Direct liquid chromatographic enantioseparation of sotalol and other β-blockers using an α1-acid glycoprotein-based chiral stationary phase

The behaviour of an α₁-acid glycoprotein-based chiral stationary phase (Chiral AGP) towards changes in pH and organic modifier in the mobile phase was investigated in order to deduce suitable conditions for the liquid chromatographic enantioseparation of a series of β-adrenoreceptor blocking drugs. The effects of the pH of the mobile phase on retention, selectivity and resolution were studied. Methanol was the only non-ionic modifier tested in the mobile phase while different aliphatic carboxylic acids (C₄ to C₈) and alkanesulfonic acids (C₆ to C₈) were used as ionic modifiers. The influence of the nature and concentration of these modifiers on retention and enantioselectivity was investigated. Under these conditions, enantiomeric separations could be obtained for more than 70% of the β-blocking agents examined. The use of heptanoic acid as an ionic additive in the mobile phase has permitted the resolution of sotalol enantiomers. An enantioselective assay for sotalol was then developed and validated.     

Separation of inorganic anions in acidic solution by capillary electrophoresis

Inorganic anions are almost always determined by capillary electrophoresis (CE) at an alkaline pH, so the analytes will be fully ionized. However, a long-chain quaternary ammonium salt usually must be added as a flow modifier to the carrier electrolyte to reverse the direction of the electroosmotic flow. By working at a sufficiently acidic pH, the electroosmotic flow in fused-silica capillaries is virtually eliminated, and anions can be separated simply by differences in their electrophoretic mobilities. Excellent separations were obtained for AuCl₄⁻ and the chloro complexes of platinum group elements in HCl solution at pH 2.0 to 2.4. No additional buffer or flow modifier was needed. This CE technique is an excellent way to follow slow hydrolytic reactions in which one or more of the chloride ligands is replaced by water. Sharp peaks and good separations were also obtained for MnO₄⁻, VO₃⁻, chromate, molybdate, ferrocyanide, ferricyanide and stable complex ions such as chromium oxalate (CrO₃³⁻).     

大活络丸原子吸收指纹图谱和鉴别的研究Ⅰ. 建立生产厂的厂标的无机元素指纹图谱的探讨

目前中药绝大多数指纹图谱都是对中药有机成分,进行研究和建立的指纹图谱,建立无机元素指纹图谱的研究未见报道。文章通过对江西樟树制药厂生产的27批次的大活络丸用原子吸收光谱仪测定的12种无机元素及其建立指纹图谱的研究,尝试用向量相似法和成分数据分析法对大活络丸和不同种类的中药进行鉴别。研究表明无机元素用这两种方法具有较强的预测能力,完全可以达到区分和鉴别是否是大活络丸的效果; 并且证明中药无机元素质量控制标准的建立是可行的。文章通过无机元素指纹图谱建立和不同种类中药的鉴别,为目前中药无机元素质量标准的建立提供了新思路、新方法。     

The reason of the collapse of an ancient kiln in Egnazia from mineralogical and thermal analysis of ceramic finds

Two kilns, one of which collapsed during firing cycle together with its entire pottery load, have been excavated at the Egnazia site in Southern Italy. To understand the reason for the collapse, ‘Broad Line’ typology pottery finds were analysed by complementary analytical techniques. Analytical results not only suggest as cause of collapse sudden overheating in kiln due to uncontrolled increases in temperature, but also indicate a good technological cycle from the recovery of raw materials to the manufacturing and firing process, which tends to disprove the common assumption of non-professional production.     

Crystallization behavior of some unimodal and bimodal linear low‐density polyethylenes at moderate and high supercooling

Effect of molar mass distribution (MMD) and composition distribution (CD) on crystallization behavior of linear low‐density polyethylene materials at moderate and high supercooling was studied using differential scanning calorimetry, hot‐stage polarized light microscopy, small‐angle light scattering, and chip nanocalorimetry methods. A set of uni‐ and bimodal materials having small variation in average molar mass, density, and melt flow rate, but large differences in MMD and CD, was investigated. The results indicate a clear effect of structural heterogeneity on morphology and crystallization behavior of the materials. Broader MMD and CD increased in average radius of superstructures, melting, crystallization temperatures, and isothermal crystallization rate at different supercoolings. Origin of such behavior is discussed. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 1577–1588, 2008     

Generalized balanced tournament designs and related codes

A generalized balanced tournament design, or a GBTD(k, m) in short, is a (km, k, k − 1)-BIBD defined on a km-set V. Its blocks can be arranged into an m × (km − 1) array in such a way that (1) every element of V is contained in exactly one cell of each column, and (2) every element of V is contained in at most k cells of each row. In this paper, we present a new construction for GBTDs and show that a GBTD(4, m) exists for any integer m ≥ 5 with at most eight possible exceptions. A link between a GBTD(k, m) and a near constant composition code is also mentioned. The derived code is optimal in the sense of its size.      

Analysis of the Conformational Composition of 2-Alkyl-4-phenyl-1,3,2-oxazaborinanes

The empirical MM2 and semiempirical AM1 methods were used to calculate the energy of model 2-methyl-4-phenyl-1,3,2-oxazaborinane with full optimization of the molecular geometry. Comparison of the experimental coupling constants for the 2-isobutyl analog and calculated coupling constants as well as the data for the relative energy of the individual conformers indicated that these compounds form a multicomponent equilibrium system containing sofa and a family of half-chair forms.     

Influence of the kind of the Alcoholic Modifier on Chiral Separation of 4-Substituted-Pyrrolidin-2-Ones Using Amylose Based Chiral Stationary Phase

ABSTRACT

The enantioselective separation of 4-substituted-pyrrolidin-2-ones was investigated on a silica-based amylose tris (3, 5-dimetliylphenylcarbamate) (Chiralpak AD) using, normal phase methodology with a mobile phase consisting of H-hexane-alcohol (ethanol, 1-propanol or 2-propanol) in various percentage. Effects of variation of concentration of alcohol and the nature of aliphatic alcohols in the mobile phase were studied. In a general manner, for the ten compounds analysed, the retention times increased and the separations factors were improved on changing the alcohol modifier from 2-propanol to ethanol. The effects of substitution were analysed. Baseline separation was easily obtained in many cases with a maximum resolution factor of 11.     

One-parameter families of supersymmetric isospectral potentials from Riccati solutions in function composition form

In the context of supersymmetric quantum mechanics, we define a potential through a particular Riccati solution of the composition form (F°f)(x)=F(f(x))$(F°f)\left(x\right)=F\left(f\left(x\right)\right)$ and obtain a generalized Mielnik construction of one-parameter isospectral potentials when we use the general Riccati solution. Some examples for special cases of F$F$ and f$f$ are given to illustrate the method. An interesting result is obtained in the case of a parametric double well potential generated by this method, for which it is shown that the parameter of the potential controls the heights of the localization probability in the two wells, and for certain values of the parameter the height of the localization probability can be higher in the smaller well.