Table of Content

10 August 2008, Volume 29 Issue 8

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高等学校化学学报2008年第29卷第8期目次

2008, 29(8):  0.  doi:

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下期目次预览

2008, 29(8):  0.  doi:

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研究论文

Hydrothermal Syntheses of Hollow Carbon Nano-materials by Ostwald Ripening

CHEN Kai^1,2;MA Ding¹*;HUANG Wei-Xin²;BAO Xin-He¹

2008, 29(8):  1501-1504.  doi:

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A facile method to fabricate carbon nano-materials, with starch as a carbon precursor and ferrous salt as an additive, was reported. TEM studies indicated that the FeOOH nanorods were first generated as templates, on which carbon deposited, leading to the formation of FeOOH/carbon core-shell composite nanowires. With longer reaction time, the FeOOH cores can be dissolved spontaneously, leaving hollow carbon nanorods. The mechanism of this dissolution was attributed to Ostwald ripening. When glucose or CD was used as the precursor, hollow carbon spheres would be obtained, which could be attributed to the different surfactant effects of those precursors. This provides a very efficient method to prepare hollow carbon nanostructures via the one-pot synthesis approach. The new synthetic method has a potential to be extended to the preparation of various hollow nanostructures.

Preparation of Large Area Single Crystal Bismuth Nanowire Arrays

JIN Chuan-Gui*, TAN Jie

2008, 29(8):  1505-1509.  doi:

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The ordered nanowire arrays of semi-metal bismuth were successfully prepared by electrodeposition into the pores of anodic alumina membrane(AAO). The structure and morphologies of the as-prepared sample were characterized by X-ray diffraction(XRD), field emission scanning electron microscopy(FE-SEM), and transmission electron microscopy(TEM). XRD result indicates that the as-prepared sample is bismuth with a hexagonal structure, and has a preferential growth direction along the [110] direction. The FE-SEM photos clearly show that the bismuth nanowire arrays are large-area, high-filling and highly ordered. TEM results indicate that the diameter of nanowires is uniform, the surface of nanowires is smooth, and the ratio of nanowires is high. The clear lattice stripes and bright selected electron diffraction spots of HRTEM photo demonstrate single crystal nature of the as-prepared sample.

Synthesis, Crystal Structure and Properties of an Inorganic/Organic Hybrid Supramolecule Compound of the Four-electron Reduced α-Keggin-type Phosphomolybdate

ZHANG Li-Juan², LI Yu-Hao², ZHOU Yun-Shan^1,2*, HAN Rui-Xue², ZHANG Li-Hui²

2008, 29(8):  1510-1514.  doi:

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The first four-electron reduced α-Keggin type phosphomolybdate-based organic-inorganic hybrid supramolecule compound was hydrothermally synthesized in the necessary presence of copper ion by reacting α-Keggin type phosphomolybdic acid and 1,6-hexanediamine, and characterized thoroughly via single-crystal X-ray diffraction, elemental analysis, IR,UV-Vis, TG/DTA, XPS, magnetic and electrochemical studies.

Preparation and Characterization of Polymer-derived Si-B-N-C Fibers

TANG Yun, WANG Jun*, LI Xiao-Dong, LI Wen-Hua, WANG Hao, WANG Xiao-Zhou

2008, 29(8):  1515-1518.  doi:

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Si-B-N-C ceramic fibers were prepared by polymer derived method using precursor polyborosilazane. The composition, structure, high temperature stability and oxidation resistance of the ceramic fibers were investigated. The results indicate that the Si-B-N-C fibers combine several desired properties relevant for an application in fiber-reinforced ceramic composites. The fibers show good mechanical properties with the tensile strength 2.1 GPa and elasticity modulus 230 GPa. The ceramic fibers resist crystallization up to 1700 ℃ and only a mixture of partial crystallized Si₃N₄, BN and SiC phases is observed when heated to 1850 ℃ in N₂ atmosphere. The fibers also show a excellent stability against oxidation, with a weight gain of only 3.3% in flowing air up to 1400 ℃.

Synthesis, Crystal Structure and Combustion Catalytic Activity of a Novel Energetic Complex [Pb(AZTZ)(bpy)(H₂O)·2H₂O]_n

ZHAO Feng-Qi¹, CHEN San-Ping², FAN Guang², XIE Gang², JIAO Bao-Juan³, GAO Sheng-Li²*

2008, 29(8):  1519-1522.  doi:

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A novel energetic complex with a formula of [Pb(AZTZ)(bpy)(H₂O)·2H₂O]_n(1)(AZTZ=5,5’-azotetrazole dianion, bpy=2,2’ bipyridine ) was synthesized and its structure was characterized by elemental analysis, IR, thermalgravimetric analysis and single crystal X-ray diffraction method. Crystal data: triclinic system, space group P1, a=0.7341(6) nm, b=1.0050(8) nm, c=1.3367(1) nm, α=95.354(1)°, β=101.450(1)°, γ=101.233(1)°, V=0.8927(1) nm³, Z=2, S=1.030, final R indices[I>2σ(I)], R₁=0.0301, wR₂=0.0605, for all reflections R₁=0.0351, wR₂=0.0630. In addition, the catalytic performance of complex 1 on the combustion of solid double-based propellant is presented, which shows that complex 1 can enhance the burning-rate of solid double-based propellant.

Preparation and Performance of Intermediate-temperature Composite Electrolytes of SDC-LSGM

XU Dan, LIU Xiao-Mei*, WANG De-Jun, ZHU Cheng-Jun, YAN Duan-Ting, PEI Li, SU Wen-Hui

2008, 29(8):  1523-1527.  doi:

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The electrolytes materials Ce_0.85Sm_0.15O_1.925(SDC) and La_0.9Sr_0.1Ga_0.8Mg_0.2O_2.85(LSGM) were synthesized by means of glycine-nitrate process(GNP), respectively, then the composite electrolytes were prepared by mixing SDC and LSGM(the mass ratio of SDC powder to LSGM powder are 9∶1, 8∶2, 5∶5, respectively). Its electrical properties were investigated by impedance spectroscopy in air. The results obtained shows that when the composition was 90% SDC and 10%(mass fraction) LSGM(SL91), the electrolyte has a higher electrical conductivity in comparison to SDC in the temperature range of 350—800 ℃. Electrolyte-supported solid oxide fuel cells(SOFC) was fabricated with NiO/SDC as the anode and Sm_0.5Sr_0.5CoO₃ as the cathode. The V-I characteristics of single fuel cell shows that the maximum output power density was 0.25 W/cm² at 800 ℃ and the maximum current density was 1.06 A/cm² for the cell with SL91 as the electrolyte. The open circuit voltage(OCV) of the single fuel cell using the composite as the electrolytes was higher than the cell using single SDC as the electrolyte in the working temperature range of 600—800 ℃. It can be confirmed that to some extent, doping LSGM to SDC can block off the electronic current caused by the Ce⁴⁺/Ce³⁺ reduction process.

Syntheses, Crystal Structure and Luminescence Properties of A Novel Two-dimensional Grid Framework Coordination Polymers [Zn(DPA)]_n

ZHANG Zhong-Qiang^1,2, HUANG Ru-Dan¹*, XU Yan-Qing¹, HU Cuang-Wen¹*

2008, 29(8):  1528-1531.  doi:

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Pyridine-2,6- dicarboxylic acid (H₂PDA) as a very important carboxylate derivative was attracted much attention in coordination chemistry. In H2PDA, there is a 120° angle between the central rigid pyridine ring and two carboxylate groups. Therefore, it could potentially provide various coordination motifs to form discrete or consecutive metal complexes under the appropriate synthesis condition. There are a few literatures reported about the complexes based on H2PDA.In this paper, a new coordination polymer [Zn(PDA)]_n(H₂PDA=Pyridine-2,6-dicarboxylic acid) was synthesized with hydrothermal method, and characterized by elemental analyses, IR spectrum,TGA and single-crystal X-ray diffraction. The compound exhibits an two-dimensional(2D) grid framework structure. The crystal crystallizes in an orthorhombic system, space group of Pbcn with a=0.6730(3) nm, b=1.4156(6) nm, c=0.7299(3) nm, V=0.6954(6) nm³, Z=4. Each Zn(Ⅱ) is five coordination with three PDA^2-, and Zn(Ⅱ) adopts a distorted trigonal bipyramid coordination mode. The two-dimensional(2D) grid framework structure is built by the connection of Zn(Ⅱ) and PDA²⁺. The border length of the grid framework is 0.5082 nm×0.5082 nm. The two pyridine rings in the adjacent PDA^2- are parallel with each other, and the center distance between them is 0.39275 nm. So, weak π-π stacking interaction exists in the structure of [Zn(PDA)]_n. The luminescent property of [Zn(PDA)]_n was investigated. The luminescence emission spectrum of [Zn(PDA)]_n is the same as the the ligand pyridine-2,6-dicarboxylic acid, and also the two weak peaks. So, we conclude that the electron transition gap is not changed when Zn(Ⅱ) coordinated to PDA^2-.

研究快报

Preparation and Characterization of Flower-like YBO₃∶Eu³⁺ Thin Film

YANG Zhi*, SONG Feng, WANG Xiao-Lin

2008, 29(8):  1532-1534.  doi:

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Flower-like YBO₃∶Eu³⁺ thin films were prepared on the AAO template by a hydrothermal method and the effects of some processing variables, such as temperature and calcinated time, were investigated. The formation of YBO₃∶Eu³⁺ thin films were confirmed by EDX, XRD and PL spectra. The PL spectra show that the characteristic emission of the YBO₃∶Eu³⁺/AAO thin film is the ⁵D₀ →⁷F₁ transition.

研究论文

Influence of Saikosaponina A on Monoamine Neurotransmitters and the Corresponding Metabolin Compositions in Depressed Rats’ Brain

GE Hong-Yan¹, CHEN Bo¹, XU Dan¹, LI You-Tian¹*, LI Yang²

2008, 29(8):  1535-1538.  doi:

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The high performance liquid chromatography was applied to investigate the influence of the chemical composition, saikosaponina A, on monoamine neurotransmitter in the depressed rats’ brain. It is shown from the analytical results that in the depressed rats’ brain, the contents of homovanillic acid, noradrenaline, dihydroxyphenyl ethylamine and 5-HT increase in the presence of the saikosaponin A. These results can help to clarify the mechanism of saikosaponin A in curing the depression.

Preparation of Localized Surface Plasmon Resonance Sensing Film with Gold Colloid by Electrostatic Assembly

WANG Ye¹, BU Feng-Quan², GU Yue-Jiao¹, XU Ping², NING Xiao-Hua¹, XU Shu-Ping¹, ZHAO Bing¹, XU Wei-Qing¹*

2008, 29(8):  1539-1543.  doi:

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This paper presents a new method to prepare localized surface plasmon resonance(LSPR) sensing film by self-assembly of polyelectrolyte. The optical signal arises from the dependence of the peak intensity and position of the localized surface plasmon spectrum of gold nanoparticles upon the refractive index of the surrounding medium. By using an electrostatic layer-by-layer assembly approach-PDDA/PSS/PVTC, 28 nm diameter colloidal gold nanoparticles are immobilized upon a glass substrate. The method yields a LSPR sensing film with good reproducibility and excellent stability. The spectroscopic response of the LSPR sensing film was investigated. The shift in the peak extinction wavelength and the change in the corresponding intensity of the LSPR band as a function of the refractive index of the solution are 71 nm/RIU and 0.21 a.u./RIU, respectively. The penetration depth of the electromagnetic field excited by LSPR upon the response of the sensing film is estimated to be about 16 nm.

Studies on the Mechanism of Copolymerization of Aniline and Propylene Oxide and Characterization of Copolymer via FTIR Technique

LI Mei-Chao^1,2*, HU Jia-Qi², LIU Yan-Na², MA Chun-An²

2008, 29(8):  1544-1548.  doi:

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Copolymerization is often used as one of the most important method to improve the physical and chemical properties of a polymer. Propylene oxide is often added to the electrolyte during electrochemical polymerization to improve some properties of the polymer. Therefore, polyaniline-poly(propylene oxide)(PAN-PPO) was synthesized in aqueous solution containing aniline and propylene oxide by electrochemical method in this paper. In situ FTIR spectroscopy was used to investigate its electrochemical copolymerization mechanism. It showed that α-ring-opening reaction of propylene oxide might be initiated by radical catalyst from aniline and its oligomer, and then copolymerization of aniline and propylene oxide took place to form structures with aliphatic-aromatic ether. In addition, the PAN-PPO film formation was regular from the middle to two sides on the platinum surface, which was characterized by FTIR microscopic image technique.

研究快报

Development of a Single-molecule Flow Analyzer

YANG Ling-Ling, ZHU Shao-Bin, HANG Wei, YAN Xiao-Mei

2008, 29(8):  1549-1551.  doi:

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A single-molecule flow analyzer based on laser induced fluorescence and hydrodynamic focusing was developed in our lab. There were three key aspects of this design for achieving single molecule detection sensitivity: (1) a detector with a high photon-detection efficiency(>65% for avalanche photo-diode detector); (2) a small probe volume obtained by sheath-protected, hydrodynamically focused sample stream to reduce background; and (3) a slow flow to provide extended dwell time(milliseconds) in the probe volume so that more fluorescence cycling can occur. The single molecule detection sensitivity was demonstrated by the successful detection of single phycoerythrin molecules. The house-constructed single-molecule flow analyzer was applied to DNA fragment sizing with linear correlation between DNA fragment length and mean burst size.

Preparation of Magnetic Fe Oxide Core/Au Shell Nanoparticles and Their Surface-enhanced Raman Spectroscopy

BAO Fang, YAO Jian-Lin, GU Ren-Ao*

2008, 29(8):  1552-1554.  doi:

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Fe oxide core/Au shell nanoparticles were prepared by the reduction of Au³⁺ onto the surfaces of Fe oxide nanoparticles and characterized by scanning electron microscopy(SEM). The results reveal that the prepared core/shell nanoparticles were covered by Au shell and the surfaces of the core/shell particles are jagged after the initial addition of Au³⁺. Surface enhanced Raman scattering(SERS) activities of these magnetic nanoparticles were studied by using pyridine(Py) as a probe molecule after a magnet was used to concentrate the colloid. It was found that the SERS intensity depends on the Au shell thickness of the core/shell nanoparticles and strengthens with the increasing shell thickness. The detection limit for Py can be very low when the magnetic Fe oxide core/Au shell nanoparticles were used and even down to 10^-7 mol/L.

研究论文

Synthesis, Characterization and Catalytic Activity of Cyclopalladated Ferrocenylimine Carbene Complex in Buchwald-Hartwig Amination

LI Jing-Ya, WU Yang-Jie*, HAN Zi-Xing, JIANG Song

2008, 29(8):  1555-1559.  doi:

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The palladium-catalyzed amination of aryl halides(Buchwald-Hartwig amination) is a rapidly developing field due to the importance of the products in many fields, e.g. pharmaceuticals, xerography, electronic materials and ligands for transition metals. In this article, a novel cyclopalladated ferrocenylimine carbene complex 3 was conveniently synthesized and characterized via IR, ¹H NMR, ¹³C NMR, HRMS and X-ray single crystal diffraction. Compound 3 was stable to air and moisture in both the solid state and solution. It was successfully applied for the Buchwald-Hartwig amination of aryl chlorides. Using 0.5%(molar fraction) of catalyst 3, in the presence of 2 equiv of ^tBuOK as a base in dioxane at 110 ℃ for 3 h, a variety of aryl chlorides and amines could be coupled to afford the coupled products in moderate or excellent yields.

Synthesis and Analytical Application of a New Heterocyclic Triazene Fluorescent Reagent 1,8-Bis(2-benthiazolydiazoamino)naphthalene

FU Guo-Liang¹, FENG Feng^1,2*, CHEN Ze-Zhong², BAI Yun-Feng², MENG Shuang-Ming², LIN Sen¹, JIANG Run-Sheng¹

2008, 29(8):  1560-1563.  doi:

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With the aid of combining 1,8-naphthalene with benthiazole through bis-triazene group, a new fluorescent reagent 1,8-bis(2-benthiazolydiazoamino)naphthalene(BBTANP) was synthesized and confirmed by means of elemental analysis, 1H NMR and infrared spectra. A chelate complex was formed by the reaction between BBTANP and Cu(Ⅱ) in a weak basic medium, which resulted in fluorescence enhancement. The possible response mechanism of BBTANP to Cu(Ⅱ) was discussed. The reaction showed a high selectivity and a high sensitivity for Cu(Ⅱ). A new spectrofluorimetric method for the determination of trace Cu(Ⅱ) with this reagent was developed. The excitation and emission wavelengths of BBTANP/Cu(Ⅱ) system were 362 and 459 nm in a basic medium, respectively. Under the optimal conditions, a linear response to copper was obtained in the concentration range from 8.0×10^-7 to 1.0×10^-5 mol/L, and the detection limit was 1.3×10^-7 mol/L. The method is selective, sensitive and simple. It has been used to determine trace copper in lake water with satisfactory results.

Immobilization of Cellulase Based on Polyvinyl Alcohol/Fe₂O₃ Nanoparticles

LIAO Hong-Dong, YUAN Li, TONG Chun-Yi, ZHU Yong-Hua, LI Du, LIU Xuan-Ming*

2008, 29(8):  1564-1568.  doi:

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To improve the enzyme activity and reusability, a new soluble, easy separated carrier was made to immolize cellulase. The immobilized cellulase based on polyvinyl alcohol/Fe₂O₃ nanoparticles was prepared with cyclic freezing thawing process. Analytic data from TEM, IR and VSM detection suggest that the average diameters of immobilized cellulase complexs were 1 μm, which contained about 10 nm Fe₂O₃ naoparticle. The factors affecting the activities of immobilized cellulase were researched. The activity retention of immobilized cellulase was achieved as 42% under the optimum conditions: pH=6.0, mass ratio of cellulase to PVA is equal to 4, mass ratio of PVA to Fe is equal to 50, 11 h for immobilization. The immobilized cellulase exhibited greater efficiency than free one and retained 50% relative activity after five times of cycled reuse, which indicates that this novel method of immobilization could be propitious to cellulase reuse and efficiency improvement.

Determination of S—NO Bond Dissociation Energies of S-Nitroso-N-acetyl-D,L-penicillamine Dipeptides

LI Xin, CHENG Jin-Pei*

2008, 29(8):  1569-1572.  doi:

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S-Nitrosodipeptides are generally believed to be good NO donors, and many NO-related biological functions have been directly associated with S-nitrosodipeptides, especially in the processes of NO-storage, transport and delivery. In this work, the heterolytic and homolytic S—NO bond dissociation energies of seven S-nitrosodipeptides were evaluated via titration calorimetry and relative thermodynamic cycles. The energetic scales of the heterolytic and homolytic S—NO bond dissociation energies of these RSNOs covered the ranges 234.5—246.2 and 101.6—122.1 kJ/mol, respectively, which indicated that the studied S-nitrosodipeptides were much easier to release a NO radical(NO^·) rather than a NO cation(NO⁺). The estimation of the heterolytic and homolytic(S—NO)^-· bond dissociation energies of the S-nitrosodipeptides radical anions gave the energetic ranges of 19.2—35.5 and 4.2—22.6 kJ/mol for the(S—NO)^-· bond homolysis and heterolysis, respectively, which meant that S-nitrosodipeptides radical anions were unstable at room temperature and favored to releasing a NO anion(NO^-) by heterolysis cleavage.

Interaction of Cucurbituril with N,N’-Bisalkyl-1,3-(4,4’-bispyridyl)propanes

JIANG Ping-Yue¹, XUE Sai-Feng^1,2*, WU Ming-Qiang¹, XIAO Xin¹, ZHU Qian-Jiang^1,2, TAO Zhu^1,2

2008, 29(8):  1573-1577.  doi:

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A series of N,N’-bisalkyl-1,3-(4,4’-bispyridyl)propane guests were synthesized from 1,3-(4,4’-bispyridyl)propane. The interaction and the models of self-assembly psedorotaxanes of cucurbit[7] uril with these synthetic guests were investigated via ¹H NMR technique and electronic absorption spectroscopy method. The experimental results reveal that the pseudorotaxane structure in which the host Q[7] included the 1,3-(4,4’-bispyridyl)propane core was the dominant model for the Q[7]-PC0 and Q[7]-PC2 interaction systems. For the guests having identical aliphatic substituents with chains longer than four carbon atoms, the dominant interaction models could start from Q[7] including the 1,3-(4,4’-bispyridyl)propane core, to including the substituted chains of the guest, and then a guest bearing three host Q[7] with the increase of the ratio of N_Q[7]/N_guest.

Bio-MS Studies of Non-covalent Interaction of Bis-β-carbolines Towards DNA and Nucleotides

DONG Xiao-Chun¹, XU Ying^1,2, Carlos AFONSO², JIANG Wei-Qun¹, Jean-Claude TABET²*, WEN Ren¹*

2008, 29(8):  1578-1582.  doi:

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The non-covalent complexes of five bis-β-carbolines alkaloids with five different double-stranded oligodeoxynucleotides were investigated via electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. These five antitumor compounds all showed DNA binding abilities. The binding affinities in the order of 2>3,4>5,1 were obtained, which mean that the length of the linkage chain between two β-carbolines has a remarkable effect on the formation of the non-covalent complexes. The competition binding experiments results were almost the same as that determined by relative ion abundances. The structure-activity relationships and sequence selectivity were discussed. The non-covalent bindings between the bis-β-carbolines 2, 4 and the nucleotide were then investigated by ESI-MS.

Synthesis, Crystal Structure and Biological Activity of N-(4-Benzyloxy/alkyloxyphenyl)-4,6-disubstituted-2-pyrimidinyl-amine Derivatives

WU Jing, WANG Bao-Lei, LI Yong-Hong, SONG Hai-Bin, WANG Su-Hua, LI Zheng-Ming*

2008, 29(8):  1583-1587.  doi:

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On the basis of the structures of five 4-benzyloxy/alkyloxy-anilines, 19 N-(4-benzyloxy/alkyloxy-phenyl)-(4,6-disubstituted-pyrimidin-2-yl)-amine derivatives were designed and synthesized. The structures of all the compounds were characterized by ¹H NMR, MS and elemental analyses. The single crystal structure of compound 5r was determined to further elucidate the structure. The herbicidal activity of the title compounds was evaluated through barnyardgrass cup, rape root methods and KARI test. Herbicidal assay indicate that substituted-anilines 3a, 3b, 3d, 3e exhibited good growth inhibitory activities against barnyardgrass, which are 88.5%, 77.3%, 82.4%, and 80.2%, respectively at the mass concentration of 100 μg/mL. The KARI test of compounds 5a—5s show that the compounds have a weak inhibitory effect on KARI enzyme.

Separation, Purification and Properties of Superoxide Dismutase from Ficus carica Leaves

ZHANG Lei, QU He-Zhi, HUANG Lu, DU Shan-Shan, HAO Dong-Yun, WANG Xiao-Ping

2008, 29(8):  1588-1591.  doi:

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A CuZn-SOD from Ficus carica leaves was separated and purified with ammonium sulfate fractionation, DEAE-Sepharose fast flow chromatography and Sephacryl S-100 HR chromatography techniques. One major bright band was achieved on polyacrylamide gel electrophoresis stained with nitroblue tetrazolium(NBT). The molecular weight of the enzyme subunit was determined by SDS-PAGE to be about 17800. We investigated the physical and chemical properties of the enzyme, and characterized its kinetic properties, such as the optimal pH, optimal temperature and the effect of chemical reagents and metal ions on the SOD. The results show that the stability of this purified SOD appeared to be better than other SODs reported. The analysis results of circular dichroism spectrum reveals that the enzyme possessed approximate 12.78% of α-helix in its secondary structure.

Preparation, Release-control and Cell Apoptosis of Liver Cancer in the Tea Polyphenol Manganese Loaded on a Chitosan Microparticles

HUANG He-Ning^1,2, LI Cheng¹, XIE Li-Sheng¹, HUANG He-Qing^1,3*

2008, 29(8):  1592-1597.  doi:

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The chitosan as a wrapping material was selected to prepare a microparticles of tea polyphenol manganese-chitosan(TPMn). Fluorescence characteristics of TPMn-chitosan microparticles was revealed by fluorescence microscopy. Size and distribution orderliness of TPMn-chitosan microparticles was further approved by the scanning electron microscopy and the transmission electron microscopy, respectively. The envelopment ratio of TPMn-chitosan microparticles was calculated to be 68% by RE-HPLC approach, which is in accordance with the ratio request of release-controlled drug at the micron level of microparticles. The results of kinetic studies show that two chitosan microparticles loaded on both tea polyphenol(TP) and TPMn, respectively, have capacity for controlling-release TP for exceeding 40 h, but this rate in TP microparticles was somewhat quicker than that of TPMn microparticles. Even so, both miscroparticles have capacity for inducing cells of liver cancer apoptosis, but this apoptosis rate by TPMn-chitosan microparticles was somewhat higher than that by TP-chitosan microparticles. The experimental results prove that the TPMn-chitosan microparticles was propitious to release and control TPMn for enhancing the apoptosis rate of tumour cell induced. TPMn-chitosan microparticles would have a potential for developing a new injecting drug for antitumor.

Preparation and Electroluminescence Property of a Non-doping OLED Based on Zn(Q-Ph)₂ and DCJTB

DING Hong-Liu, ZHAO Ting, SHI Guo-Yue, JIN Li-Tong*

2008, 29(8):  1598-1602.  doi:

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As electroluminescent material zinc bis(2-phenyl-8-hydroxyquinolato)[Zn(Q-Ph)₂] was synthesized and characterized by ¹H NMR, UV-Vis and MS measurements. DCJTB[4-(dicyanomethylene)-2-t-butyl-6(1,1,7,7-tetramethyljulolidyl-9-enyl)-4H-pyran], a highly efficient fluorescent dye, and Zn(Q-Ph)₂ were used to fabricate a kind of novel non-doping organic light-emitting diode with a structure of ITO/NPB{N,N’-Di[(1-naphthalenyl)-N,N’-diphenyl]-(1,1’-biphenyl)-4,4’-diamine}/DCJTB/Zn(Q-Ph)₂/AlQ₃(8-hydroxyquinoline aluminum)/Al. By changing the thickness of ultra-thin layer DCJTB, yellow-light, red-light and orange-light emission from OLEDs were studied. Their luminescent color, electroluminescent mechanism and recombination zone were optimized in this paper. When a 0.5 nm-thick DCJTB was used, a stable red emission was obtained. With a lower turn-on voltage at about 5.5 V, the non-doping OLED showed a ma-ximum brightness of 420 cd/m² and current density of 250 mA/cm² at 25 V.

Preparation and Characterization of Novel Visible-light-driven BiYWO₆ Photocatalyst and Its Application to Overall Water Splitting

LIU Hui, YUAN Jian, SHANGGUAN Wen-Feng*

2008, 29(8):  1603-1608.  doi:

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A new solid solution oxide BiYWO₆(BYW)was prepared by solid state reaction at a high temperature and discovered to split water into H₂ and O₂ under visible light. The XPS results proved the stability of RuO₂/Bi₂WO₆ in the photocatalytic reaction. RuO₂ was the most suitable cocatalyst for BYW. Sacrificial reagents were used to confirm the photocatalytic ability of BYW. The formation of solid solution of Y₂WO₆ and Bi₂WO₆ was suggested to raise the bottom position of conduction band and to make Bi6s contribute to creating new valence band higher than that of O_2p.

Preparation and Characterization of Cu(Ⅰ)/SO₄^2-/ZnO and Cu(Ⅰ)/S₂O₈^2-/ZnO Catalysts

LI Zhong*, HUANG Hai-Bin, XIE Ke-Chang

2008, 29(8):  1609-1615.  doi:

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Two novel solid acids of SO₄^2-/ZnO and S₂O₈^2-/ZnO were prepared by impregnating H₂SO₄, (NH₄)₂S₂O₈ solution respectively on amorphous zinc oxide and calcining at 500—600 ℃, and then used as carriers to prepare Cu(Ⅰ)/SO₄^2-/ZnO and Cu(Ⅰ)/S₂O₈^2-/ZnO catalysts via solid-state ion-exchange. The solid acids and catalysts were characterized by XRD, FTIR, TPD and TPR. It is observed that Zn₃O(SO₄)₂ was formed during the preparation of the solid acids, and both of Lewis and Brnsted acid sites were formed on SO₄^2-/ZnO and S₂O₈^2-/ZnO. NH₃-TPD shows that both SO₄^2-/ZnO and S₂O₈^2-/ZnO were very strong solid acids because the temperature of NH₃ desorption peaks were above 543 ℃. It is suggested by molecule structure analysis that the form of acid sites is due to the strongly electronic inductive effect of SO₄^2-, the bridge-coordination complex of ZnO and SO₄^2- causes the formation of Brфnsted and Lewis acid sites on the surface, but the chelate-coordination complex of ZnO and SO₄^2- has not any contribution to acid sites. Prepared by solid-state ion-exchange with the solid acids and CuCl at high temperature in N₂ follow, Cu(Ⅰ)/SO₄^2-/ZnO and Cu(Ⅰ)/S₂O₈^2-/ZnO catalysts, in which Cu(Ⅰ) was easy to be reduced, showed an excellent catalytic behavior in the oxidative carbonylation of methanol to dimethyl carbonate(DMC). Both of the catalysts showed high catalytic activity and selectivity: 98.13% selectivity of DMC based on methanol and 1.87 g/(g·h) space-time yield, respectively.

Strong Two-photon Absorption and Electrochemical Behavior of Dibenzofuran-triphenylamine Dentritic Chromophores

ZHANG Wei-Zhou¹, WANG Xiao-Mei¹*, FANG Xiang-Yun², JIANG Wan-Li³, ZHAO Jun-Fang²

2008, 29(8):  1616-1619.  doi:

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The motivation for the strong two-photon absorbing chromophore is based on the significantly potential applications such as three-dimensional fluorescence imaging, two-photon photodynamic therapy, optical data storage and TPE fluorescence microscopy. Thus, the relationship between molecular structure and strong TPA property is greatly valuable. Here, two-photon absorption(TPA) and electro-chemistry properties of three new dibenzofuran-based chromophores(named as OT-G1, OT-G1.5 and OT-G2) were investigated. Stronger two-photon fluorescence(TPF) and larger TPA cross-section were observed with the generation number increasing. It is interesting to find that the increasing of the HOMO energy level shows the contribution to enhancement of TPA cross-section.

Chemical Structure of Tribofilms and Thermalfilms of Benzothiazole Derivatives Containing Ester Group

WU Hua*, LI Jing, REN Tian-Hui

2008, 29(8):  1620-1624.  doi:

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Two kinds of 2-mercaptobenzothiazole derivatives MBTT and MBTA are synthesized, which are characterized by means of element analysis and ¹H NMR. X-ray absorption near edge structure(XANES) spectroscopy was used to analyze the chemical structure of both thermal films and tribofilms. To our know-ledge, this would be the first comprehensive study where XANES were used to examine the tribofilms and thermalfilms from heterocyclic compounds. According to the XANES analytic results, in mineral oil, the tribofilms generated from two additives MBTT and MBTA are composed of FeS₂. However, in RSO, the corresponding tribofilms are composed of FeSO₄. The thermalfilms are composed of FeSO₄ in both mineral oil and RSO.

A Theoretical Study on Complexes of Transition Metals Complex with Extended-TTF Dithiolate Ligands

HUANG Bin, CAO Ze-Xing*

2008, 29(8):  1625-1628.  doi:

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Geometries and properties of complexes of transition metals with extended-TTF dithiolate ligands were investigated by density functional theory. The effects of metal replacement and ligand modification on the structures and properties were explored. The results indicate that the HOMO-LUMO gaps in these complexes are very small. The complexation of transition metals with the extended TTF dithiolate ligand as well as the oxidation of complex plays an important role in reducing the HOMO-LUMO gap.

Relationship Between Electron Affinity/Hardness and the Clusters Size of V_n/Cr_n Clusters

NIE Xiao-Qin, XU Wen-Guo*, LU Shi-Xiang

2008, 29(8):  1629-1634.  doi:

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The relationship between the electron affinities, the hardness and the clusters size was studied for Vanadium clusters and Chromium clusters. According to the Spheroidal Jellium Model, a new formula E_A(R)=W_∞-ae²/R-b/R²(R=r_sN^1/3), which relates to the relationship of E_A vs. n, is put forward with considering the polarization, the d-s hybridization in the atoms(or molecules) and the screening effect on the surface. Then the EA values at the infinite size are close to the metal’s work functions, and an excellent fitness is obtained that the E_A values are accorded with E_A(R)=W_∞-ae²/R-b/R² well even in small size clusters. Meanwhile, the clusters which changed to the bulk metallic clusters are began at V₁₈ and Cr₂₁, and the structures of some abnormal clusters V₅, V₇, V₉, V₁₃, Cr₆, Cr₁₀ and Cr₁₇ are analyzed in detail.

Theoretical Studies on Electronic Structures and Catalytic Activities of Superoxide Dismutase Mimetics of Imidazolate-bridged Dinuclear Cu(Ⅱ) Complexes

LU Qing-Xia, TAN Hong-Wei, CHEN Guang-Ju*, WANG Yan*

2008, 29(8):  1635-1640.  doi:

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Electronic properties of superoxide dismutase(SOD) mimetics, the water-insoluble imidazolate-bridged dinuclear Cu(Ⅱ) complex, {[Cu(L)(H₂O)(β-CD)]₂(im)}³⁺, where L is 4-(4’-tert-butyl)benzyl-diethylenetriamine, β-CD is β-cyclodextrin and im is imidazolate, and its guanidinium-containing derivatives were studied with semi-expire PM3 and ab initio DFT/B3LYP methods. The analysis of charge distribution and bond characters for all studied systems were performed by using the Natural Bond Orbital(NBO) theory. The present calculated results show that the combination of the central Cu ion in the complex with water molecule is weak. It is possibly occurred that the water molecule is substituted by the superoxide radical anion in the catalytic reaction. β-Cyclodextrin linked to the guanidine causes more positive charge localizing at the central Cu cation of {[Cu(L)(H₂O)(β-GCD)]₂(im)}³⁺, which is favorable to catalyze the dismutation reaction. The combination of Cu ion in the complexes with the ligand N atom linked to two pentagons is much weaker than other ligands N atoms around the central Cu ion of these complexes. The structures of spin quimtuplet state of {[Cu(L)(OOH)(β-CD)]₂(im)}³⁺ and {[Cu(L)(OOH)(β-GCD)]₂(im)}⁵⁺ are more stable than those of spin singlet states of these complexes. Additionally, the imidazolate-bridge localized at the middle of two central Cu ions in these complexes is helpful to stabilize these mimetic complexes.

Forecasting for the Stable Isomers of [C,O,S] System

ZHOU Zhong-Jun, LIU Hui-Ling, HUANG Xu-Ri*, SUN Chia-Chung

2008, 29(8):  1641-1643.  doi:

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The singlet and triplet PESs of COS were investigated by DFT, QCISD, and CCSD(T) levels. At the QCISD level of theory, it is shown that a total of six minimum isomers are connected by four transitional states. Through an analysis of thermodynamic and kinetic stabilities, there is only a linear singlet isomer ¹1(O—C—S) located as the global state.

研究快报

Selective Deposition of Metal Patterns on Glass Based on Self-assembly and Inkjet Printing

WANG Jin-Yi¹, LIU Ran², CAI Wen-Bin¹*

2008, 29(8):  1644-1646.  doi:

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Selective metallization on glass is widely used in the production of printed circuit boards(PCB),display panels and solar cells. Selective masking and etching steps are used in the traditional photolithographic processes to create the regions of metallization on non-conducting substrates; however, these processes require high-cost facilities and complicated operations. To address these issues, a non-photolithographic process to form metal patterns on glass was proposed and put into practice, which combines self-assembly of aminosilane, desktop inkjet printing of a catalyst ink, and selective electroless plating of Au, Cu or Ni-B alloy on the catalyst template to form desired patterns with a minimal line width of about 200 μm. The adherence of the metal layer deposited on glass is significantly enhanced due to the surface modification of self-assembled aminosilane layer. The non-photolithographic approach could be cost-effective for prototype and small patch of production of metallic patterns, simple electric circuits and other electronic device parts.

Improving Quality of Microarray Chip Based on Superhydrophilic-Superhydrophobic Patterned Surface

YIN Qi-Ming, YE Jia-Ming, ZHOU Yong-Liang*

2008, 29(8):  1647-1649.  doi:

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Microarray chip including genechip has been of great application in fields of biology, quarantine, pharmacy and so on. Most of microarray chips were prepared by spotting aqueous droplet on the surface of substrate. Due to “coffee-ring stain effect”, there always was a denser perimeter where sample was concentrated during the process of droplet drying after spotting. So the ununiformity of spot caused by “coffee-ring stain effect” was one troublesome problem of the chip quality. Herein, superhydrophilic spot arrays on superhydrophobic AAO surface were fabricated to ease the “coffee-ring stain effect”. Furthermore, a protein array is prepared on this patterned surface where immunoreactions are carried out. As a result, spot uniformity is greatly improved in a wide range of concentration and volume.

研究论文

Synthesis and Micellization of Polyacrylamide/Poly(γ-benzyl-L-glutamate) Graft Copolymer

WU Qiu-Hua, WEI Tian-Zhu, LIANG Fang, SONG Xi-Ming, HAN Guang-Xi, ZHANG Guo-Lin*

2008, 29(8):  1650-1654.  doi:

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Polyacrylamide/poly(γ-benzyl-L-glutamate)(PAM-g-BLG) amphiphilic graft copolymers were synthesized by ring-opening polymerization of N-carboxy-γ-benzyl-L-glutamate anhydride(BLG-NCA) in N,N-dimethylformamide(DMF) initiated by polyacrylamide. The structure of the copolymers was determined via IR, ¹H NMR and GPC. The fluorescence technique was used to determine micellization and the critical micelle concentrations(CMC) of copolymer in water. The diameter and distribution of micelles were characte-rized by DLS and its shape was observed by TEM. The results show that BLG-NCA could be initiated by polyacrylamide to produce graft copolymer. The round nano-micells were formed by these copolymers in water. The CMC of copolymer solution and the size of micell were reduced with the increase of the proportion of hydrophobic parts.

PET Surface Chemistry Grafting Induced by 193 nm Laser

WU Gang¹*, WANG Ying-Jun¹, CHEN Xiao-Feng¹, YE Jian-Dong¹, WEI Kun¹, LEON Betty²

2008, 29(8):  1655-1659.  doi:

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Surface physical and chemical properties have very important impacts on biocompatibility of biopolymers. In this article, a 193nm excimer laser was used for the PET surface modification. The PET film was irradiated in a vacuum chamber filled with controlled ammonia flux. Surface roughness measurement, water contact angle, FTIR/ATR, XPS and Tof-SIMS were used to characterize the modified PET film surface. Water contact angle decreasing indicates that the chemical composition changed after laser irradiation in ammonia and no significant surface roughness was observed. The character amino group vibration absorption bands were displayed in FTIR/ATR spectrum at 3352 and 1613 cm^-1, respectively. XPS binding energies of C_1s at 285.5 eV and N_1s at 398.9 eV verified the C—N bond’s formation on the PET film surface. Fragment ions mapping in Tof-SIMS also shows that the proofs of amine molecule fragments could be extracted from the laser irradiated PET surface. All the results prove that the excimer laser can be used as a useful tool for the biopolymer surface modification and chemical patterning.

Preparation of Porous Magnetic Chitosan Microsphere via High Voltage Electrostatic Method

HU Qiao-Ling*, QU Jian, WANG Zheng-Ke, FEI Ruo-Chong, CHAI Fei-Ben, WU Jia, WANG You-Xiang

2008, 29(8):  1660-1664.  doi:

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Porous magnetic chitosan microspheres with average diameter about 600 μm were prepared by high voltage electrostatic method through mixing Fe₃O₄ particles into CS with silicagel as pore-forming agent and then adding them into thermal NaOH solution to get porous structure. This research studied the preparation technology , as well as the structure and morphology of microsphere with SEM, the results of which indicate that holes of porous magnetic chitosan microspheres with the size approximately 50 μm were uniformly dispersed in the microsphere when the mass volume fraction of chitosan acetic acid aqueous solution was 5% and m_S∶m_CS was 4∶1. Due to its large amount of hydroxyl groups and amino groups, porous magnetic chitosan microspheres could be widely used to deal with acidic dyestuff to improve environment and separated from dirty water by adding magnetic field.

Synthesis of α,β-Poly[(N-succinyl)-L-aspartamide] and in vitro Cytotoxicity of Its cis-Dichlorodiammine Platinum Macromolecular Prodrug

WANG Cheng-Yun, GONG Yan-Bao, LIU Shun-Ying, LUO Shu-Fang, HUANG Jing, YU Jia-Hui*

2008, 29(8):  1665-1670.  doi:

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It is reported that conjugated CDDP to polymer carriers can effectively reduce drug's cytotoxicity. In this paper, α,β-poly[(N-succinyl)-L-aspart amide](PSAA) was successfully synthesized via ring cleavage reaction of L-asprtic acid to polysuccinmide in a homogeneous system at room temperature, with the aid of water/triethylamine as a mixed solvent, and characterized by FTIR and ¹H NMR. The influence of volume ratios of water to triethylamine on the reaction was evaluated. PSAA-CDDP and PAsp-CDDP macromolecular prodrugs were prepared with conjugation of PSAA and α,β-poly(L-aspartic acid)(PAsp) with cis-dichlorodiammine platinum(CDDP), respectively. The results show that the cytotoxicity of PSAA or PAsp was rather low. The drugs could be released from PSAA-CDDP or PAsp-CDDP in a controllable manner. The in vitro cytotoxi-city of PSAA-CDDP or PAsp-CDDP against Bel-7402 cells increased with increasing dosage, but was lower than that of CDDP with the corresponding dosage. The cytotoxicity was ranked as PAsp-CDDP<PSAA-CDDP<CDDP.

Interaction of Copolymer-paclitexal Conjugate Micelles with C₆ Glioma Cells

WANG Zhan-Feng¹, LUO Yi-Nan¹, ZHENG Yong-Hui², HAN Hai-Ling³, HONG Xin-Yu¹, JING Xia-Bin²*

2008, 29(8):  1671-1676.  doi:

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Nanoscale micelles of poly(ethylene)-b-poly(lactic acid)/paclitexal conjugate(PEG-PLA/PTX) were prepared and their interaction with rat brain glioma C₆ cells was examined by MTT, electron microscopy, flow cytometry(FCM), and confocal laser scanning microscopy(CLSM). The results show that the copolymer/paclitaxel conjugate micelles can enter the cell, and are distributed in cytoplasm. The paclitaxel can be released from the conjugate micelles and react with the genes in the cell nuclei, causing changes in the gene molecules, and thus, leading to changes in growth cycle of the cells, resulting in G₂-M cell cycle arrest and inducing apoptosis of C₆ cells. Therefore, PEG-PLA/PTX micelles may be used in chemotherapy of brain glioma.

Preparation and Characterization of Absorptive Functional Fiber Copolymerized by n-Butyl Methacrylate with Hydroxyethyl Methacrylate

XU Nai-Ku¹, XIAO Chang-Fa¹*, FENG Yan²

2008, 29(8):  1677-1683.  doi:

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The attempt was made to prepare fiber which could absorb organic matter and to investigate its peculiarity. Firstly, resin was synthesized by the copolymerization of n-butyl methacrylate(BMA) and hydroxyethyl methacrylate(HEMA) when benzoyl peroxide(BPO) was used as an initiator, then crosslinking structure of copolymer was investigated by Fourier-transform infrared(FTIR) and nuclear magnetic resonance(NMR) spectrometer and the results show that chemical crosslinking structure was not formed between macromolecules, but intermolecular and intramolecular hydrogen bonding action existed so that physical crosslinking structure which located between molecules of copolymer was formed. Functional fiber to absorb low molecular weight organic matter was prepared by gelation-spinning and the effect of mass fraction of HEMA in monomer feed ratio on saturated absorbency was studied, it could be found from the result that not only toluene and trichloroe-thylene saturated absorbency increased with the increase of mass fraction of HEMA but also trichloroethylene saturated absorbency was higher than toluene saturated absorbency for fiber obtained by the same mass fraction of HEMA in monomer feed ratio. Crystallization behavior of fibers was analyzed by wide angle X-ray diffractometer(WAXD) and universal thermal gravimetric analyzer and the result indicates that as mass fraction of HEMA being enhanced, the crystallization ability was weakened. Finally, the result which was analyzed by scanning electron microscope(SEM) shows that mass fraction of HEMA had a great impact on the surface morphology of fibers.

Norbornene Polymerization Catalyzed by Bispyrazolylimineylimine Nickel(Ⅱ)/MAO Catalytic Systems

WANG Yuan-Yuan, ZHU Fang-Ming, LIN Shang-An*

2008, 29(8):  1684-1688.  doi:

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Two bispyrazolylimine nickel complexes[bis-N-(phenyl-1,3,5-dimethylpyrazolylmethylene)phenylimine nickel dibromide] (Cat.1) and [bis-4-methoxy-N-(phenyl-1,3,5-dimethylpyrazolylmethylene) phenylimine nickel dibromide](Cat.2) were synthesized. Norbornene polymerization catalyzed by Cat.1/MAO and Cat.2/MAO systems was investigated. The catalytic efficiency, molecular weight and molecular weight distribution were influenced by the polymerization conditions, such as the polymerization temperature, Al/Ni molar ratio and catalyst concentration. The results show that Cat.1/MAO and Cat.2/MAO systems displayed a high catalytic efficiency with 10⁵ g PNBE/(mol Ni) magnitude order. The molecular weights of PNBE were higher than 10⁵ and the molecular weight distributions were around 2. According to ¹H NMR and the FTIR spectra, the mechanism of the norbornene polymerization is vinyl-addition type polymerization.

Notroxide Mediated Radical Polymerization of Styrene Irradiated by TEMPO with UV Light

HUANG Jian-Ying¹*, ZOU You-Si²

2008, 29(8):  1689-1693.  doi:

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Nitroxide mediated radical polymerization(NMRP) was employed to synthesize polystyrene in the presence of TEMPO irradiated with UV light at 50 ℃. The polymerization exhibited the characteristic of a controlled polymerization. In comparison with the thermal-initiated polymerization, the condition of UV-irradiated polymerization is milder and the rate is faster. The photopolymerization can be realized at 50 ℃ and the conversion can reach 99% within 10 h. The influence of concentration of photo-initiator and light intensity was discussed. The molecular weight can be controlled in the range of 3×10⁴—1×10⁵ and the higher light intensity is good for controlling the polymerization.

Fabrication of Protein Microcapsules by Controlled Precipitation and Cross-linking

TONG Wei-Jun, ZHU Yi, GAO Chang-You*

2008, 29(8):  1694-1697.  doi:

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Bovine serum albumin(BSA) microcapsules, which have a uniform shape and size and can be well dispersed in water, were fabricated by the controlled precipitation of BSA on the surface of MnCO₃ microparticles though desolvation, followed by cross-linking and core removal. The thickness of the capsule walls were controlled by the amount of the added non-solvent(ethanol). The as-prepared microcapsules are permeable to TRITC-dextran with a molecular weight of 70000, but not up to 155000, implying that the pore size in the capsule walls is between 18.5—26.2 nm. Due to the excessive carboxylic groups on the BSA molecules, which can be fully charged at an alkaline condition, the BSA capsules expanded their size at pH>10. This method is applicable to other proteins and enzymes as well, and the pH-sensitive protein capsules may find potential applications in biomedical field because of their biodegradability and biocompatibility.

Arrangement of Fluorine-containing Group Side Chains on the Latex Film Surface

QIN Zong-Gen¹* , TU Wei-Ping²

2008, 29(8):  1698-1702.  doi:

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The self-crosslinking fluorine-containing latex film was attributed and characterized with Static Contact Angle Instrument and X-ray Photoelectron Spectrum(XPS), and then the surface free energy of the latex film was calculated by the use of experimentation and group contribution method respectively. The purpose is to examine the arrangement of fluorine-containing group side chains on the latex film surface. The results show that the surface free energy of the latex film can be decreased along with increase of fluorine-containing monomer amount when its amount is below 20.3％, but that when above 20.3％, variation of surface free energy of the latex film is less and the fluorine-containing latex film has a strong self-recovery capability. Further studies on the film surface show that the arrangement of fluorine-containing group side chains on the latex film surface is random and irregular.

Photochemical Synthesis and Characterization of Polyethyleneimine-coated Magnetic Nanogel Used as Cancer-targeted Carrier

LIU Hong-Ling¹*, LI Jun²

2008, 29(8):  1703-1706.  doi:

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The polyethyleneimine(PEI)-coated magnetic nanogel was synthesized via photochemical polymerization under UV-light irradiation. Modified with folic acid, which was expected to be able to identify tumor surface receptors and to have a high binding force with cancer cells, the FA-PEI-Fe₃O₄ nanogel was prepared. The FA-PEI-Fe₃O₄ nanogel was characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, scan electron microscope and vibrating sample magnetometer, respectively. The results showed that the magnetic nanogel was regular shape with a mean diameter of 140 nm. With high saturation magnetization and folate modification, the FA-PEI-Fe₃O₄ nanogel suggests promising potential application in cancer-targeted drug delivery.