Two‐dimensional chromatography as a tool for studying band broadening in size‐exclusion chromatography

Comprehensive 2‐D size‐exclusion chromatography (SEC×SEC) has been realized. SEC×SEC is not a useful technique for characterizing complex polymers. However, it is potentially an elegant tool to study band‐broadening phenomena. If narrow fractions can be collected from the first dimension, the band broadening in the second dimension is only due to chromatographic dispersion. This would allow a clear distinction to be made between chromatographic band broadening (column and extra‐column) and SEC selectivity (band broadening due to sample polydispersity). In comparison with MALDI‐MS, SEC×SEC allows the study of polymers across a much broader molar‐mass range.     

Two-dimensional separation system of coupling capillary liquid chromatography to capillary electrophoresis for analysis of Escherichia coli metabolites

A two-dimensional (2-D) separation system of coupling chromatography to electrophoresis was developed for profiling Escherichia coli metabolites. Capillary liquid chromatography (LC) with a monolithic silica-octadecyl silica column (500 x 0.2 mm ID) was used as the first dimension, from which the effluent fractions were further analyzed by capillary electrophoresis (CE) acting as the second dimension. Field-enhanced stacking was selectively employed as a concentration strategy to interface the two dimensions, which proved to be beneficial for the detection of metabolites. An artificial sample containing 118 standards, some of which lack chromophores or have weak UV absorbance, was used to optimize the 2-D separation system. Under the optimum conditions, 63 components in the artificial sample having absorbance at 254 nm could be well resolved and detected. The utility of the system was demonstrated by comprehensive analysis of E. coli metabolites. Comparing with the previous 2-D separation system we published in Anal. Chem. 2004, 76, 1419-1428, using a longer monolithic column in the first dimension improved the separation efficiency and offered the possibility of increasing the injection volume without compromising the separation efficiency. In the second dimension, field-enhanced stacking was used to improve the concentration sensitivity of the metabolites, and more metabolites in E. coli cell extract were detected and identified using the developed 2-D separation system. In addition, preliminary investigation for future CE-mass spectrometry coupling was also made in the study by using volatile buffers in the capillary LC and CE techniques.     

Synthesis of Substituted Hydroxyspiro([1]benzopyran-2,4'(1'H)-pyrimidine)-2'(3'H)thiones and Hydroxyspiro-([1]benzopyran-2,4'(1'H)-pyrimidin)-2'(3'H)ones

We have developed a novel regioselective method for synthesis of substituted spiro([1]benzopyran-2,4'-(1'H)pyrimidine)-2'-(3'H)thiones and spiro([1]benzopyran-2,4'-(1'H)pyrimidin)-2'-(3'H)ones having one or two hydroxyl groups on the benzene ring.     

Age-dependent variations of cell response to oxidative stress: proteomic approach to protein expression and phosphorylation

We investigated the protein profiles of variously aged rat astrocytes in response to oxidative stress. After H2O2-exposure of cells at 100 microM for 30 min, the relative intensity of ten protein spots changed on two-dimensional (2-D) gels compared with control gels after silver staining. Matrix-assisted laser desorption/ionization-time of flight-mass spectrometry (MALDI-TOF-MS) analysis after in-gel digestion revealed that six of these spots corresponded to three kinds of proteins, each of which was composed of a protein and its modified form with a different isoelectric point (pI). These three proteins were identified as peroxiredoxins (PRDXs) II and III, and calpactin I light chain (p11). H2O2-exposure increased the intensity of the spot with lower pI and simultaneously decreased that of the spot with higher pI for both PRDXs II and III. In addition, the expression of annexin VII, S-adenosyl-L-homocysteine hydrolase, elongation factor II fragment (EF-II), and adenosine deaminase was increased by H2O2-exposure in astrocytes from variously aged rats. Using the Pro-Q Diamond staining, heat shock protein 60 kDa (Hsp 60) and alpha-tubulin were observed to be phosphorylated upon H2O2-exposure. While phosphorylation of alpha-tubulin was correlated positively with age, the changes in abundance of ten protein spots as described above were independent of age. These results suggest that aging does not suppress the responses aimed at limiting injury and promoting repair brought about by severe oxidative stress, and might affect cell dynamics including the formation of microtubules.     

二维卷积在动力学分析中的应用

本文用计算机模拟和二维卷积研究了稀土与间乙酰基偶氮氯膦的显色反应，选择不同的模型参数可描述这类反应的细节，二维卷积则增强对叠合二维谱的分辨。     

Diffusion in a one-dimensional gas of hard point particles

We simulate the classical diffusion of a particle of massM in an infinite one-dimensional system of hard point particles of massm in equilibrium. Each computer run corresponds to about 10⁸ collisions of the diffusive particle. We find that (t) 1/t fort large enough, and a crossover from an M m regime where=2 to=3 forM=m. The diffusion constant has a sharp maximum atM=m. We study moments x(t)² and x(t)⁴, and examine the behavior ofq ² (t)=x(t)⁴/3x(t)²². We find thatq(t)1 (consistent with a normal distribution) in theM limit (for all timest) and in the t limit for allM. On sabbatical leave from IVIC-Instituto Venezolano de Investigaciones Cientificas.     

一锅法制备全乙酰吡喃溴代糖

将未保护的吡喃糖与醋酸酐在分子碘的催化下制得全乙酰吡喃糖 ,随后不经分离直接与溴化氢的冰醋酸溶液( 4 5 %)反应得到全乙酰吡喃溴代糖 .这种一锅法制备全乙酰吡喃溴代糖操作方便 ,收率高 ,经济实用且对环境友好     

A new Monte Carlo simulation for two models of self-avoiding lattice trees in two dimensions

By means of a new Monte Carlo sampling of a grand canonical ensemble, we verify universality for the critical exponents and of two models of lattice trees constrained to be self-avoiding on sites or on bonds. The attrition constants are also obtained. This algorithm, a generalization of that recently proposed by Berretti and Sokal for random walks, appears to optimize the critical slowing down in the scaling region. Systematic and statistical errors are carefully estimated.     

Evaluation of a retention model in comprehensive two-dimensional gas chromatography

Modeling the retention in comprehensive two-dimensional gas chromatography (GC x GC) was achieved using retention indices obtained in conventional GC. Predicted results were compared with experimental data obtained in the two-dimensional separation of a synthetic hydrocarbon mixture. This proved to be helpful in optimizing the operating conditions of GC x GC separation of a complex petroleum sample and in identifying chemical families.     

SBS单组分橡胶防水涂料

探讨了SBS单组分橡胶防水涂料的组成、制备方法及其对性能的影响因素,详细地介绍了该涂料在防水工程应用上的两大独特优势:(1)优异的抗基层形变能力。这一优势,使其具备了屋面防水专用材料和特效材料的条件,解决了以往防水材料一直不能解决的“零点开裂”问题。(2)创造出多种复合防水工法,既克服和解决了卷材与涂料的各自缺点,又发挥了各自的优点,使这种复合防水层成为最有效的防水层。