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    10 August 2007, Volume 28 Issue 8
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    高等学校化学学报2007年第28卷第8期目次
    2007, 28(8):  0.  doi:
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    下期目次预览
    2007, 28(8):  0.  doi:
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    研究论文
    Synthesis of TS-1 Nanocrystals on Silica Gel via Steam-assisted Dry Gel Conversion Method
    KE Xue-Bin1, XU Li1, ZENG Chang-Feng2, ZHANG Li-Xiong1*, XU Nan-Ping1
    2007, 28(8):  1411-1415.  doi:
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    TS-1 nanocrystals were synthesized on silica gel via dry gel conversion method, at first silica gel was impregnated with TS-1 synthesis solution and then followed by steam treatment at 130 ℃ for 2 d. The product was characterized with XRD, FTIR, UV-Vis, NMR, N2 adsorption, ICP, SEM and TEM. The results indicate that TS-1 crystals were grown on silica gel with a size of ca. 20 nm, a BET specific surface area of 113.2 m2/g and a mesopore size of 23.7 nm. The product exhibited a higher catalyst performance than TS-1 powders, which was prepared by conventionally hydrothermal synthesis, for benzene hydroxylation with n(benzene)/n(H2O2)=3 and sulfolane as the solvent at 100 ℃ for 2 h. The benzene conversion and TOF were 8.7% and 11.37, respectively, with more than 99% of phenol selectivity.
    Photoluminescence and Electroluminescence Properties of Samarium Complex Sm(DBM)3phen
    DENG Rui-Ping1,2, YU Jiang-Bo1, ZHANG Hong-Jie1*, LI Zhe-Feng1,2, ZHOU Liang1,2, PENG Ze-Ping1,2, GUO Zhi-Yong1,2
    2007, 28(8):  1416-1419.  doi:
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    Photoluminescence(PL) and electroluminescence(EL) properties of a samarium complex Sm(DBM)phen(DBM=dibenzoylmethane, phen=1,10-phenanthroline) were investigated. A series of devices based on Sm(DBM)phen were fabricated. The results show that Sm(DBM)phen owns good electron injecting and transporting properties. By optimizing the device structure, bright efficient orange EL devices could be achieved, and the maximum brightness and efficiency were 150 cd/m2 and 0.72 cd/A, respectively. The device showed the characteristic emission peaks of the Sm3+ ion at all operating voltages. It was noticed that the relative intensity of Sm3+ emission peaks differed from each other in PL and EL cases, which could be ascribed to the change of coordination sites of the Sm3+ ion during the evaporation of the samarium complex in the EL case.
    Effect of Mg2NiH4 on the Thermal Decomposition of Ammonium Perchlorate
    LIU Lei-Li1*, LI Feng-Sheng2, ZHI Chun-Lei2, TAN Ling-Hua2, YANG Yi2, ZHANG Qing-Si1
    2007, 28(8):  1420-1423.  doi:
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    Magnesium-based hydrogen storage material Mg2NiH4 was prepared with replacement-diffusion method and its structure was determined by XRD, ICP and DSC-TG. The thermal decomposition behavior of ammonium perchlorate(AP) was investigated in the presence of Mg2NiH4 by the method of DSC. The results show that Mg2NiH4 had obvious influence on the thermal decomposition of AP. Mg2NiH4 showed an evident catalytic effect on the lower temperature thermal decomposition of AP, and the higher thermal decomposition temperature of AP was decreased by Mg2NiH4, with a clear increase at DSC heat release. The catalytic effect of Mg2NiH4 on the thermal decomposition of AP was enhanced with the increase in content, and the DSC heat release was at its biggest value when the content of Mg2NiH4 was 30%(mass fraction). With the increase of hydrogen storage, the catalytic effect became stronger. The mechanism of catalyzing the thermal decomposition of AP is as follows: H2 released from Mg2NiH4 and Mg, Ni reacted with the decomposed product of AP.
    Synthesis and Properties of Novel Porphyrin

    HOU Jun1, ZHOU Zi-Yan1, WU Xue1*, ZHU Dong-Xia2, LI Peng2

    2007, 28(8):  1424-1427.  doi:
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    The preparation of a novel porphyrin derivative bearing oligo(p-phenylene) group and its zinc complex was reported, which involved a microwave irradiation and a synthesis based on the template effects, respectively. Both of the porphyrin derivative and its zinc complex were fully characterized through IR, NMR and MALDI-TOF-MS. Optical properties(UV-Vis and fluorescence) was also studied for both compounds according to the spectra analysis, respectively. For zinc complex the thermal stabilities and electrochemistry were studied by TGA and CV. Further fabrication with the zinc complex as a dopant resulted in an electroluminescent device emission at 556 nm.
    研究快报
    Preparation and Structure Characterization of Ordered Cubic Zr-doped Mesoporous Silica by EISA Method
    CHU Bin, WANG Run-Wei, SHEN Qi-Hui, CHEN Lu, WAN Li-Feng, ZHU Guang-Shan, QIU Shi-Lun*
    2007, 28(8):  1428-1430.  doi:
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    Highly ordered cubic Zr-doped mesoporous silica was directly prepared with Evaporation-Induced Self Assembly method(EISA) with triblock copolymers(Pluronic P123) as the structure-directing agents. The mesoporous material was characterized via small-angle powder X-ray diffraction(XRD), transmission electron microscopy(TEM), and nitrogen adsorption. The results show that the product has a face-centered cubic structure with space group of Fd3m. N2 sorption revealed that the Zr-doped mesoporous silica has not only ordered structures, but also high surface area(550 m2/g), large pore volume(0.66 cm3/g), as well as uniform pore size(4.0 nm).
    研究简报
    Syntheses, Crystal Structures and Decomposition Kinetics of Complexes of Zinc and Nickel with Amido-Schiff-base as the Ligand
    HAN Jing1, XING Yong-Heng1*, ZHANG Xing-Jing2, ZHOU Guang-Hua2, AN Yue2, GE Mao-Fa2
    2007, 28(8):  1431-1433.  doi:
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    Two new complexes, (C9H7NO3)Zn(C3H4N2)2(1) and (C9H7NO3)Ni(C3H4N2)2(C4H5N2O)•CH3OH•0.5H2O(2), with salicylideneglycinyl as the ligands, were synthesized successfully at room temperature in methanol solution, and characterized via elemental analyses, IR spectra, UV-Vis and fluorescence spectra, and X-ray diffraction and thermogravimetric analyses were also carried out.
    Hydrothermal Synthesis and Characterization of a New Supramolecular Compound [H3N(CH2)3NH3]•[Pb2(SIP)2]•6H2O
    MA Kui-Rong1,2, XU Jia-Ning1, WANG Li1, SHI Jing1, WANG Ying1, HA Jing1, NING De-Kuan1, FAN Yong1*, SONG Tian-You1*
    2007, 28(8):  1434-1436.  doi:
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    A new three-dimensional supramolecule, [H3N(CH2)3NH3]•[Pb2(SIP)2]•6H2O was synthesized under the hydrothermal condition. Its structure was determined with single crystal X-ray diffraction analysis and further characterized via XRD, IR, fluorescent spectrum and elemental analysis. The compound crystallizes in triclinic space group P1, with a=0.79946(16) nm, b=0.9881(2) nm, c=1.0343(2) nm, α=81.25(3)°, β=84.95(3)°, γ=68.13(3)°, V=0.7489(3) nm3, Z=1, R1=0.0226, wR2=0.0486, GOF=1.099. Along the [001] direction, binuclear cluster units [Pb2(SIP)2]2- link to each other via O1 and O4 forming two-dimensional anionic layers, then these layers are stacked down the c axis and was further linked by N—H…O and O—H…O hydrogen bonds to build the three-dimensional supramolecular structure. Fluorescent spectrum of compound 1 shows that there are two strong fluorescent emission peaks at λ=349 nm and 393 nm and a weak fluorescent emission peak at 384 nm(λmax, excitation=236 nm).
    Synthesis, Structure and Properties of a Novel Lanthanide Metal-organic Coordination Polymer with Three-dimensional Open Framework, Tm(BTC)(DMF)(DMSO)
    NA Li-Yan1,2, JIANG Hui-Ming2, YANG Bao-Ling2, HAI Hua2, NING Gui-Ling1*
    2007, 28(8):  1437-1439.  doi:
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    A three-dimensional(3D) lanthanide metal-organic coordination polymer with a three-dimensional open framework, Tm(BTC)(DMF)(DMSO), was synthesized by reaction of the lanthanide ions(Tm3+) with 1,3,5-benzenetricarboxylic acid(H3BTC) in a mixed solution of DMF(N,N'-dimethylformamide) and DMSO(dimethyl sulphoxide). This compound crystallizes in a monoclinic space group P21/n with unit cell parameters a=1.0801(2) nm, b=1.5550(3) nm, c=1.0906(2) nm, β=100.401°, V=1.8017(6) nm3 and Z=4. The compound exhibits one-dimensional channels along the [100] direction and could uptake carbon dioxide at 1×105 Pa.
    Effect of Mesoporous Silica Pore Structure on the Release Profiles of Captopril Drug
    QU Feng-Yu1*, CUI Ling-Fei1, HUANG Shi-Ying2, ZHU Guang-Shan2*
    2007, 28(8):  1440-1442.  doi:
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    A series of mesoporous silica with variable pore structures were prepared. The influence of mesoporous structure on drug release profiles was studied. It is found that mesoporous pore structure has a great effect on the drug release rate. The cubic pore structure MCM-48 has a faster drug release rate than that of MCM-41 system; while SBA-16 with “cage-like” pore structure system has the lowest drug release rate.
    研究论文
    Thermodynamic Studies on 4-Hydroxybenzoic Acid-imprinted Polymer Monolith by Frontal Analysis
    ZHENG Chao1, LIU Zhao-Sheng2, GAO Ru-Yu3*, ZHANG Yu-Kui4
    2007, 28(8):  1443-1448.  doi:
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    The adsorption isotherms of 4-hydroxybenzoic acid imprinted monolith which was prepared by in situ therm-initiated polymerization were determined with the frontal analysis successfully. Adsorption isotherms of the monolith were measured at 20, 40 and 50 ℃ by using acetonitrile, tetrahydrofuran, methanol and acetonitrile containing 1%, 3%, 5% and 7%(volumn fraction) acetic acid as the mobile phase, respectively. The results show that the adsorption capacity of the monolith for the template was found to be much stronger than 2-hydroxybenzoic acid. The experimental data was fitted by Bi-Langmuir isotherm, and the saturation capacity and association constant of imprinted monolith was achieved. The content of acetic acid in the mobile phase, the nature of the organic mobile phase and the temperature showed some influence on the adsorbent ability and selectivity of the imprinted polymer. This phenomenon can be explained that the saturation capacity and association constant of 4-hydroxybenzoic acid on the binding sites was influenced by the chromatographic conditions much more significantly than 2-hydroxybenzoic acid.
    Mechanism of Interaction Between Nano Gold Colloid and Monoclonal Antibody(McAb) of Aflatoxin B1
    SUN Xiu-Lan1,2* ZHANG Yin-Zhi1, SHAO Jing-Dong3, ZENG Jie4
    2007, 28(8):  1449-1453.  doi:
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    The optimal condition for AFB1 conjugating to nanogold particles was obtained by studying the preparation and the reaction. Optimum pH for conjugation was determined to be 7.4, reaction time was 5 min, and the least stable content of McAb to colloidal gold in five diameters(10.7—67.4 nm) was 0.07, 0.051, 0.033, 0.019, 0.012 mg/L gold solution, respectively. Combination of McAb with nanogold particles was also characterized with TEM, IR spectra and immunoreactivity. The results show that the titer of McAb increased obviously. Colloidal gold has a powerful ability to quench the McAb fluorescence via a nonradiative energy transfer mechanism. The fluorescence quenching data were analyzed according to Stern-Volmer equation. The binding constant of reaction was obtained. The data of enthalpy and entropy proved that the main interactions were London-van der Waals force and hydrogen bond between colloidal and McAb. From the synchronous spectrum colloidal gold has not obvious effect on the conformation of McAb. It was proposed that the small change of conformation of McAb was the reason of increase of titer, affinity and stability.
    Fabrication of Silver Nanoparticle Multilayer Films by Using DDAB Films as a Template and Their Application to Surface-enhanced Raman Scattering
    LI Yan-Cai1, ZHOU Ji2, SONG Yan-Tao1, SUN Chang-Qing1*
    2007, 28(8):  1454-1457.  doi:
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    Highly ordered silver nanoparticle multilayer films were achieved conveniently by using didodecyldimethylammonium bromide(DDAB) films as a template. The obtained thin films were characterized by UV-Vis spectroscopy, cyclic voltammerty(CV) and atomic force microscopy(AFM) in detail. The well-ordered superlattice structure of the DDAB template and the silver nanoparticle multilayer films were also identified by X-ray diffraction(XRD). The application of the as-prepared silver nanoparticle multilayer films in surface-enhanced Raman spectroscopy(SERS) was investigated by using 4-mercaptopyridine(4-MPY) as the probe molecules. It was found that the silver nanoparticle multilayer films exhibied a remarkable enhancement ability, and can be used as SERS substrates.
    Rapid and Sensitive Analysis of Genetically Modified Maize by Multiplex PCR and Capillary Electrophoresis with Laser-induced Fluorescence Detection
    ZHOU Ying, LI Yuan-Qian*, PEI Xiao-Fang
    2007, 28(8):  1458-1463.  doi:
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    A rapid method for detection of genetically modified maize by multiplex polymerase chain reaction(PCR) followed by capillary electrophoresis with laser-induced fluorescence was developed. The triplex PCR procedure was applied to simultaneously amplify CaMV 35S promoter and the junction between hsp70 intron 1 and CryIA(b) gene as well as Invertase gene. The amplified products were analyzed by capillary sieving electrophoresis with laser-induced fluorescence detection. The parameters of multiplex PCR and capillary sieving electrophoresis were optimized. Under the optimal conditions, the proposed method was able to simultaneously detect the three heterogenous genes existing in genetically modified maize. The amplified DNA fragments were sequenced and showed the good agreement with original gene, which indicated the reliability of the amplification reaction. The limit of detection was 0.05%, which is much lower than 1% threshold for labeling genetically modified food required by the European Community. There was a good agreement in the determined results of maize and its products by using this method and real-time quantitative PCR method. Compared with conventional agarose gel electrophoresis, the proposed method offered a more specific and sensitive procedure to rapid screening, identification and detection of genetically modified maize.
    Labeled Immunoassay of Dual-Analyte Utilizing Surface-Enhanced Raman Spectroscopy
    GE Ming, YAO Jian-Lin, CUI Yan, JIANG Yun, GU Ren-Ao*
    2007, 28(8):  1464-1468.  doi:
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    Au film which was used as immunoassay substrate was modified by 16-mercaptohexadecanoic acid(16-MHA) via self-assembled monolayer(SAM) technology. A sandwich assay which contains captured antibodies, antigens and labeled immuno-colloids was formed. Two different Raman reporter molecules(4,4'-bipyridine and thiophenol), which served as respective labels for each type of antibodies, were selected. SERS has the advantage of a small line width of Raman bands and high sensibility. The presence of dual-analyte was established by distinguishing the corresponding labeled reporter's Raman spectrum. By chosing suitable Raman reporter molecules and immuno-colloids of certain size, detection limit ranges from 1 to 100 fg/mL were achieved.
    Inducement and Degradation Function of P450 in Phanerochaete chrysosporium by in Situ Spectroscopic Analysis
    NING Da-Liang, WANG Hui*, ZHUANG Yuan, LI Dong
    2007, 28(8):  1469-1474.  doi:
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    The method of inducement-in situ spectra analysis was developed and used to directly detect and characterize microsome P450 and its inducement in Phanerochaete chrysosporium(PC) by n-hexane, benzoic acid, naphthalene and pentachlorophenol at molecular level. The results demonstrate that the content of P450 after inducement by n-hexane, benzoic acid, naphthalene reached a high level of 7.5, 5.6 and 3.1 times of that without inducement, respectively. The inducement of P450 in fungi by pentachlorophenol has not been reported before this study. The substrate binding spectra of benzoic acid with P450 from PC grown in both low nitrogen medium and PDB medium, and NADPH-dependent degradation of benzoic acid in PC microsome were detected, which provide a direct evidence of the function of P450 to catabolize benzoic acid. However, the inhibition was not observed during the degradation of benzoic acid by PC with P450 inhibitor aminobenzotriazole, which indicates that other catabolic pathway may also exist in PC.
    Simultaneous Adsorption of Organic Pollutant and Heavy Metal onto Surfactant-Modified Organobentonites with Chelating Ligands
    SUN Hong-Liang1,2*, ZHU Li-Zhong1
    2007, 28(8):  1475-1479.  doi:
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    The surfactant-modified organobentonites with chelating ligands, IMB-CTMA-Am, were synthesized, where IMB refers to natural bentonite obtained from Inner Mongolia of China, CTMAB refers to quaternary ammonium cation surfactant of cetyltrimethylammonium bromide, and Am refers to the chelating ligands, respectively. The adsorbent samples were characterized by X-ray diffraction(XRD), thermogravimetric and differential thermal(TG-DTA) analyses, specific surface area(N2-BET) measurements, and elemental analysis. The results indicated that CTMA+ and Am intercalated into the lamellae of bentonites successfully. The adsorption experiments showed that IMB-CTMA-Am could effectively adsorb organic pollutant p-nitrophenol(PNP) and heavy metal ion Pb2+ in waste water system simultaneously. The adsorption capabilities of IMB-CTMA-Am are greater than natural bentonite IMB and modified bentonite IMB-CTMA. Fourier transform infrared(FTIR) spectrum study revealed that the N—H vibrational frequency of IMB-CTMA-Am was downshifted after Pb2+ adsorption, which demonstrates the formation of a metal complex between metal ion Pb2+ and Am in the interlayers of the modified bentonites. The adsorption capacity of Pb2+ onto IMB-CTMA-Am agrees with the stability constant of the complex formed.
    研究简报
    Microwave-assisted Extraction of Rutin and Quercetin from Euonymus alatus(Thunb.) Sieb
    ZHANG Fan1, YANG Yi1*, GUO Zhen-Ku2
    2007, 28(8):  1480-1482.  doi:
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    A detail procedure for extracting rutin and quercetin from Euonymus alatus(Thunb.) Sieb was developed with an obturated microwave-assisted extraction(MAE) device with pressure and temperature controlling units. The effects of solvent concentration, ratio of solution to solid, radiation time and microwave power were discussed in orthogonal experiments. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction was a rapid method with a higher yield and less solvent consumption. The mechanism of the microwave-assisted extraction was studied by scanning electronic micrograph. In the case of microwave heating, the build-up pressure within the cells could exceed their capacity for expansion, and caused their rupture more rapidly than that in conventional extraction.
    Synthesis, Characterization and Biological Functionalization of Superparamagnetic/Fluorescent Bifunctional Nanoparticles
    TAN Fang1, ZHUANG Zhi-Xia1,2*, YANG Huang-Hao2, CHEN Cheng-Xiang1, WANG Xiao-Ru1,2
    2007, 28(8):  1483-1485.  doi:
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    A novel class of fluorescent/superparamagnetic bifunctional nanoparticles was synthesized via the reverse microemulsion technique. These nanoparticles were studied with transmission electron microscopy(TEM) and SQUID microscopy. The results show that these nanoparticles have a typical diameter of 40 nm and a saturated magnetic moment of 1.9 emu/g at room temperature. The experiment results also show that these nanoparticles exhibit a strong excitonic photoluminescence. Then, these bifunctional nanoparticles were modified with vancomycin for binding. The results show that these vancomycin modified nanoparticles can capture selectively bacterias.
    Application of HPLC-ESI-MS/MS to the Determination of a Novel Antitumour Platinum Complex
    SU Qiang1,2, LIU Qing-Fei2, LIANG Qiong-Lin3, WANG Yi-Ming2,3, BI Kai-Shun1, LIU Wei-Ping4, LUO Guo-An2,3*
    2007, 28(8):  1486-1488.  doi:
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    A novel platinum complex, named as saliplatin, was designed, synthesized and characterized with element analysis, coupled inductively plasma-mass spectrum, gravitational thermal-differential thermal analysis, ultraviolet-visible absorption spectrum, infrared spectrum, fast atom bombment mass spectrum and 1H NMR, etc. Its purity was investigated and determined. HPLC-ESI-MS was employed to separate the platinum complex and the impurity, and to identify and quantify the latter. It proved that the impurity in this novel compound was 3,5-diisopropylsalycilic acid, a reactant used in the synthesis of the novel platinum complex, identified with ESI-MS. The mass fraction was determined with HPLC as 4.3%, which meant that the purity of this new substance was 95.7%.
    研究论文
    Hydrosilylation of Terminal Alkynes Catalyzed by Pt(DVDS)-Phan Complex
    ZHANG Xiao-Yun, WU Wei*, XIE Zhao-Jun, XIA Dao-Hong
    2007, 28(8):  1489-1492.  doi:
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    The catalyst system Pt(DVDS)-proazaphosphatrane, containing a bulky aminophospine ligand, was used to catalyze the hydrosilylation of various terminal alkynes with Et3SiH or Ph3SiH. These reactions occurred efficiently and stereo- and regioselectively. Anti-markonikov E-products or Markonikov α-products were obtained with a selectivity >95% in a yield >90% except in one case where the selectivity and the yield were a little lower.
    Expression and Activities of Recombinant Directing Agent SL41 Against HIV-1 in Pichia pastoris
    LI Chang1,2, WANG Hong3, JIN Ning-Yi1*, JIN Hong-Tao1,2, LIU Yu-Sheng1,2, YU Fang1, LI Zi-Jian1, ZHANG Li-Shu1
    2007, 28(8):  1493-1496.  doi:
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    The humanize anti-HIV-1 single chain Fv fragment(ScFv) gp41 gene and super antigen staphylococcal exterotoxin A(SEA) gene were fused via soft linker peptide, and cloned into expression vector pPIC9k. The recombinant plasmid was linearized and transferred into Pichia pastoris strains GS115 by electroporation. High copies of trransformants were obtained with Muts and Mut+ phenotype identification, PCR amplification and screening of G418. After flask culture and inducing expression by methanol, the targeted protein was well expressed and performed via SDS-PAGE and Western Blot. The highest production was 47.9 mg/L when different parameters were optimized. The primarily-purified protein was analyzed with antibody affinity assay, cellular binding activity and cellular killing activity using the HIV-1 infection target cell models prepared by our laboratory. The results suggest that the constructed anti-HIV-1 gp41 recombinant agent SL41 has a good biological activity and specific CTL cytotoxicity activity. This research will provide a potential values for AIDS treatment and the settled solid foundation for clinical trials.
    Studies on the Synthesis and Cytotoxic Activities of 13-cis-Retinoyl Sugar Derivatives
    XIANG Jian-Nan1,2,3*, CHEN Chao-Yue4, JIANG Li-Hui1, ZHOU Hou-Xiang1, YIN Kai1, DENG Xiao-Qiang1, CHEN Jing1, HE Xiao-Xiao2,3, WANG Ke-Min1,2,3
    2007, 28(8):  1497-1502.  doi:
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    In order to decrease the toxicities of retinoids and enhance the pharmaceutical effects, especially the cytotoxic activities, retinoic acids were modified by glycosyl groups. Nine new retinoyl sugar derivatives of 13-cis-retinoic acid(5a—5d, 6a, 10a—10c, 11a) were synthesized in good yields. Their structures were characterized and their cytotoxic activities were determined in vitro with MTT assay by using human cancer lines including A549 cells lines etc. The results show that glucoside derivatives exhibited interesting cytotoxic activities and their cytotoxic activities are stronger than glycosyl esters. Deactylation of compounds 5a and 10a also improved their bioactivities, respectively.
    Design, Synthesis and Activity Evaluation of Novel Selective Serotonin Reuptake Inhibitors
    YANG Jing, WANG Xiao-Fang, DU Guan-Hua, QIN Fang, WEN Hui, YANG Guang-Zhong*
    2007, 28(8):  1503-1507.  doi:
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    Depression is a kind of common and severe mental illness. During the past two decades, selective serotonin reuptake inhibitors(SSRIs) have been proved to be a safer and more effective resistance than the first-generation antidepressants(TCAs and MAOIs), and have gained incredible popularity.Based on the conformation analysis and pharmacophore information of SSRIs, flexible database searching from the NCI-3D and Maybridge-3D database was performed. Three classes of the new compounds structures were designed and 27 analogues were prepared and evaluated as potential antidepressant agents. Biphenylbenzamidine derivative Ⅰ-19 showed good activity of affinity to the 5-HT transporter. It can be used as the lead structure for drug design with the objective of making more potent inhibitors against 5-HT transporter.
    One New Flavanoid and Anti-HIV Active Constituents from Boussingaultia gracilis Miers var. pseudobaselloides Bailey
    GU Qiong1,4, MA Yun-Bao1,3, ZHANG Xue-Mei1,3, WANG Rui-Rui2,4, ZHOU Jun1,3, ZHENG Yong-Tang2,3, CHEN Ji-Jun1,3*
    2007, 28(8):  1508-1511.  doi:
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    Boussingaultia gracilis Miers var. pseudobaselloides Bailey(Basellaceae) is a folk medicine used as an analgesic and supplements, only a few research was reported on the chemical constituents of this plant. This paper presented its chemical and anti-HIV active constituents. By column chromatography(Silica and Sephadex LH-20 gel) methods, two flavanols and four flavones were isolated from the 70%(volume fraction) ethanol extract. Based on extensive spectral analysis(UV, IR, MS and 1D, 2D NMR), compounds 1—6 were identified as bougracol A(1), 4,7-dihydroxy-5-methoxy-8-methyl-6-formyl-flavane(2), 7-O-methylunonal(3), 5,7-dihydroxy-6,8-dimethyl-2-phenyl-4H-1-benzopyran-4-one(4), desmosflavone(5) and demethoxymatteucinol(6). Among them, compound 1, a new flavan-diols, was deduced to be 7-hydroxy-5-methoxy-8-methyl-6-formyl-flavan-3,4-diols, and compounds 2—6 were firstly obtained from this plant. Anti-HIV assay suggests that compounds 1, 2, 5, 6 showed weak anti-HIV activities with EC50 values of 45.09, 48.73, 55.47 and 82.75 μmol/L, and TI values of 1.41, 1.20, 7.15 and >8.51, respectively.
    Synthesis and Bioactivity of 3-N-Benzyloxycarbonyl-β-aminobutyric Saccharide Carboxylate
    ZANG Hong-Jun1, LI Zheng-Ming2*, FAN Zhi-Jin2, LIU Xiu-Feng2, WANG Su-Hua2
    2007, 28(8):  1512-1515.  doi:
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    The plant activators such as D,L-β-aminobutyric acids can induce systemically acquired resiatance in the treated plants against the pathogen infection. Saccharide carboxylate compounds are known for their physiological and pharmaceutical importance. In order to investigate the synergic effect of the glucose and β-aminobutyric acid , eight new glycosyl esters of β-aminobutyric acid were synthesized with the reaction of 3-N-benzyloxycarbonyl-β-aminobutyric acid with acetylated glycosyl bromide or di-O-isopropyllidene-glucose. The structures were confirmed via elemental analysis and 1H NMR. Bioassay results indicate that several compounds show a better induced activity against pathogen infection than salicylic acid.
    研究简报
    Simple Method for Synthesizing Laminine
    LI Qun*, PENG Yan-Lei, LI Shun-Xin
    2007, 28(8):  1516-1518.  doi:
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    Laminine(4) is a kind of non-protein amino acids in the kelp, which can prevent and cure hypertension. Because of its trace amount in the nature, it was always prepared by using bio-mimetic synthesis methods. And none or few of the synthetic methods of compound 4 were reported so far. In this article, with lysine(1) as the starting material, compound 4 was prepared with bio-mimetic synthesis method, with a yield of 37.6% and a purity of 97.2%. The structure of compound 4 was determined via HPLC, IR, MS, 1H NMR, 13C NMR and element analysis, and some of its physical and chemical properties were also studied. The results show that compound 4 is white crystalloid and has no smell, the quasi-molecular ion peak of compound 4 is m/z 207.1, and chemical shift δ 3.63(s, 9H), the features at 2945, 2863 and 1480 cm-1 in IR spectrum all show that ε-amino group of compound 4 is fully alkylated. This method could get pure laminine with simple operations, and it could be considered as a green technology with great industrial profits and notable ecological values.
    研究论文
    Preparation and Luminescent Properties of Rare Earth Ions in M2B5O9Cl∶Re(M=Ca, Sr, Ba; Re=Eu, Tb)
    MO Feng-Shan1, LIU Xiao-Tang2*, SHI Chun-Shan3
    2007, 28(8):  1519-1522.  doi:
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    M2B5O9X∶Re(M=Ca, Sr, Ba; X=Cl, Br; Re=Eu, Tb) phosphors were synthesized via solid state method. The products were characterized with X-ray powder diffraction and luminescence spectrometer. The luminescent properties as well as the influences of the matrix composition and other doping ions on the luminescence of the rare earth ions of the co-doped phosphors were investigated. The coexistence of Eu3+, Eu2+and Tb3+ were observed in these matrices. The phenomenon may be explained by the electron transfer theory. The sensitization of Ce3+ ion improves the intensity of emission of Eu2+ and Tb3+. The competition between electron transfer among conjugate rare earth ions and energy migration might be the reasons for the observation. We predict a novel trichromatic phosphor co-doped with Eu3+-Tb3+ in M2B5O9X.
    Oxidation of Styrene Catalyzed by Ionic Manganese Porphyrin Immobilized in Ionic Liquid
    LIU Ye, ZHANG Hong-Jiao, WU Hai-Hong, LIU Xiu-Li, CAI Yue-Qin, LU Yong*
    2007, 28(8):  1523-1527.  doi:
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    Without the additional involvement of axial ligand and organic solvent, the ionic manganese porphyrin [MnⅢ(BF4)T(N-Me-4-Py)P][BF4]4(1d) immobilized in [BMIM]BF4 efficiently catalyzed the oxidation of styrene with a good activity(87% conv.) and epoxide selectivity(90%) under mild reaction conditions. The generality of 1d-[BMIM]BF4 system to the substrates of styrene derivatives with different electronical effects also lead to the pleasing results. The degradation of metalloporphyrin coming from the π-π stacking of porphyrin itself and the oxidation destruction was greatly suppressed in this built-up 1d-[BMIM]BF4 system.
    Synthesis and Characterization of a New Organic-inorganic Hybrid Mesoporous Basic Catalyst
    WANG Hong-Su1, WU Shu-Jie1, SHAO Yan-Qiu1,2, XU Ling1, SONG Ke1, XU Hai-Yan1, KAN Qiu-Bin1*
    2007, 28(8):  1528-1531.  doi:
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    A hybrid mesoporous HMS silica materials were synthesized via co-condensation between tetraethylorthosilicate(TEOS) and bis[3-(trimethoxysilyl)propyl]amine(BTMSPA) by using octadecylamine as the template through the “S0I0” route. The sequential addition of TEOS and BTMSPA resulted in well-ordered porous hybrid silicates. The synthesized materials were characterized by means of X-ray diffraction, N2 gas adsorption-desorption experiments, 29Si MAS NMR and condensation reaction of benzaldehyde with 2'-hydroxyacetopheone.
    Studies on the Co-doping Modified Spinel LiMn1.98Cr0.02O4-yCly
    FENG Ji-Jun1*, XU Rong-Qi1, TANG Zhi-Yuan2, AI Hong-Qi1
    2007, 28(8):  1532-1536.  doi:
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    The co-doping modified spinel LiMn1.98Cr0.02O4-yCly(y=0, 0.01, 0.02, 0.03, 0.04, 0.05, 0.10) as the cathode for lithium ion battery were synthesized with high-temperature solid-state reaction method. X-ray diffraction were used to characterize the crystal structure of the produced materials. The effects of co-doping modification in stabilizing the crystal frame and improving the electrochemical properties were comparatively investigated in terms of crystal structure, charge and discharge capacity, cycle performance and rate performance. The investigation comes to the conclusions that the co-doping modified cathode materials held the high enough initial capacity and represented an excellent cycle performance as well. In addition, the rate performance was also improved obviously. Among the co-doped materials, the most outstanding general performance belongs to LiMn1.98Cr0.02O3.96Cl0.04 which showed an initial specific discharge capacity of more than 127 mA·h/g and kept 110 mA·h/g after 50 cycles.
    Mathematical Modeling of Non-adiabatic Polymerization Fronts
    LU Guo-Dong, YAN Qing-Zhi*, GE Chang-Chun
    2007, 28(8):  1537-1542.  doi:
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    A mathematical model for simulating the front propagation process in a non-adiabatic system, including the effect of reactor size on propagating front, was developed. From the model, the expressions for the temperature at front and the front propagation velocity were derived. The model reliability was supported in comparison of its predictions, in terms of propagating velocity of the starch-grafting-acrylic acid propagation front, with the measured data under various conditions such as initiator concentration, initial temperature, and tube size when the formation of bubbles due to solvent evaporation was absent. On the other hand, the deviation of the theoretical values from the experimental data occurred when a large number of bubbles were formed during the reaction.
    Studies on Dehydrogenation of 2-Butanol over Supported Copper Catalysts Prepared by Sol-Gel and Impregnation Methods
    JI Ding-Hao, LIU Gang, JIA Ming-Jun, ZHANG Wen-Xiang, WANG Guo-Jia, WU Tong-Hao, WANG Zhen-Lü*
    2007, 28(8):  1543-1546.  doi:
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    The Cu/SiO2 catalysts were prepared by sol-gel and impregnation methods. The effect of the diffe-rent preparing methods and contents of copper on the structure and property of the catalysts was studied, and the activity of these catalysts on the dehydrogenation of 2-butanol and the selectivity for MEK were also investigated. These catalysts were characterized by means of BET, XRD, EPR and TPR. The results indicat that the high dispersing copper catalysts could be prepared by using sol-gel method. There were two kinds of copper species on the surface of catalysts, one was the unreduced isolated Cu2+, the other was the copper oxide clusters. There was only the copper oxide clusters on the catalyst prepared by impregnation method. The results show that the isolated Cu2+ was inactive for dehydrogenation of 2-butanol. The copper oxide clusters could be reduced to Cu0 during the reaction, Cu0 was the main stable active sites for this reaction.
    Ligand Binding Affinity of Cyanide Complex of Single Mutant F106L Murine Met-Neuroglobin
    DU Wei-Hong1,3, YIN Guo-Wei1, LI Yan-Jie2, WEI Qun2, LI Juan3, FANG Wei-Hai3*
    2007, 28(8):  1547-1551.  doi:
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    Neuroglobin(Ngb), a recently discovered mammalian heme protein, is predominantly expressed in vertebrate brain and retina. The site G5(F106) in protein structure has been proved as one of the key proximal residues in maintenance of heme pocket conformation. Herein, to investigate the attributions of heme pocket structure of Ngb, especially in proximal side, the mutant F106L was implemented in laboratory. Solution 1H NMR method was utilized to study the binding process of exterior ligand CN- to F106L Ngb mutant. The results indicate that in the binding of CN- with NgbF106L a dynamic process exists and the Ngb F106LCN complex could reversibly release CN-, hence the interior His64 might rebind to iron as the sixth ligand. It reveals that the G5 residue in Ngb serves to conservation in partial conformation of heme pocket predominantly. Furthermore, molecular mechanics calculation suggests that proximal residues like G5 and FG5 in Ngb also take an important role in serving for structural stability and controlling the thermodynamics and kinetics of coordination equilibrium of met-neuroglobin with exterior ligand.
    Molecular Docking Study on Interaction Mode Between Yeast AHAS and Sulfonylureas Inhibitors
    LI Qiong1, CHEN Pei-Quan1,2, CHEN Lan1, SUN Hong-Wei1,2*, SHEN Rong-Xin,1 LAI Cheng-Ming1, LI Zheng-Ming1
    2007, 28(8):  1552-1555.  doi:
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    On the basis of the complex structures of AHAS and sulfonylureas inhibitors, systematic molecule docking study of five sulfonylureas inhibitors to AHAS were performed with autodock 3.0 package. The systematic docking results indicate that two kinds of docking modes are consistent basically each other, and closely correlated with experimental results as well. The further research reveals that the sequence of docking results were not affected via the appearance of FAD and TPP. Due to the VDW interaction between R2 substituent and flavin ring of FAD, the docking complex of inhibitors to AHAS became more stable. It was assumed that the unfavorable electrostatic interaction between the inhibitors and TPP may be the factor which accelerates the degradation of TPP.
    Modification Studies on the Novel Anode Material Li4Ti5O12 with Characteristic of Fleetly Charging for Lithium Ion Batteries
    YU Hai-Ying, XIE Hai-Ming, YANG Gui-Ling, YAN Xue-Dong, WANG Rong-Shun*
    2007, 28(8):  1556-1560.  doi:
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    Spinel Li4Ti5O12 for the lithium ion battery was used as an anode material, during the process of Li+ intercalation and de-intercalation, its crystal structure did almost no change, so it is regarded as a “zero strain” material. But Li4Ti5O12 has a poor electric conductivity, only 10-9 S/cm, which affects its cycling stability and high rate characteristics. Here, Li4Ti5O12/polyacene (PAS) composite was prepared via a solid-state method using TiO2-anatase, Li2CO3, and polymer degradation carbonousPolyacene(PAS) as precursors. Doping with PAS greatly improved the electric conductivity and electrochemical performance over the pure Li4Ti5O12. The conclusion, which was measured by four-probe apparatus, showed that electric conducti-vity of the composite was enhanced for nine-magnitude order. The electrochemical tests indicated that the Li4Ti5O12 doping with mass fraction of 10% of PAS exhibited the initial specific capacity is 137.3 mA·h/g at 10C, and it is still 100 mA·h/g over 200 cycles.
    Theoretical Investigation of Electronic Structures and Optical Properties of Conjugated Polymers Derived from Fluorene and Benzoselenadiazole
    LI Yan1,2, FENG Ji-Kang1,2*, REN Ai-Min1, YANG Li1
    2007, 28(8):  1561-1565.  doi:
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    The ground states of poly(9,9-diethylfluorene-co-alt-benzoselenadiazole) were full optimized with DFT at B3LYP/3-21G* level, in which the comonomer molar ratios of9,9-diethylfluorene(DEF) and benzo-selenadiazole(BSeD) are 1∶1 and 2∶1. TDDFT and ZINDO calculations of the lowest excitation energies and absorption wavelengths were performed at the optimized geometries of the ground states. Band gaps of the corresponding polymers were obtained by extrapolating HOMO-LUMO gaps and the lowest excitation energies as well as the maximal absorption wavelengths of the polymers to the infinite chain length. By the extrapolation results, the bond gaps are becoming lower with increasing the concentration of BSeD, while the maximal absorption wavelengths are red-shifted. The excited geometry is optimized by ab initio CIS/3-21G* and the emission spectra was computed based on the excited geometry. By the calculation results, the excited geometry was more planar.
    Quantum Chemistry Calculation on 5'-pTpTpCp-3' Cleavage by Serine/Histamine Amide
    LIU Hua-Nai1*, WANG Bing-Feng2, SUN Ming3, ZHANG Lei1
    2007, 28(8):  1566-1569.  doi:
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    A quantum chemistry calculation was carried out to study the mechanism of 5'-pTpTpCp-3' cleavage by the L/D-Ser-Hism. The effective molecular recognition between L/D-Ser-Hism and DNA through multi-hydrogen-bonds and the corresponding structural parameters were obtained. The results could be used to explain the mechanism of DNA cleavage by L/D-Ser-Hism.
    研究快报
    Direct Catalytic Hydroxylation of Several Typical Aromatic Compounds over Fe/Activated Carbon Catalyst
    ZHONG Yong-Ke, LI Gui-Ying*, ZHU Liang-Fang, TANG Dian-Yong, HU Chang-Wei*
    2007, 28(8):  1570-1572.  doi:
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    Fe/activated carbon was found to be catalytically effective for the one-step hydroxylation of several typical substituted aromatic compounds under milder reaction conditions(303 K, atmospheric pressure). It was found that the ring oxidation is predominant for all the substrates studied and the selectivity to ring oxidation was much greater than those reported previously. A comparison of the conversions with that of benzene revealed that electron-donating substituents increase the conversions of the substrates, while electron-withdrawing substituents decrease the conversions. The formation of o- and p-hydroxylated products for electron-donating substituted aromatic compounds and o-, m-, p-hydroxylated products for electron-withdrawing substituted aromatic compounds revealed an electrophilc mechanism. The predominant selectivity to o-hydroxylated products for the aromatic compounds with substituents which could coordianated with Fe also shows a new mechanism. This coordianation was affected by the steric hindrance of the substituents. The latter mechanism was also confirmed by DFT method.
    研究论文
    27Al NMR Studies on HPAM/AlCit Crosslinking System with Low Concentration Polymer
    LIN Mei-Qin*, DONG Zhao-Xia, LI Ming-Yuan, WU Zhao-Liang
    2007, 28(8):  1573-1576.  doi:
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    The change of the chemical shift and the spin-lattice relaxation time of Al in the reaction process of partially hydrolyzed polyacrylamide(HPAM) with a low concentration and high molecular weight and aluminum citrate(AlCit) system are investigated via 27Al NMR measurement. The experimental results show that after crosslinking the chemical shift of Al which crosslinked with the carboxyl of HPAM increased, but the chemical shift of Al which didn't react with HPAM almost kept the same. There are three phases of aluminum in the HPAM/AlCit crosslinking system.These three phases of aluminum correspond to three different spin-lattice relaxation time of Al. When the concentration of HPAM is less than or equal to 200 mg/L, the spin-lattice relaxation time(τ13) of Al was decreased with the increase of reaction time after crosslinking, the linked polymer solution was formed mostly by intra-molecular crosslinking reaction between HPAM and AlCit when the concentration of HPAM was more than or equal to 250 mg/L, the spin-lattice relaxation time(τ13) of Al was increased with the increase of reaction time after crosslinking, the linked polymer solution was formed mostly by inter-molecular crosslinking reaction between HPAM and AlCit.
    Replication of Superhydrophobic Surfaces of Polymer from Abrasive Papers
    XIE Yong-Yuan, ZHOU Yong-Liang*, YU Xiao-Chun, XIA Hai-Ping
    2007, 28(8):  1577-1580.  doi:
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    Abrasive papers are well-known tool for polishing solid surface with different roughnesses. Here we present a facile method for making superhydrophobic surface using the metallographic abrasive papers as the mold. The rough surfaces of polymers including polydimethylsiloxane, polyethylene, polypropylene, and polystyrene were prepared with casting or hot embossing on the abrasive paper molds. SEM results reveal that the roughness of the polymer surface could be controlled by selecting the mold. Contact angle measurement shows that the water contact angle(WCA) on the as-prepared surfaces increased with the increase of roughness of the abrasive papers used, especially, the WCA on the surfaces prepared with types of W7, W5 abrasive papers can reach more than 150°, alias superhydrophobic surface. The replicas show that the changing from Wenzel state to Cassie state indicated the roughness changing. And the difference of WCA on rough surface between polymers with different intrinsic contact angles is decreased while Wenzel state changes to Cassie state.
    Preparation of a Novel Amphiphilic Copolymer Microspheres with Phenylborate Moieties and Its Glucose-sensitive Properties
    TANG Yu, WANG Zhen, LI Chao-Xing*
    2007, 28(8):  1581-1585.  doi:
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    A novel amphiphilic copolymer was prepared via copolymerization of N-acryloyl-3-aminophenylboronic acid with β-cyclodextrin containing maleic anhydride. The copolymer was characterized with 13C NMR, IR and UV-Vis techniques. The self-assembling morphology of the polymer microspheres in methanol was studied via SEM. The reaction mechanism of polymer with methanol and self-assembling mechanism were discussed with research on the solubility of the polymer in various solvents. Gliclazide as the model drug was loaded in the copolymer microspheres and the drug release oscillating behavior was studied. The results indicate that the microspheres respond to glucose rapidly in 30 min, and the microspheres exhibit self-regulated“on-off” release behavior between the solution with 3 g/L of the glucose and the medium without glucose.
    Synthesis and Blue Electroluminescent Properties of Copolymers Derived from Silafluorene and Thiophene
    JIANG Xi, TIAN Ren-Yu, MO Yue-Qi*, CAO Yong
    2007, 28(8):  1586-1592.  doi:
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    Two series of silafluorene based copolymers containing a small molar fraction(1%—3%) of thiophene derivatives moieties were synthesized with Yamamoto coupling reaction: poly{9,9-dihexyl-3,6-silafluorene-co-[2,5-di(phenylene-4-yl)-thiophene]}(PSiF-DPT) and poly{9,9-dihexyl-3,6-silafluorene-co-[2,5-di-((2-methylphenylene)-4-yl)-thiophene]}(PSiF-DMPT). These copolymers were characterized via UV-Vis absorption spectra and photoluminescence spectra. Polymer light-emitting diodes(PLED) were fabricated to investigate these electroluminescent properties. It was found that the thiophene derivatives moieties became the efficient blue emitter via efficient energy transfer from the polysilafluorene segments. With the decrease of the coplanarity of thiophene derivatives or its feed ratio, the PL and EL spectra can be blue shifted. The color purity can be adjusted to CIE(0.19,0.16) with a EL quantum efficiency of 0.46%.
    Preparation and Characterization on Cecropin B Peptide Grafted with Silk Fibroin Films
    BAI Li-Qiang1, MA Ting-Fang2, YAO Ju-Ming1*
    2007, 28(8):  1593-1597.  doi:
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    The undisolvable Bombyx mori silk fibroin film was prepared from the regenerated silk fibroin solution followed with the 60%(volume fraction) ethanol aqueous solution treatment. The silk fibroin film was grafted with Cecropin B peptide via the carbodiimide chemistry. The secondary structure, the film surface properties and the bacteriostatic activity of the obtained silk fibroin film were analyzed with FTIR, SEM, EDS and the antibacterial tests. The results show that the Cecropin B peptide is covalently grafted onto the surface of silk fibroin film, which is undisolvable and has an effective and permanent bacteriostatic activity.
    UV Curing Behavior and Kinetics of Hyperbranched Polysiloxane
    ZHANG Guo-Bin, FAN Xiao-Dong*, KONG Jie, LIU Yu-Yang, WANG Sheng-Jie, SI Qing-Fa
    2007, 28(8):  1598-1605.  doi:
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    Ultraviolet(UV) curing behavior and kinetics of hyperbranched polysiloxane(HBP) were studied via isothermal Differential Photo Calorimeter(DPC) technology. Firstly, the influences of the factors such as photoinitiator's concentration, light intensity, temperature and atmosphere, on UV curing behavior were investigated in detail. It is found that both curing rate(R) and ultimate vinyl conversion(C) could be raised by the increase of photoinitiator's concentration and UV light intensity as well as elevating temperature. Oxygen possessed an inhibition effect on the curing, however, it could be reduced by enhancing UV light intensity. The results could be confirmed by that induction period can be reduced by higher UV light intensity. Secondly, curing kinetics were also studied by using an autocatalytic model with a diffusion term attached. The kine-tic parameters were calculated from that model, and correspondingly, the total apparent reaction exponent and apparent activation energy were obtained within the range of 6—7 and 9.95 kJ/mol, respectively. Comparative results between kinetic calculations and experimental measurements show that the autocatalytic model used was suitable to simulate the autocatalysis phenomena at the initial stage and the termination process could be controlled by diffusion. Finally, comparison of curing behavior between the HBP and two low-functionality monomers indicates that the unique hyperbranched structure and the corresponding high multifunctionality led to the gelation at the very initial stage of curing, as a result, relatively low ultimate vinyl conversion was observed.
    研究快报
    Synthesis and Chiral Recognation of Hollow Chiral Polymer Microspheres with Amide Side Group
    YAO Jin-Shui*, ZHANG Xian, WEI Ming-Xing
    2007, 28(8):  1606-1608.  doi:
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    Two kinds of chiral monomers, (-)α-phenylethyl-acrylamide and (-)α- phenylethyl-10-undecendyl amide, were synthesized via consendation of (S)-α-phenyl ethyl amine and acryl chloride or 10-undecendyl chloride.Their structures and purities were determined via IR, 1H NMR and elemental analysis. The seeded microspheres of polystyrene(about 3 μm) were prepared with dispersion polymerization, and monodisperse hollow chiral polymer microspheres were prepared with two-stage swelling procedure via copolymerization of styrene, divinyl benzene and the chiral monomers synthesized above.The average diameter of the microsphere was about 10 μm.The chiral polymer microspheres were used to be the stationary phase of HPLC. The molar ratio of (S)-α-ethyl hydroxy phenylbutyrate and (R)-α-ethylhydroxy phenylbutyrate were determined via chiral HPLC. The chromatography results showed that the chiral recognition was very higy when using chiral polymer microsphere,prepared by S-10-undecylenoyl(α-phenyl)ethylamide as chiral monomer, as chiral stationary phase of HPLC.
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