value at the center of Cs:hept (-5.1 ppm) is more negative than that of C60 (-2.8 ppm). The NICS value at the center of the heptagonal ring in Cs:hept (-2.5 ppm) indicates weakly aromatic character. In contrast, the C58(6-) and C58(8-) ions of the C3v:0001 and Cs:hept geometries possess large aromatic character, with NICS values between -14.0 and -26.2 ppm. To clarify the thermodynamic stabilities of C58 isomers at different temperatures, the entropy contributions are taken into account on the basis of the Gibbs energy at the B3LYP/6-31G(d) level. The C3v:0001 isomer prevails in a wide range of temperatures, and the Cs:hept isomer is also an important component around 2800 K. The IR spectra of C58 isomers are simulated to facilitate experimental identification of different isomers. In addition, the electronic spectra and the second-order hyperpolarizabilities are predicted by ZINDO and the sum-over-states model. The static second-order hyperpolarizability of the C3v:0001 isomer is 96.5 % larger than that of C60, and its second-order hyperpolarizabilities at external field frequencies are at least nine times larger than those of C60.