Preparative purification of gentamicin components using high-speed counter-current chromatography coupled with electrospray mass spectrometry

We developed a useful and preparative method based on high-speed counter-current chromatography with mass spectrometry (HSCCC/MS) to purify gentamicin C1a, C2/2a and C1 from standard powder. The analytes were purified on the HSCCC model CCC-1000 (multi-layer coil planet centrifuge) with a volatile two-phase solvent system composed of n-butanol/10% aqueous ammonia solution (50:50, v/v) and detected on an LCMS-2020EV quadrupole mass spectrometer fitted with an electrospray ionization (ESI) source system in positive ionization following scan mode (m/z 100-500). The HSCCC/ESI-MS peaks indicated that gentamicin C1a (m/z 450: [M+H](+)), C2/2a (m/z 464: [M+H](+)) and C1 (m/z 478: [M+H](+)) have the peak resolution values of 1.3 and 1.7 from 30 mg of loaded gentamicin powder. The HSCCC yielded 3.9 mg of gentamicin C1a, 12.6 mg of gentamicin C2/2a and 12.0 mg of gentamicin C1. These purified substances were analyzed by LC/MS with scan positive-mode. Based on the LC/MS chromatograms and spectra of the fractions, analytes were estimated to be over 95% pure. These gentamicin isomers of C1a, C2/2a and C1 were evaluated for their antibacterial activities. The overall results indicate that this approach of HSCCC/MS is a powerful technique for the purification of gentamicin components.     

Asymptotic stability for quasi-linear systems whose linear approximation is not assumed to be uniformly attractive

Sufficient conditions are obtained for uniform stability and asymptotic stability of the zero solution of two-dimensional quasi-linear systems under the assumption that the zero solution of linear approximation is not always uniformly attractive. A class of quasi-linear systems considered in this paper includes a planar system equivalent to the damped pendulum x′??+ h(t)x??+ sin x = 0, where h(t) is permitted to change sign. Some suitable examples are included to illustrate the main results.     

Lattice- and network-structure in plastic ice

We have investigated structural and energetic characteristics of plastic ice, which was found in a high pressure region such as 10 GPa by molecular dynamics simulation and free energy calculation. It was predicted that plastic ice intervenes between ice VII and liquid water, in which diffusion is suppressed but rotation is allowed. In the present work, the structure in plastic ice is explored from both local and global view points and focus is placed on the local arrangement, the extent of deviation from the ideal lattice position, and the hydrogen-bonded patterns. The roles of the attractive interaction and the repulsive part of Lennard-Jones potential are also examined. It is found that the higher interaction energy in plastic ice induces a large dislocation of water molecules, which eventually conducts a facile rotation. There are a large amount of hydrogen-bonds which do not orient to the tetrahedral directions. These orientational defects give rise to fusion of the two interpenetrating sublattices of ice VII leading to a plastic phase rather than defect-containing ice VII, which results in a unique network structure of the plastic ice.     

Synergic extraction of metals with α-acyl-d-camphor and optically active lewis bases

Solvent extraction of europium (III), zinc (II) cobalt (II) with α-acyl-d-camphor and optically active isomers of quinine and quinidine was studied in order to obtain information on chirality recognition based on adduct formation between a chiral metal chelate and optically active isomers. It was possible to differentiate clearly between the adduct formation of quinine and that of quinidine in the synergic extraction of cobalt and europium with 3-heptafluorobutyryl- d-camphor and cobalt with 3-trifluoroacetyl-d-camphor.     

Improvement of the hydrothermal stability of MCM-48 mesoporous molecular sieves

This is a review of our recent reports about improving the hydrothermal stability of MCM-48 mesoporous molecular sieves and the related works done by other groups. It presents the different effects of direct addition of various anions, including F^?, SO₄ ^2?, NO₃ ^? and Cl^?, on the improvement of the hydrothermal stability of MCM-48. The different effects of anions on the improvement of the hydrothermal stability and the critical factors influencing the formation of hydrothermally stable MCM-48 are also explained by careful analysis and discussion.     

Column fractionation of acrylonitrile-styrene copolymers

An acrylonitrile-styrene copolymer having 51.4 wt % acrylonitrile content was fractionated using dimethylformamide and a toluene–n-propanol mixture as solvent and nonsolvent, respectively. From characterization of the fractions, it is shown that the copolymer was fractionated principally in accordance with composition. The weight distribution curve of the copolymer was expressed as a function of both molecular weight and chemical composition on a two-dimensional contour map. The same plotting technique was applied to a copolymer having nearly the azeotropic composition.     

Selective separation of water–alcohol binary mixture through poly(maleimide-co-acrylonitrile) membrane

Separation of various alcohols and water through a membrane was carried out by means of a hydrogen-bonding interaction. A membrane obtained from poly(maleimide-co-acrylonitrile) was effective for a selective separation of water from aqueous alcohol solution by pervaporation technique. Spectroscopic analyses verified that this high selectivity was attributed to the hydrogen-bonding interaction between water and maleimide units in the membrane.     

The structure of neopeptins,inhibitors of fungal cell wall biosynthesis

The structures of neopeptins A (1), B (2), and C (3) were elucidated on the basis of chemical and spectroscopic evidences.