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    10 May 2008, Volume 29 Issue 5
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    高等学校化学学报2008年第29卷第5期目次
    2008, 29(5):  0.  doi:
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    下期目次预览
    2008, 29(5):  1.  doi:
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    研究论文
    Synthesis and Luminescent Properties of an Organic Europium(Ⅲ) Complex Containing a Carbazole and an Oxadiazole Fragments as Carrier-transporting Functional Groups
    TANG Huai-Jun1, TANG Hao2, ZHANG Zhi-Guo1, YUAN Ji-Bing1,3, ZHANG Ke-Li1*
    2008, 29(5):  871-875.  doi:
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    A novel europium(Ⅲ) complex containing a carbazole and an oxadiazole fragments as carrier-transporting functional groups was synthesized. Besides photoluminescence and some other physical properties of it were studied, an electroluminescence device doped with the europium complex, ITO/NPB(40 nm)/2\^5% Eu complex: CBP(30 nm)/BCP(10 nm)/Alq3(30 nm)/LiF(1 nm)/Al(100 nm) was fabricated and measured, NPB was N,N’-di(naphthalene-1-yl)-N,N’-diphenyl-benzidiue, CBP was 4,4’-bis(carbazole-9-yl)-biphenyl, BCP was 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline and Alq3 was tris(8-hydroxyquinoline) aluminium, respectively. The device gave pure and bright red light-emitting centered at 612 nm with the half peak bandwidth 4 nm. The turn-on voltage brightness was about 6 V and the maximum luminance brightness 1778 cd/m2 at a driving voltage of 17.3 V.
    Synthesis, Crystal Structure and Antibacterial Activity of Two Novel Complexes of N,N'-Bis(o-oxy-acetate)benzylpropylenediamine with Cu(Ⅱ) and Ni(Ⅱ) and a Complex N-(o-oxy-acetate)benzylpropylenediamine with Cu(Ⅱ)
    WANG Zhan-Liang, ZHU Dong-Sheng, WANG Rong-Shun*
    2008, 29(5):  876-881.  doi:
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    Complex Cu(Ⅱ)L1·H2O·0.25CH3CH2OH(2)[L1=N,N'-bis(o-oxy-acetate) benzylpro-pylenediamine(1)] was synthesized via the reactions between compound 1 and Cu(Ⅱ) dichloride in the solvents of water and ethanol, and Cu(Ⅱ)ClL2·3H2O(3)[L2=N-(o-oxy-acetate) benzylpropylenediamine ] was prepared via the reaction between compound 1 and Cu(Ⅱ) dichloride in the solvents of water and ethanol(pH=8~9). Complex Ni(Ⅱ)L1·2.75H2O(4) was also synthesized by the reactions between the compounds 1 and Ni(Ⅱ) dichloride in water. Compounds 1—4 were characterized by elemental analysis, 1H NMR, FTIR spectroscopy and single crystal X-ray diffraction analysis. There are one molecule(hostmolecule), one water molecule(guestmolecule) and quarter ethanol molecule in one asymmetric unit of complex 2, the Cu(Ⅱ) atom exhibits a distorted octahedral geometry. There are one molecule(hostmolecule) and three water molecules in each unit of complex 3, the Cu(Ⅱ) atom exhibits a distorted octahedral geometry. In the asymmetric unit of complex 4, the Ni(Ⅱ) atom also exhibits a distorted octahedral geometry. Complexes 2 and 3 exhibit good antibacterial properties, while the antibacterial properties decrease in the following order: complex 3>complex 2> compound 1.
    Extraction Mechanism and Property of Phenyl Alanine with n-Octyl-L-hydroxyproline
    CUI Yu1, YIN Shao-Hong1, SUN Guo-Xin1*, TIAN Xiao-Qiang1,2, CUI Yu-Hua1
    2008, 29(5):  882-886.  doi:
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    A novel chiral extractant n-octyl-L-hydroxyproline was synthesized. The extraction mechanism and property of D- or L-phenyl alanine with n-octyl-L-hydroxyproline with n-octane and n-octanol(volume ratio, 7∶3) as the diluent was investigated. The effect of concentrations of extractant and copper ion and pH on the extraction of phenyl alanine was studied. The influence of temperature on the extraction shows that the extraction is endothermic reaction. The extracted species were characterized and the structure was suggested. This result will be helpful for the further study on extracting and separating D,L-phenyl alanine.
    Preparation of Orthorhombic Boron Nitride by Hydrothermal Synthesis Method

    LAI Ze-Feng1,2, GAO Zhi-Zeng2, LIAN Gang1,2, LI Kai1, JING Hai-Peng1, CUI De-Liang1*, ZHAO Xian1, TAO Xu-Tang1

    2008, 29(5):  887-891.  doi:
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    High crystalline orthorhombic boron nitride(oBN) crystallites were prepared by hydrothermal synthesis method. Powder X-ray diffraction(XRD) and high resolution transmission electron microscopy(HRTEM) were used to investigate the phases and crystalline perfection of the BN samples. It is found that the samples are of high crystalline and the dominating phase is oBN when the reaction temperature is 400 ℃. Furthermore, the crystalline perfection and yield of the samples can be improved by adding hydrazine hydrate(N2H4·H2O) and ammonium chloride(NH4Cl) to the solution of reaction reagents. In order to obtain oBN crystallites with high crystalline perfection and high yield, the temperature rising speed should be decreased appropriately during the reaction process. However, oBN becomes less stable, and at the same time, the stability of cBN is improved if the temperature rising speed is slow enough. In addition, the molar ratio of the reactants also has important effects on the phases and the crystalline perfection of the BN samples. These results will be of great significance for controlling the phases of BN and preparing pure cBN.

    Construction of Pretreatment Units with Esterified Silica Monolithic Column and Affinity Membrane on Micro-fluidic Chip

    XU Yi1,2,3*, ZHANG Jian1,2, ZHANG Wen-Pin1,2,3, ZHANG Zhong-Feng1, WEN Zhi-Yu2,3

    2008, 29(5):  892-896.  doi:
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    C18 esterified silica monolithic column emerging from chromatogram realm was made by use of solid-phase extraction medium material in μ-TAS. Several simple solid-phase extraction pretreatment units were set up to preconcentrate dobutamine hydrochloride which was detected by dobutamine hydrochloride-KMnO4-Luminol chemiluminescence system. Trace dobutamine hydrochloride in serum was enriched by C18 esterified silica monolithic column, the average enrichment was 77.2 times, RSD was 12.35%. In order to overcome the shortage of conformable precision, polyamide affinity membrane modified by cibacron blue F3GA was introduced into the pretreatment unit to get rid of interferer from large molecule such as albumin in serum. The affinity membrane was combined with micro-fluidic chip by embedded and external methods and using external-combination pretreatment unit, average enrichment was 89.36 times, RSD was 4.37%. The result indicate the feasibility and validity of the pretreatment unit for trace medicine enrich in serum.
    Fluorescence Cross-correlation Spectroscopy Using Single Wavelength Laser Excitation
    XIE Chao, DONG Chao-Qing, REN Ji-Cun*
    2008, 29(5):  897-901.  doi:
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    The basic principle of fluorescence cross-correlation spectroscopy were introduced in this article. A setup of fluorescence cross-correlation spectroscopy(FCCS) was established with single wavelength laser. After the optimization of the setup, the detection volume is about 0.7 fL. This home-built setup was successfully applied for study of the binding reaction of human immunoglobulin G with goat anti-human immunoglobulin G. With quantum dots(745 nm) and Rhodamine B(580 nm) as probes and 532 nm laser beam as excitation source, the cross-talk effect was near completely suppressed. The molecule numbers in a highly focused volume, concentration, diffusion time and hydrodynamic radius of the reaction product can be determined by FCCS system.
    On-line Isolation of Lysozyme from Egg-white Using Multi-walled Carbon Nanotubes
    DU Zhuo, ZHANG Na, WANG Jian-Hua*
    2008, 29(5):  902-905.  doi:
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    A novel procedure for the extraction of lysozyme from egg-white using carbon nanotubes as a sorbent was developed. Carbon nanotubes after oxidation and purification were used to pack a micro-column which was incorporated into a sequential injection system for facilitating online selective sorption of lysozyme from egg-white. The retained protein was afterwards quantitatively eluted by a carbonate buffer. With a sample loading volume of 2.0 mL, an enrichment factor of 12 was obtained, along with a retention efficiency of 100% and a recovery rate of 100%. A sampling frequency of 10 h-1 was achieved along with a precision of 3.0% RSD. Lysozyme of 0.4 g could be extracted from 100 mL egg-white. SDS-PAGE demonstrated that the purity of the obtained lysozyme was as high as that of pure reagent.
    Analysis of Geniposide and Total Nitrogen Content in Qingkailing Injection Intermediate by Near Infrared Spectroscopy and Synergy Interval Partial Least Squares
    ZHU Xiang-Rong1,2, LI Na2, SHI Xin-Yuan2, QIAO Yan-Jiang2, ZHANG Zhuo-Yong1*
    2008, 29(5):  906-911.  doi:
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    Near infrared spectrometry combined with chemometric methods was used for establishing a new method to determine the content of total nitrogen and geniposide in Qingkailing injections. The training and testing sets are partitioned by Kernard-Stone algorithm. Synergy interval partial least squares(siPLS) is used for selecting effective spectral regions and building the quantitative calibration models of the total nitrogen and geniposide. Pre-treatments of spectra are discussed in detail. Correlation coefficient obtained is 0.999, RMSECV is 0.023, RMSEP is 0.074 for the total nitrogen, and correlation coefficient is 0.708, RMSECV is 0.023, RMSEP is 0.159 for geniposide, respectively. The predictive results show that the proposed method is rapid, non-destructive and credible, which can be applied to control the quality of Chinese medicine injection online in industry scenes extensively.
    Metathetical Reaction of Organic Uranyl Species with Water in the Gas Phase
    HU Bin1, CHEN Lan-Hui3, HUAN Yan-Fu2, ZHANG Xie1, LI Ming2, LIANG Hua-Zheng1, CHEN Huan-Wen1,2*
    2008, 29(5):  912-915.  doi:
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    Negatively charged organic uranyl species(CH3UO2OH) was prepared and characterized with electrospray ionization tandem mass spectrometry implemented on an LTQ-MS instrument. Experimentally, it was found that ionic species of CH3UO2OH underwent metathetical reaction with water molecules present in the ion trap to produce negative ions of m/z 304 and a neutral methane species in the gas phase. The transient state of the reaction was observed and identified in the gas phase by tandem mass spectrometry. The mechanism was discussed in detail. The Gibbs free energy(ΔrG), enthalpy(ΔrH) and entropy(ΔrS) for the reaction were calculated, on the basis of the experimental measurements, to be -473.0 kJ/mol, -236.5 kJ/mol and 0.792 kJ·mol-1·K-1, respectively. The reaction rate constant was experimentally estimated to be 2.26 s-1.
    Synthesis and Fluorescence Properties of 3-Pyridin-3-yl-indolizines
    SHEN Zhu-Ying1, WANG Bing-Xiang1*, SHEN Jian1,2, HU Hong-Wen1
    2008, 29(5):  916-918.  doi:
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    A one-pot procedure was developed to prepare 3-pyridin-3-yl-indolizines(2a—2c) by a 1,3-dipolar cycloaddition reaction of pyridinium N-ylides to electron-deficient alkenes in the presence of tetrakispyridine cobalt(Ⅱ) dichromate(TPCD). The absorption and fluorescence spectra of compounds 2a—2c in ethanol were measured, and their fluorescence quantum yields were determined. The analysis result of the absorption and fluorescence spectra in different solvents indicates that 3-pyridin-3-yl substituent in indolizine ring apparently affects the fluorescence properties.
    Syntheses of Two Kinds of Tosylamine Compounds and Their Fluorescence Switch Character for the Oxidation-reduction of Fe3+
    YANG Yun-Xu*, DENG Xiao-Rong, JI Xing-Yue, QIN Li-Juan, SUN Zhen
    2008, 29(5):  919-922.  doi:
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    Two kinds of Tosylamine compounds(I, II) were synthesized and their fluorescence abilities were studied. Through the study of their recognition with Cu2+, Zn2+, Pb2+, Mg2+, Cd2+, Mn2+, Ca2+, Hg2+, Fe2+, Fe3+, Ni2+, Co2+ cations, it was found that both of the two kinds of compounds had recognition to Fe3+ in EtOH/H2O system through a series of iron-reorganization study. The fluorescence was changed by the addition of Fe3+, in which the fluorescence intensity of compounds I, II at 338 nm or 339 nm decreased. Under the co-existence of NH2OH·HCl and H2O2, both of the two compounds showed up that there could be a fluorescence switch by oxidation-reduction of Fe3+.
    Tumor Targeted Gene Vector Modified with G250 Monoclonal Antibody for Gene Therapy
    HAN Su-Fang1, DUAN Ya-Jun1, WANG Yan-Ming1, ZHENG Jun-Nian2, WU Yi2, CAI Rong1, OU Lai-Liang1, KONG De-Ling1*, YU Yao-Ting1
    2008, 29(5):  923-926.  doi:
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    The present study developed a tumor targeted gene vector by modification of PEI with G250 monoclonal antibody. G250mAb can specially combine with the G250 which is a tumor associated with antigen expressed highly in Hela cells. G250mAb was prepared from the ascites of Balb/c mice, and conjugated to PEI via disulfide bonds and generated G250mAb-PEI conjugate.G250mAb-PEI can condense plasmid DNA and form G250mAb-PEI/DNA complex, which can protect DNA from DNaseI digestion. Targeting effect and transfection efficiency of G250mAb-PEI was evaluated via co-culture technology. The results demonstrate that G250mAb-PEI can specially target the Hela cells. The transfection efficiency to Hela is two folds of HepG2 which was G250 negative. The tumor targeting effect was also demonstrated in transfection of smooth muscle cells(SMC). The transfection efficiency of SMC is almost 20 folds lower than that of Hela cells. In addition, the cytotoxicity of G250mAb-PEI which was determined by MTT assay on NIH 3T3 cells was much lower than PEI. In summary, G250mAb-PEI is a highly efficient gene vector with a low cytotoxicity and targeting effect. More work need to be done to evaluate the potential of the vector in vivo gene therapy.
    Synthesis of New Immobilized Chiral Salen Mn(Ⅲ) Complex as Effective Catalyst for Asymmetric Epoxidation of Styrene
    BAO He-Bin1,2, FU Xiang-Kai1,2,3*, BAI Ruo-Fei1,2, REN Wen-Shan1,2, TU Xiao-Bo1,2
    2008, 29(5):  927-931.  doi:
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    Chiral salen complexes are among the most important catalyts for asymmetric synthesis. But the soluble salen manganese complex are more difficult to be separated and to handle than the technically well established heterogeneous catalysts. An important strategy to combine the best property of the two types is the heterogenization or immobilization of active salen complex on supports or carriers, which may be seperated by filtration or precipitation. In this paper, a new way of the covalent immobilization of Salen Mn(Ⅲ) complex on a organic-innoganic mataterial to produce a stable heterogeneous catalyst for epoxidation are reported. Chiral Mn(Salen) complex was axially immobilized onto sulfomethylated zirconium oligostyrenyl phosphonate-phosphate(ZSMSPP), then characterized by FTIR, diffusion reflection UV-Vis, AAS, SEM, TEM, TG and N2 volumetric adsorption. The effects of reaction parameters such as oxidant, temperature, time and catalyst amount in the epoxidation of styrene are discussed, the result shows that this heterogeneous catalyst exihibits effective catalytic activity, and this heterogeneous Salen Mn(Ⅲ) catalyst is relatively stable and can be recyled for six times in the asymmetric epoxidation of styrene.
    Synthesis and Spectral Properties of New Water-soluble Fluorescent Label Squarylium Indocyanine Dyes
    SONG Bo1,2, ZHANG Qian2, PENG Xiao-Jun1*, MA Wen-Hui1,2, WANG Bing-Shuai1, FU Xin-Mei1
    2008, 29(5):  932-935.  doi:
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    Six water-soluble squarylium indocyanine dyes were synthesized and their structures were confirmed by 1H NMR and MS spectroscopy. The absorption and emission spectra of these dyes in water, methanol, ethanol, DMF, DMSO were studied. The spectra of these dyes exhibit a negative solvatochromism. The photo stability of these dyes in water was investigated as well. It is demonstrated that the electron-withdrawing group on N-position of cyanine dyes improves the photo stability as compared with the dyes with electron-donating group which decreases the photo stability obviously.
    Isolation and Purification and Structural Characterization of Acidic Polysaccharide FCP5-A from Fruit of Cornus officinalis
    YANG Li-Yan1, HUANG Lin-Juan1, WANG Zhong-Fu1*, CAO Chun-Yang2, SUN Wen-Ji1
    2008, 29(5):  936-940.  doi:
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    Fruit of Cornus officinalis has been used in Chinese traditional medicine for over two thousand of years. Polysaccharides, as important components of Cornus officinalis, have attracted much attention. An acidic polysaccharide FCP5-A was isolated from fruit of Cornus officinalis with water extraction and column chromatography. HPGPC shows that it was homogeneous polysaccharide with an average molecular weigh of 8.7×104. Monosaccharide analysis by GC shows that it was composed of rhamnose, arabinose, galactose and galacturonic acid with a molar ratio of 1∶ 5.7∶ 0.6∶ 1.2. By means of IR, GC, partial hydrolysis with acid, uronic acid reduction, methylation, GC-MS and 13C NMR analysis, the results indicate that FCP5-A was a branched polysaccharide rich in arabinose. The backbone was composed of 1,2-linked Rha and 1,4-linked GalA, with side chains attached to O-4 of the rhamnosyl residues. The side chains contained highly branched arabinan and short linear 1,3-linked galactan. It was concluded that FCP5-A was a new acidic branched polysaccharide of Cornus officinalis.
    Separatian and Identification of Constituents from Ligularia atroviolacea
    SHI Shu-Yun1,2*, ZHAO Yu2, ZHANG Yu-Ping1, HUANG Ke-Long1, LIU Su-Qin1
    2008, 29(5):  941-943.  doi:
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    A new and three known furanoeremophilanes were separated from Ligularia atroviolacea via chemical investigation, which were identified as 1α-chloro-6β-isobutyroxy-9-oxo-10β-hydroxy-furanoeremophilane(1), 1α-hydroxy-6β-isobutyroxy-9-oxo-10β-H-furanoeremophilane(2), 1α-hydroxy-6β-isobutyroxy-9-oxo-10α-H-furanoeremophilane(3), 1α,10β-dihydroxy-6β-angeloyloxy-9-oxo-furanoeremophilane(4). Their structures were established by spectroscopic methods including 2D-NMR. The absolute structure of compound 1 was determined by X-ray diffraction analysis.
    Differentiation of Live and Dead Cell of Bacterial Plant Pathogen in Polymerase Chain Reaction Assays Using a DNA Binding Dye
    FENG Jian-Jun1, Ji-yoen KIM1, LIU Xi-Li1, Norm W. Schaad2, LI Jian-Qiang1*
    2008, 29(5):  944-948.  doi:
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    Polymerase chain reaction(PCR) assays are quicker and often just as sensitive as agar plating assays for detecting plant pathogenic bacteria. However, PCR can be used to detects both live and dead cells. Since dead cells do not cause disease, their detection can be a problem in seed-health testing. Ethidium monoazide(EMA), a DNA binding dye, can prevent the amplification of DNA from dead cells of food-borne bacteria. To test the use of EMA for detecting live cells of Acidovorax avenae subsp. citrulli(Aac), seed extracts, spiked with Aac containing 3×106, 3×107, and 3×108 cfu/mL, were treated with EMA at 0, 1, 2, 3, and 4 mg/L and incubated at room temperature and at 75 ℃ for 3 min to kill Aac. After 10 min in the dark, the mixtures were put on ice under light for 5, 10, and 15 min to allow EMA to be effective, then assayed by classical PCR and agar plating. The results show that heat-treated suspensions containing dead cells of Aac at a level of 3×106 cfu/mL were PCR negative when pretreated with 2 mg/L or greater EMA and 10 min or more exposures. However, all treatments without EMA containing Aac at 3×106 cfu/mL or greater were ineffective as PCR results were positive. These preliminary results show that the addition of EMA to seed extracts containing moderate numbers of Aac has a potential for the specific detection of live cells.
    Studies on Adsorption Behavior of Benzene and Propylene in MCM-22 by Grand Canonical Monte Carlo Simulation
    SUN Xiao-Yan, LI Jian-Wei*, YU Hai-Qing, LI Ying-Xia, CHEN Biao-Hua
    2008, 29(5):  949-953.  doi:
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    The adsorption behavior of benzene and propylene in MCM-22 zeolite was studied by grand canonical Monte Carlo(GCMC) simulations. From the mass clouds of GCMC simulations, it can be found that the benzene and the propylene molecules show different adsorption behavior in the zeolite cavities. Both benzene and propylene molecules were mainly adsorbed in the 10-MR channels and the 12-MR supercages. But obviously, propylene has higher localization than that of benzene. Besides the two localizations, propylene can be steadily located in the short 10-MR windows interconnecting the 12-MR supercages, while the benzene can not do. From the potential energy distribution, it can be seen that both benzene and propylene have two-pinked and the potential energy of propylene is higher than that of benzene, so benzene can be adsorbed more steadily than propylene. When the temperature rises from 298 K to 443 K, the numbers of propylene reduce significantly, while benzene changes little. When benzene and propylene were adsorbed in zeolite at the same time, they have competitive adsorption, therefore the potential energy distribution is changed obviously. The adsorption isotherms of benzene and propylene at different temperatures and 1×10-3—5.0 kPa were simulated, the loadings of propylene are significantly lower than those of benzene.
    High Temperature Modification on Activated Carbons and Adsorption Kinetics of Perfluoroisobutene(PFIB) on Carbon Bed
    YE Ping-Wei1,2, LUAN Zhi-Qiang2*, ZHANG Jing-Chang1*, ZHANG Zhong-Liang2, LI Kai2, LI Yan2, MA Lan2, CAO Wei-Liang1
    2008, 29(5):  954-958.  doi:
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    The high temperature modifications(400—800 ℃) were carried out on granular activated carbons in the N2 flow and the adsorption behavior of PFIB on the carbon bed under various airflow humidity were studied. The breakthrough curves were processed through Wheeler equation and the dynamic model based on the linear equilibrium was used to correlate the experimental data. The results show that the pore structure didn’t change obviously and the surface oxygen amount decreased with the increase of modification temperature; the selective adsorption capacities to PFIB increased greatly and the carbon bed’s effective protection time to PFIB prolonged under high humidity of airflow. The theoretical breakthrough curves are in agreement with the experimental data very well, and this dynamic model can be used to predict the breakthrough behavior and to design and select the parameters of the cartridge canister.
    Surface-Enhanced Raman Scatting Substrates Fabricated by Combining Chemical Assembly and Electrodeposition Methods
    GAO Min-Xia, LIN Xiu-Mei, REN Bin*
    2008, 29(5):  959-962.  doi:
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    We reported a method to prepare SERS substrates with a high and uniform SERS activity by combining chemical assembly and electrochemical deposition methods. We systematically investigated the effect of the electrode potential on the surface morphology of the Au nanoparticles on the ITO surface. It is found that Au nanoparticles with very uniform structure and proper electromagnetic coupling can be obtained by electrodeposition at -0.04 V(vs. SCE) for 5 min. In situ electrochemical UV-Vis absorption spectroscopy was used to monitor the deposition process by measuring the absorption spectra. A new peak between 600 and 700 nm was observed in the UV spectra during the electrochemical deposition process, which can be used as a measurement of whether and how the electromagnetic field of nanoparticles couples. SERS mapping was performed to demonstrate that the substrate was very uniform with a signal deviation less than 20%, meeting the standard for commercial SERS substrates.
    Volumetric Properties of the Interaction of Arabinose with HCl Aqueous Solution at Different Temperatures
    ZHUO Ke-Lei1*, LIU Yao-Hui1, ZHANG Qiu-Fen2, LIU Hong-Xun1, WANG Jian-Ji1
    2008, 29(5):  963-968.  doi:
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    The interactions of electrolytes with saccharides are very important not only in exploring the stability of polysaccharides in biological systems but also in the chemical industry of saccharides and in the treatment of waste water containing saccharides. In this work, the density data were measured for arabinose+HCl+water at 10 K intervals from 278.15 to 318.15 K. The apparent molar volumes(VΦ,A) and standard apparent molar volumes(VΦ,A0) for arabinose in hydrochloric acids(0.2—2.1087 mol/kg) were calculated. Volumetric interaction parameters of arabinose with HCl in water were also evaluated. The apparent molar volumes and standard apparent molar volumes for arabinose in aqueous HCl solutions increase lineally with increasing molality of HCl. At a given temperature, the standard transfer apparent molar volumes(ΔtVΦ,A0) of arabinose from water to aqueous HCl solutions are positive and increase with increasing molality of HCl. In the temperature range studied, the relationship between(VΦ,A0) for arabinose and temperature is as follows: VΦ,A0=b0+b1(T-273.15)0.84. Pair volumetric interaction parameters of arabinose with HCl in water(VEN)are more than zero and vary slightly with the change of temperatures.
    Wettability of the Superhydrophobic Surface Under Condensation State Condition
    CHEN Xiao-Ling1*, LÜ Tian1, CHEN Xiang2
    2008, 29(5):  969-972.  doi:
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    The wettability of superhydrophobic surface has become the hot point in many fields. The wettability of the superhydrophobic surface under condensation state condition is studied by measurement of the contact angle and observation of polarizing light microscopy. It is found that the water vapor could condense in the small gap of the rough surface and the superhydrophobicity of the rough surface is destroyed. And the wettability of the superhydrophobic surface showed the heterogeneity, even some part became hydrophilic. According to the analysis, a calculation model is proposed for the condensing droplets on superhydrophobic surface and it was validated by the measurements of contact angle.
    Studies on Graphite Anode During Electrochemical Scan Cycles by EIS, Raman Spectroscopy and XRD
    ZHUANG Quan-Chao1,2, XU Jin-Mei1, TIAN Jing-Hua1, FAN Xiao-Yong1, DONG Quan-Feng1, SUN Shi-Gang1*
    2008, 29(5):  973-976.  doi:
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    The graphite anode during electrochemical scan cycles in 1 mol/L LiPF6-EC-DEC-DMC electrolyte solutions was investigated by EIS, Raman spectroscopy and XRD. It was found that the resistance of the SEI film increases almost linearly during the prolonged cycling in the 4—10 electrochemical scan cycles. However, the interface resistance between the graphite anode and the electrolyte solution decreases due to the decrease of the charge transfer resistance. After the electrochemical scan cycles, the active material on the surface of graphite anode is exfoliated and pulverized, and become amorphous, while the bulk of the active material remains unchanged.
    Optimizing Strategies Research on the Later Stage of Protein Structure Model
    ZHANG Lu-Jia1, XU Tao1, YUAN Pei-Qing2, WEI Dong-Zhi1*
    2008, 29(5):  977-980.  doi:
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    Homology modeling is the most widely used and fully developed method for protein structure prediction. Researchers of this field paid great attention to either improvement of modeling method or update of modeling algorithm in the past while ignoring the fact that different structure optimizing methods could contribute to the accuracy of the final structure as well. Lip8 was chosen as an example to find out the influences of different optimizing methods. After a initial Lip8 model was built by the method of homology modeling, four ways were applied to optimize the model based on two different strategies called “grade unpacking” and “fitting together”. Each of these ways was considered under two different conditions: with periodic bounded cubic(PBC) water surrounded or without, which resulted in 8 optimized structures all together. Procheck, Errat, Profile 3D and Ramachandran plot were used to evaluate each final model. From the results, we found that “grade unpacking” strategy combining with molecular dynamics optimization under explicit water could get a better model.
    Specific Heat Capacity, Thermodynamic Properties, Adiabatic Time-to-Explosion and Thermal Sensitivity Probability Density Distribution of 3,4-dinitrofurazanfuroxan(DNTF)
    GAO Hong-Xu1, ZHAO Feng-Qi1*, HU Rong-Zu1, XU Kang-Zhen2, ZHANG Hai3, WANG Peng4, DU Zhi-Ming4, XU Si-Yu1, YI Jian-Hua1, MA Hai-Xia2, CHANG Chun-Ran2, SONG Ji-Rong2,5
    2008, 29(5):  981-986.  doi:
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    3,4-Dinitrofurazanfuroxan(DNTF) is a novel energy density material and possesses a high energy, low melting point, good thermal stability and moderate sensitivity. It can be used in solid rocket propellant, warhead and explosive net with a broad prospect of applications. The specific heat capacity of DNTF was determined with the continuous cp mode of mircocalorimeter (Micro-DSCⅢ). The equation of cp to temperature is cp＝0.31064＋2.109×10-3T (285 K<T<345 K). The standard mole specific heat capacity of DNTF was 293.10 J/(mol·K) at 298.15 K. Furthermore, specific heat capacity of DNTF were calculated by DFT-RB3LYP/6-31+G(d) method in Gaussian 98W package and using the above determination result of specific heat capacity. The thermodynamic functions of DNTF, relative to the standard temperature 298.15 K, were calculated through thermodynamic relationship and the adiabatic time-to-explosion(tTIad) was also obtained. The tTIad of DNTF is 103.7 s. The thermal sensitivity probability density distribution function of energetic materials was deducted and thermal sensitivity probability density distribution curve of DNTF was constructed.
    Adsorption Property of Lignin and Naphthalene Dispersants on Coal-water Interface
    ZHOU Ming-Song1,2, QIU Xue-Qing1,2*, YANG Dong-Jie1,2
    2008, 29(5):  987-992.  doi:
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    The adsorption amount and kinetics of two lignin series dispersants(SL and MSSL) and one naphthalene dispersant(FDN) on Datong coal surface were studied, the results show that the adsorbed amounts of SL and MSSL on coal surface were far more than that of FDN. However, the fitted parameters of Langmuir equilibrium constant K and adsorption rate constant ka of SL and MSSL were less than that of FDN, which indicat that the adsorption ability of SL and MSSL on coal surface was inferior to that of FDN, and the adsorption rate of SL and MSSL on coal surface was lower than that of FDN. The adsorption layer of dispersant on coal surface was studied by using IR and XPS methods, and the results show that the coal with adsorbed SL and MSSL have evident “red shift” phenomenon. Moreover, the adsorbed layer thickness of SL and MSSL on coal surface was 7.22 and 4.61 nm respectively, however, that of FDN was thinner, only 2.11 nm. It is generalized that the hydrogen bond is the main adsorption force of SL and MSSL on coal surface, the adsorbed amount is rather large, the adsorbed layer is rather thick, and the multi-point adsorption on coal surface is the main form. The main form of FDN adsorbed on coal surface is horizontal adsorption by π-electron polarized adsorption, and the adsorbed strength is rather large, but the adsorbed layer is rather thin.
    Effect of Surfactants on Structure and Performance of Cu-Zn-Al Catalyst Prepared by Complete Liquid-phase Technology
    FAN Jin-Chuan, WU Hui, HUANG Wei*, XIE Ke-Chang
    2008, 29(5):  993-999.  doi:
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    A series of Cu-Zn-Al bifunctional slurry catalysts were prepared via the complete liquid-phase technology with different surfactants as the modifiers. The catalysts were characterized with N2 adsorption, XRD and XPS, and the catalytic activity of the catalysts for direct synthesis of DME from syngas was evaluated in a slurry reactor. The effect of different kinds of surfactants on catalyst structure and performance was investigated. The results show that the surfactants can adjust specific surface area, pore structure, phase structure and crystalline size of the catalysts by acting with active metal mainly, thereby affect the catalytic activity of the catalysts. Nonionic surfactant can promote catalytic performance of the catalyst, cationic and anionic surfactants are unfavorable for the catalyst. The intensity of the function between surfactant and active metal is the key that has influence catalytic performance.
    Influence of Potential Jump ψ Across Loose Region of Double Electric Layer upon Electro-chemical Oscillation in Pt-Electrode B-Z Reaction System
    LI Zhi, LIN Feng, HAN Yu-Min, LUO Jiu-Li*
    2008, 29(5):  1000-1004.  doi:
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    On the basis of a perfect analysis of the dissipations in the successive steps of a steady Pt- electrode B-Z reaction processes, the hesitation of electro-chemical step comparing with the diffusion step was expressed quantitatively by their contributions to the dissipation of electrode chemical reaction system. A theory of non-equilibrium thermodynamics of the potential jump ψ across the loose region of double electric layer was established. Consequently, an explicit formula for the calculation of ψ was given under the approximation of Boltzmann distribution. Meanwhile, a generalized dynamical model for Pt electrode B-Z reaction was suggested, by means of which the influence of ψ on the evolutionary dynamic behavior is further discussed in this paper. It turns out that the existence of ψ will further increase the non-linearity of dynamical mechanism of this electrode chemical reaction system. As one of the important results, it will degenerate the electro-chemical oscillation region. The corresponding degeneration of phase region favorable to the electro-chemical oscillation was plotted explicitly on the plane of externally controlled parameter-intrinsic parameter, simultaneously together with a computer simulation.
    Theoretical Study of the Diels-Alder Reactions of Lewis Base-Stabilized Borabenzenes with Dienophiles
    WANG Yan1,2, FANG De-Cai1*, LIU Ruo-Zhuang1
    2008, 29(5):  1005-1010.  doi:
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    Density functional theory(DFT) calculations at the B3LYP/6-31G(d) level of theory were employed to study the mechanism and the potential energy surface of Diels-Alder reactions between Lewis base stabilized borabenzene and dienophiles. The solvent effect and substituent effect were also considered. The results indicate that some of the reactions take place in a simple concerted way, while other reactions will form an intermolecular complex first and then proceed through a concerted transition state to obtain final products. The studies on the solvent and substituent effects reveal that the CH2Cl2 solvent will elevate the activation barriers, while CO2Me or CN groups on C atom of acetylene or ethylene may lower the activation barriers considerably. The Diels-Alder reactions forming one C—B bond and one C—C bond are always more favorable than the corresponding Diels-Alder reactions forming two C—C bonds, both thermodynamically and kinetically, which is in agreement with experimental observation.
    Theoretical Studies on the Electronic Structure and Spectra Properties of 1,1-Dimethyl-2,5-diaryl-3,4-diphenylsilole
    CHANG Qing1, WU Shui-Xing1, KAN Yu-He2, YANG Shuang-Yang1, TENG Yun-Lei1, YANG Guo-Chun1, SU Zhong-Min1*
    2008, 29(5):  1011-1015.  doi:
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    The ground states and low-lying excited states of the four silole derivatives are fully optimized with the density functional theory-B3LYP and configuration interaction singles(CIS). On the basis of the geometries, we computed the ionization potentials(PI), electron affinities(EA), reorganization energies, and other energies. And we obtained the absorption and emission spectra with time-dependent density functional theory(TD-DFT) calculation on the ground states and excited states, respectively. The results for the four derivatives are studied in comparison to each other. Then we analyzed the varieties of the energies and the spectra, and explain that pyspy can act as electron injection material, and assign that the hole transfer material can be achieved based on prspr, finally point out that thsth and fusfu can act as emitting materials in bulk state.
    Theoretical Study on the Supramolecular System of β-CD-Styrene Oxide and β-CD-Protonated Styrene Oxide
    YANG Zuo-Yin, DING Zhi-Xin, ZHANG Jing-Chang, CAO Wei-Liang*
    2008, 29(5):  1016-1020.  doi:
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    The molecular dynamic simulation and quantum chemistry methods were employed to study the supramolecular systems of β-CD-styrene oxide and β-CD-protonated styrene oxide. The results show that, when the phenyl group of protonated styrene oxide points to the secondary rim of β-CD, the system is inclined to be more stable and its attractive energy is relatively larger. But the case for styrene oxide is in disagreement with the protonated partner. However, in the view of kinetics, the phenyl group of styrene oxide maybe finally point to the secondary rim of β-CD due to its comparatively less repulsive energy in the complex. The property of electron density analyzed by topological study indicates that hydrogen bond was formed between the host and guest molecules when the phenyl group of guest molecules points to the secondary rim of β-CD. As a result, it is suggested that the orientation effect on styrene oxide in the inner phase of β-CD might mostly be attributed to the interactions between the host and guest molecules, such as H-bond, dipole action, etc..
    Studies on the Property Opetimization of Poly(ether-anhydride) Gels and the Application for Delivery of Hydrophobic Drugs
    YANG Ji1,2, CAI Zheng1, XIAN Dan1, WANG Zheng1*
    2008, 29(5):  1021-1026.  doi:
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    On the basis of the preparation of poly(ether-anhydride) gels, two synthesized photocrosslinkable hydrophobic monomers were added respectively to copolymerize with poly(ether-anhydride) macromers under UV irradiation to form crosslinked gel networks. Accordingly, swelling capacity and hydrophilicity/hydrophobicity of gels were modified and the compatibility between hydrophobic drugs and gels was regulated. The hydrophobic drug indomathecin was post-loaded in the gel networks as a model drug, which was proved to be distributed in an amorphous or molecular state by employing X-ray diffraction. It was tested that the drug loading and encapsulation efficacy in the modified gels were increased, and the dissolution rate from the gels was effectively improved. Compared to the pure poly(ether-anhydride) gels, in vitro drug release behavior from the modified gels was delayed and more suitable for clinical application.
    Loading and Release of Lysozyme by Casein-g-dextran Graft Copolymer
    YU Shao-Yong, GAO Gao, YAO Ping*, JIANG Ming
    2008, 29(5):  1027-1032.  doi:
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    Proteins are natural amphoteric polyelectrolyte. We studied the encapsulation and release of lysozyme as a model protein-drug using natural biomacromolecules. We prepared non-toxic β-casein-g-dextran copolymer through Maillard reaction and fabricated β-casein-g-dextran/lysozyme micelles through electrostatic attractive force between β-casein and lysozyme. The micelles with β-casein/lysozyme core and dextran shell are stable against dilution. The micelles dissociate in acidic, alkaline or salt solution where the electrostatic attraction disappears. The lysozyme released from the micelles shows the same activity as the nature lysozyme. Addition of Ca2+ ion can improve the stability of the micelles in acidic solution but cannot do so in alkaline or salt solution. Replacing β-casein-g-dextran with more hydrophobic casein-g-dextran and crosslinking the micelles with Ca2+ ion lead to the resultant micelles much more stable in acidic solution; the stability in alkaline or salt solution can also be improved.
    Synthesis and Characterization of Liquid Crystalline Poly(p-phenylene ethynylene)s with Laterally Attached Dipolar Unit
    ZHENG Shi-Jun1*, HUANG Yuan-Can1, WEN Gang1, LUO Fei1, LI Shao-Feng1, CAO Shao-Kui1, CHEN Si2
    2008, 29(5):  1033-1037.  doi:
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    Poly(p-phenylene ethynylene)s containing laterally attached dipolar unit were synthesized with Sonogashira coupling reaction using different Pd catalysts in order to develop new organic materials with polarized dichroism. The structures and properties of the intermediate were identified via elementary analysis, IR, NMR etc. The polymers were soluble in common organic solvents and exhibited enantiotropic liquid crystal behavior. It is found that the polymers prepared with different Pd catalysts have similar molecular weights and mesophase temperature. The kind of catalysts has a large effect on the structures of the polymer main chain and polymers textures. The study of thermal WAXD suggests that the polymers formed a Nematic phase.
    Fluorescence Spectrum Study of Sol-gel Transition in Alginate Aqueous Solutions Induced by Calcium Cations
    LU Lu1, LIU Xin-Xing2, TONG Zhen2*
    2008, 29(5):  1038-1040.  doi:
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    In order to establish an experiment method to determine the gelation point for the physical gelation without disturbing the system mechanically, the fluorescence spectrum was used to monitor the sol-gel transition in the aqueous solutions of FITC labeled alginate induced by Ca2+. The slope change was found from the curves of the emission strength and fluorescence anisotropy against gelation time, indicating the gelation time of 80 min, which just equaled that determined by rheology measurement. The label fluorescence strength and anisotropy can be used to determine the gel point for the physical gelation.
    Mechanism and Electric Field Properties of the Dual Electrode Mode Electrospining
    LI Mei*, LI Zhi-Qiang*, LI Zhen
    2008, 29(5):  1041-1045.  doi:
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    A novel, high speed electrospinning process, dual electrode mode electrospinning was developed. With coexistence of both positively and negatively charged nozzles, the electrospun fibers interact between nozzles, interconnect with each other, and are stretched on a movable collecting roll. By electrospinning the biodegradable polymer via the dual electrode mode process, a highly intertwined, mathematics mode was obtained. Moreover, the productivity was increased more than 10 times in comparison to that by using the conventional single electrode mode process, which is essential for commercialization of the electrospinning process.
    Fabrication of Ag/Polypyrrole (PPy) Coaxial Nanocables Through Ions Adsorption Method
    XIE Hu-Xiao, QIU Teng, LI Xiao-Yu*
    2008, 29(5):  1046-1049.  doi:
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    A new method for the fabrication of Ag/PPy coaxial nanocables based on the ion adsorption on the nanowires' surface was developed. The Ag nanowires(NWs) with uniform diameters of about 40—50 nm were obtained through polyol reduction with poly(vinylpyrrolidone) (PVP) as the capping agent. The Ag-NW was dispersed in the Cu(Ac)2 aqueous solution for the adsorption of Cu2+ on the surface of the Ag-NWs. The Cu2+ on the Ag-NW surface was then served as the active central to oxidize pyrrole monomer to PPy on the surface of Ag-NWs. The structures of the coaxial nanocables' of the final products were characterized by TEM, FTIR, Raman spectrum and XPS to study the composite of the finial product and the chemical environment of Cu+.
    Molecular Network Structure and Gaussian Modulus of Plasticized Poly(vinyl chloride) Material
    LÜ Rui-Hua, ZHOU Chang-Lin, LEI Jing-Xin*, LI Qi-Man
    2008, 29(5):  1050-1055.  doi:
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    The influences of the content of plasticizer, filler(CaCO3, carbon black) and n-butyl nitrile rubber(NBR) on the network structure, molecular slippage and Gaussian modulus of plasticized poly(vinyl chloride)(PPVC) were studied by employing stress relaxation experiment and Haward model. The network structure of PPVC comprises the main network formed by macromolecule entanglement and the secondary network formed by interaction forces between molecule(van der Waals force). The viscoelastic behavior of PPVC materials is in accordance with Haward model before their main networks extend to the critical value. Although plasticizer, CaCO3, carbon black do not change the entanglement structure of PPVC, plasticizer can decrease Gaussian modulus and increase the molecular slippage by decreasing the density of main network and weakening the secondary network. However, CaCO3 and carbon black can increase Gaussian modulus and decrease the molecular slippage by increasing the density of main network and strengthening the secondary network. NBR not only decreases the entanglement density of macromolecular chain but also weakens the secondary network, which results in the reduction of Gaussian modulus of PPVC material.
    Influence of Polymer Chain Orientation on Interfacial Tension Measurement with DDRM Simulated by Dissipative Particle Dynamics
    MAO Wei, KONG Bin, YANG Xiao-Zhen*
    2008, 29(5):  1056-1060.  doi:
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    When the deformed drop retraction method(DDRM) is used to measure interfacial tension, the elastic relaxation of polymer chain should be faster than the ellipsoidal droplet retraction. We investigated the influence of polymer chain orientation during the retraction processes using DPD method. The result indicates that the influence of orientation is related to the direction of chain orientation. If the direction of chain orientation is parallel to the fluid direction, the measurement of the interfacial tension clearly deviates from the standard, but if it is perpendicular to the fluid direction, the measurement has nearly no deviation.
    Preparation of Thermoresponsive Chitosan Copolymer and Its Cytocompatibility and Detachability
    CHEN Li1*, LI Shi-Geng1, XIAO Fei1, ZHANG Ai-Hua2, YAO Kang-De2
    2008, 29(5):  1061-1064.  doi:
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    In this study, Chitosan(CS) based macromer was used to modify NIPAAm to make a novel temperature-responsive film for cell adhesion and detachment. CS was coupled with acrylic acid(AAc) to prepare a macromer(CS-AAc). Then, it was copolymerized with N-isopropylacrylamide(NIPAAm) to synthesize a P(CS-AAc-NIPAAm) film. The novel copolymer obtained was characterized via FTIR and XPS. There was thermo-response for the film against water, and this phenomenon was coincided with the data of dynamic contact angle against water. Moreover, the cytocompatibility of the film was investigated with fibroblast culture in vitro. The result reveal that the film exhibited a good cytocompatibility, when the temperature declined, it had the cell detachability.
    Chitosan-based Self-assembled Nanomicelles as a Novel Carrier for Paclitaxel
    WANG Yin-Song1*, WANG Yu-Mei1, LI Rong-Shan1, ZHAO Jing1, ZHANG Qi-Qing2,3
    2008, 29(5):  1065-1069.  doi:
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    Self-assembled nanomicelles of N-cholesterol succinyl O-carboxymethyl chitosan(CCMC) were prepared by probe sonication method. The amphiphilic property and the critical micelle concentration(cmc) of CCMC were determined by fluorescence probe technique; the morphology and the size of CCMC self-assembled nanomicelles were analyzed by transmission electron microscopy(TEM) and the dynamic laser light scattering(LLS). Paclitaxel(PTX), being used as model drug, was entrapped into CCMC self-assembled nanomicelles by dialysis method. The drug loading and release properties were estimated by high performance liquid chromatography(HPLC). The results show that CCMC was an amphiphilic polymer and formed regularly spherical nanomicelles(mean diameter=198.4 nm) in aqueous medium by self-assembly, and the cmc value of CCMC was 0.018 mg/mL. PTX-loading CCMC self-assembled nanomicelles were successfully prepared, with drug loading content as high as 34.9%, and their mean diameter increased with increasing the drug loading content. PTX continuously released from CCMC self-assembled nanomicelles in the release media of phosphate buffered saline(PBS) solutions, and its release was sensitive to the pH of the release media.
    Growing Behavior of Endothelial Cells on Electrospun Aligned Nanofibrous Film of Polyurethane
    HAN Zhao-Zhao1, KONG Hua1, MENG Jie2, WANG Chao-Ying3, ZHU Guang-Jin1, XIE Si-Shen3, XU Hai-Yan1*
    2008, 29(5):  1070-1073.  doi:
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    The nanofibrous film of polyurethane(PU) with aligned topography was fabricated by electrospinning for human umbilical vein endothelial cells(HUVEC) growth. The morphology of nanofibrous film was observed and characterized by scanning electron microscopy(SEM). The cells growth behavior including proli-feration, cytoskeleton formation of actin, tublin and vinculin, and tissue factor(TF) release was investigated via cell viability assay, confocal observation and TF assay. The average diameter of the generated fiber was around 300—500 nm. The experimental results indicate that the aligned nanofibrous film of PU exhibited promotional influence on the cell proliferation. It was also observed that the film possessed an advantage of supporting HUVEC migrating and aggregating along the axis of the aligned nanofibers, which is one of the important functions in the process of endothelium regeneration. It was also demonstrated that the endothelial cells growing on the film expressed non-thrombogenic phenotype with low tissue factor released. These results indicate the favorable interactions between ECs and the film, implying that the aligned nanofibrous film of PU has a promising potential for vascular engineering.
    研究快报
    Synthesis of Fluorinated Poly(arylene ether)s Bearing a Sulfonic Acid Group on a Pendant Group
    JING Li-Wei, LIU Bai-Jun*, GUAN Shao-Wei, JIANG Zhen-Hua
    2008, 29(5):  1074-1076.  doi:
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    Six highly fluorinated poly(arylene ether)s were prepared by using a nucleophilic polycondensation reaction and their sulfonation selectivity was investigated. Single site of each repeated unit on pendant phenyl group could be obtained via the postsulfonation approach under mild reaction conditions. Phenylated fluorinated poly(arylene ether)(Ph-FPAE) showed more excellent controllability over substituted sites and sulfonation degree when chlorosulfonic acid was used as sulfonation reagent. The resulting sulfonated Ph-FPAE(Ph-SFPAE) exhibited good thermal stability, solubility and hot-water dimensional stability, and also had a proton conductivity of 0.10 S/cm at 100 ℃. The results showed that Ph-SFPAE might be a candidate material for proton exchange membrane in fuel cell applications.
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