Table of Content

10 January 2007, Volume 28 Issue 1

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目次

高等学校化学学报2007年第28卷第1期目次

2007, 28(1):  0.  doi:

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研究论文

Preparation of Monodisperse Nanocrystalline Barium Titanate

CUI Bin^1,2, WANG Xun¹, LI Ya-Dong¹

2007, 28(1):  1-5.  doi:

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Monodisperse cubic BaTiO₃ nanocrystallines coated by oleic acid were synthesized through solvothermal method, and the average size of the nanoparticals was 6.0 nm. The microstructure of BaTiO₃ nanocrystallines was characterized by the techniques of XRD and TEM, while the effects of the length of alcohol chain, the content of oleic acid and heat treatment temperature on the phase composition and morphology of BaTiO₃ were also investigated. The result shows that the as-prepared nanoparticals have small size, narrow size distribution and good monodispersity, and the surfaces of which are nonpolar and can be dissolved in nonpolar solvent. Because the surfaces of nanocrystallines are coated by oleophilic long alkyl chain, they are incompatible with water surroundings to form some repulsion. With the coaction of gravity and repulsion, nanocrystallines can be separated effectively from liquid phase environment.

Preparation and Characterization of Layered Zirconium Phosphates Based on Water-in-oil Microemulsion

TANG Kang-Jian, YIN Zhi-Lei, CAO Xue-Jing, YU Ji-Hong, XU Ru-Ren

2007, 28(1):  6-9.  doi:

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Layered zirconium phosphates[Zr(HPO₄)₂·H₂O, (H₃O)⁺Zr₂(PO₄)₃ and Zr(HPO₄)₈·H₂O] were synthesized in water/oil(W/O) microemulsion system containing heptane, CTAB/butanol and water water. X-ray diffraction(XRD), transmission electron microscopy(TEM) and scanning electron microscopy(SEM) were utilized to characterize the structure, morphology and size. It was found that the preparation of zirconium phosphate in W/O microemulsion could control structure based on the microemulsion composition(i.e. three layered zirconium phosphates obtained with different ratio of water and oil) and morphology based on the reacted conditions(i.e. the size and morphology of α-zirconium phosphate can be controlled with different reacted time and temperature in microemulsion). We believe that the simple synthetic method based on microemusion would benefit the controllable synthesis of zirconium phosphates greatly.

Photochemical Synthesis and the Seeding-mediated Growth of Gold Nanoparticles Under the Sunlight Radiation

WU Hong-Cheng, DONG Shou-An, DONG Ying-Nan, TANG Chun, YANG Sheng-Chun

2007, 28(1):  10-15.  doi:

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In the aqueous citrate-chloroauric acid solution, well-dispersed gold nanoparticles were synthesized by the photochemical reduction under the UV solar radiation on plateau. The influences of the pH of the mixture solution and the UV solar radiation conditions on the photochemical reaction rate and the size of gold nanoparticles were investigated. By means of seeding-mediated growth approach, monodispersed spherical gold nanoparticles with an average diameter from 4.9 nm to 9.7 nm and with a narrow size distribution were obtained by varying the ratio of Au(0) seed to Au(Ⅲ) ion under suitable conditions. Based on the charac-terization by UV-Vis adsorption spectrum and transmission electron microscope(TEM), the mechanisms of the freedom radical reaction, the nucleation and growth during the formation process of the gold particles were discussed.


Preparation and Oxygen Sensing Properties of Hybrid Materials Based on a Covalently Grafted Ruthenium(Ⅱ) Complex

ZHANG Hao-Ran¹, BAI Yan³, LI Bin², LEI Bing-Fu², FU Chun-Yan¹

2007, 28(1):  16-20.  doi:

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The preparation and oxygen sensing properties of mesoporous materials DWM with a structure similar to that of MSU-type mesoporous materials based on covalently grafted Ru(bpy)²⁺₃ fragments through the Si—CH₂ covalent bonds were described in this paper. The 2,2'-bipyridyl covalently grafted to 3-aminopropyltriethoxysilane was used as one of the sol-gel precursor and the ligand of Ru(bpy)₂Cl₂·2H₂O complex to prepare the sol-gel derived silicates. The luminescence of the covalently grafted Ru(Ⅱ) luminophore within the mesoporous matrix can be extremely quenched by oxygen with a good sensitivity and rapid response time, which suggests that the covalently grafting strategy presented in this paper can be used to develop superior oxygen sensor. In addition, the mesoporous structure possesses a higher sensitivity than that of the amorphous one due to the inner porous channels of the mesoporous matrix favor the diffusion of oxygen, resulting in the higher sensitivity and shorter response time. Furthermore, the covalently grafting method possesses the distinct advantages over those physically entrapped methods due to the Si—CH₂ covalent bond, which greatly minimized the dye leaching effect and ensure the good stability.

Fast Crystallization of LTA Zeolite from Highly Efficient NaY Seed Solution

XIONG Xiao-Yun¹, FAN Feng-Tao², MA Jun³, LI Cai-Jin¹, LIU Shu-Zhen¹, FENG Zhao-Chi², LIANG De-Sheng¹, LI Shou-Gui¹, XIAO Feng-Shou¹

2007, 28(1):  21-25.  doi:

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A new route for fast crystallization of LTA zeolite by using highly efficient NaY seed solution as a silica source was demostrated. Compared with water glass, NaY seed solution used in the synthesis of LTA zeolite shows obvious advantages including relatively short crystallization time, low crystallization temperature, small crystal size and low alkalinity. Characterization of NaY seed solution by ²⁹Si NMR and UV Raman techniques suggests that zeolite primary building units such as six-membered ring contained in NaY seed solution possibly promote the nucleation and growth of LTA zeolite.

研究简报

Preparation and Bacterial Separation Function of Norvancomycin Hydrochloride-immobilized Magnetic Nanoparticles

KE Shi-Jian, JI Jian

2007, 28(1):  26-28.  doi:

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APTES-bounded MNP were prepared by chemical coprecipitation, followed by coating with (γ-aminopropyl)triethoxysilane. Norvancomycin hydrochloride(Van) was then immobilized onto the amino-functionalized nanopartiles. Powder X-ray diffraction(XRD) results show the inverse spinel structure of MNP. The physics property measurement system(PPMS) indicates that the MNP are superparamagnetic. The presence of Van and APTES on the surface of MNP is confirmed by FTIR. By a separation assay of S. aureus and E. coli BL21, it is proved that MNP-APTES-Van can selectively capture S. aureus within 10 min, which can be isolated readily by applying an external magnetic field.

研究论文

Nanoliter-scale Etched Capillary Electrospray Interface of Mass Spectrometry

DUAN Ji-Cheng, LIU He-Chun, LIANG Zhen, ZHANG Wei-Bing, ZHANG Li-Hua, ZHANG Yu-Kui

2007, 28(1):  29-33.  doi:

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A nanoliter-scale electrospray interface for mass spectrometry was developed by modifying the commercial sheathflow interface for capillary electrophoresis coupling with mass spectrometry(CE-MS). The interface was fabricated by using HF etching on a 50 μm i.d. fused-silica capillary. The outer wall of the interface was shown a porous structure, and its thickness was as thin as about 10 μm. A protein sample, cytochrome c, was analyzed by using the etched interface at the volumetric flow rate as low as 20 nL/min. The influence of contacting electrolyte between the etched capillary and the stainless steel sheath tube on ESI was investigated and explained. The comparative study of electrospray performance of the commercial micro stainless steel interface and the etched one was carried out by using protein as sample. The higher response signal was achieved by using the modified interface in the flow rate range of 50—500 nL/min. The sensitivity of detection was increased 3.6 times at the flow rate of 200 nL/min compared with the commercial micro interface.

Predictive Studies on Interaction Between DNA and Target Molecules

WANG Lan, GENG Zai-Xin, LU Xiao-Quan, LIU Hong-De, WANG Rui, CHEN Jing

2007, 28(1):  34-39.  doi:

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On the basis of the quantified data of molecular structures and the experimental results, the pattern recognition techniques, multiple linear regression and artificial neural network were applied to studying the main influencing factors for the interaction between DNA and the target molecules, and two predictable models of binding constant and one binding mode which have a high accurate were established. First, 21 structural descriptors(parameters) were used to describe a target molecule. After filtering, 10 descriptors were found to affect remarkably the interaction between the target molecules and DNA. These studies could afford valuable information to design and filter molecules of anticancer drugs.

Correlation Analysis of Relationships Among Structure, Function and Evolution of Proteins Based on Discrete Wavelet Transform

QIU Jian-Ding¹, LIANG Ru-Ping¹, MO Jin-Yuan²

2007, 28(1):  40-45.  doi:

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A new method based on the combination of the discrete wavelet transform(DWT) and cross-covariance, named as sequence wavelet hiberarchy correlation method(SWHCM), is presented which reveals the relationship among the structure, function and evolution of proteins via the hydrophobic character of amino acids. The trypsin proteins of different species were chosen as the examples to describe the application of this method to revealing the evolution relationship according to the evolution vectors. The protein phosphatase, hemoglobin and lysozome were chosen as the examples to describe the intrinsic function-sequence relationship according to the function vectors by using this method. We can draw a conclusion that our non-parametric method is simple, visual and performs reasonably well without knowing the structure of proteins in advance, which is a promising approach to revealing the relationship between two compared proteins at different spatial resolutions.

Chirality Molecules and Chiral Topological Indices

WANG Jun, XU Lu

2007, 28(1):  46-48.  doi:

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In this paper, the symmetry of 28 racemoids(unusual amino acids), such as symmetrical face, symmetrical node and axis, were recognized by using expert system of structure elucidation of organic compound, and the configurations of those compounds were recognized by using the program developed by our laboratory. On the basis, with chiral topological indices, the elution order with HPLC were performed by using Fisher analysis and artificial neural network for enantiomers of these compounds. Artificial neural network gave out a better result than that obtained by using Fisher analysis.

Electrochemical Studies on Interaction Between Dinuclear Copper(Ⅱ) Complex Containing Dimethylglyoxime and DNA

XU Gui-Yun^1,2, JIAO Kui², LI Yan-Tuan³, REN Yong², ZHANG Xu-Zhi²

2007, 28(1):  49-52.  doi:

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Cyclic voltammetry was used to study the interaction between dinuclear copper(Ⅱ) complex containing dimethylglyoxime[Cu₂(Hdmg)₄] and DNA. The influences of pH, temperature, ionic strength and concentration of Cu₂(Hdmg)₄ on the interaction were described, and the mechanism of the interaction was also discussed. The result shows that Cu₂(Hdmg)₄ can interact with the bases of DNA to form non-electroactive complex, which can decrease the anodic peak current of Cu₂(Hdmg)₄. The interaction between Cu₂(Hdmg)₄ and ssDNA is stranger than that between Cu₂(Hdmg)₄ and dsDNA because of the exposed bases of ssDNA. The combining ratios of Cu₂(Hdmg)₄ to ssDNA and to dsDNA are 2:1 and 1:1, and the combining constants 3.56×10⁹ and 2.75×10⁵, respectively.

研究简报

Determination of Multiple Trace Elements in Seawater Using Chelation Ion Chromatography and ICP-MS

LIU Gang^1,2, ZHONG Shao-Jun¹, QU Chen-Li^1,2, LIU Fei¹, XU Li-Jun¹

2007, 28(1):  53-55.  doi:

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An off-line chelation system combined with ICP-MS technique was developed for the quantitative determination of trace elements in seawater, namely V, Co, Ni, Cu, Zn, Mo, Cd, Pb, U and rare earth elements(REEs). The system was built based on an ion chromatography equipped with MetPac® CC-1 chelation columns which had a strong selective chelation to these target elements within a pH range 5.2—5.6. Acidified seawater samples and NH₄Ac(2 mol/L) were blended to meet suitable pH before being injected into the chelation column, thus target elements were retained while alkali and alkaline metals were excluded. Then chelated elements were eluted by HNO₃(1 mol/L) and samples were collected for ICP-MS analysis. Varying the ratio of input(gen. 200 mL) to output(gen. 5 mL), the target elements which were concentrated as 40 times as their concentrations were far beyond instrumental quantification limits. At last, a certificated seawater CASS-4 was introduced and our detected values were in good agreement with those certified values.

Preparation of Isoquinolinecarboxylic Acid Derivative as Brush-type Chiral Stationary Phase and Its Application in the Enantiomeric Resolutions of Binaphthol Derivatives

SONG Rui-Juan^1,2, GUO Ying^1,2, FU Yu^1,2, SHI Hong-Yu^1,2, LONG Yuan-De¹, HUANG Tian-Bao¹

2007, 28(1):  56-58.  doi:

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A novel chiral stationary phase(CSP) for HPLC was prepared by synthesizing 3,5-dinitrobenzoyl-(S)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid as chiral selector and bonding it with 3-aminopropylsilane modified silica. The resolutions of 8 enantiomers of binaphthol and its derivatives were achieved by using hexane-ethanol-acetic acid(98:2:0.5, volume ratio) as mobile phase with a column temperature 30 ℃ and detected at ultraviolet 254 nm. The effects of acetic acid and alcohol organic modifiers on retention and resolutions of the analytes were examined. The enantioselectivities α of the analytes on CSP could be improved by adding acetic acid to mobile phase due to masking effect of H⁺ on the residing silanol and amino group.

Microfluidic Cell Separation Chips Based on Crossflow Filtration

CHEN Xing, CUI Da-Fu, LIU Chang-Chun, LI Hui, GENG Zhao-Xin

2007, 28(1):  59-61.  doi:

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In this work, two kinds of novel microfluidic cells separation chips were described on the principle of crossflow filtration by using micro-electro mechanical systems(MEMS) technology. Whole blood is a complex mixture of various cells, such as red blood cells(RBC), white blood cells(WBC) and so on. Separation and collection of different kinds of cells is the required first step for the subsequent clinical and basic research assays. One-level filtration microfluidic chips with three coiled channels spaced by two arrays of parallel microfabricated filtration barriers of post-type or dam-type along the stream, were successfully used to separate and collect RBC and WBC from whole blood via their different sizes. The effects of the dilution times and the length of separation channels with different filtration barriers on RBC separation efficiency were investigated. When the whole blood was diluted by 50 times, the RBC separation efficiency was 91.2% and the WBC separation efficiency was 27.4% by using the microfluidic chip with dam-type filtration barriers of 160 mm long. The WBC separation efficiency was two times more than that by using microfluidic chip based on the dead-end filtration principle. The second kind of microfluidic chip had multilevel filtration barriers of post-type which was used to separate and collect plasma, RBC and WBC from whole blood.

On-line Sweeping Determination of Quinolones in Pork Tissue by Micellar Capillary Electrophoresis

ZHAO Yan-Yan^1,2, WANG Li-Juan¹, LI Yue-Qiu², HAN Yuan-Yuan², DU Guang-Ling²

2007, 28(1):  62-64.  doi:

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A micellar capillary electrophoresis(MCE) method based on on-line sweeping technique was developed for a determination of trace quinolones, ciprofloxacin ofloxacin and enrofloxacin in pork tissue. The pork tissue samples were deproteinized with trichloroacetic acid and in the running buffer of 20 mmol/L Na₂B₄O₇+80 mmol/L sodium dodecyl sulfate(SDS), pH=9.6, the ciprofloxacin, ofloxacin and enrofloxacin in the sample were successfully separated and detected within 200 s, in a non-coating fused-silica capillary column(48.5 cm×75 μm i.d., effective length 40 cm) at separation voltage of 18 kV, and the injection pressure of 15×10² Pa, with UV detection at 278 nm. The detection limits of ciprofloxacin, ofloxacin and enrofloxacin were 0.007, 0.016 and 0.020 mg/L, and RSD were 2.0%, 2.4% and 2.6%, respectively. This method allows of up to 600-fold accumulation concentration of ciprofloxacin and can be used to separate and detect the residuals of trace medicines in animal food.

研究论文

Synthesis of Arylenealkyne Conjugated Macrocycles Containing Long Alkylene Bridge

CHENG Xiao-Hong¹, Hoeger Sigurd²

2007, 28(1):  65-70.  doi:

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The synthesis of the first two arylenealkyne conjugated macrocycles containing long alkylene bridge via Glaser coupling of template-directed tetraacetylenes was reported. Tetraacetylenes intermediates with complex structures were constructed rapidly via quadruple Hagihara coupling of monoprotected bisacetylenes to appropriate tetraiodides and subsequent desilylation. The characterization of such compounds was carried out by NMR, GPC and UV-Vis spectra. Unfortunately the two compounds were not liquid crystals, without biaxial nematic mesophase characterc as expected.

Assembly of Luminescent Palladium(Ⅱ) Carbazyl Substituted Porphyrin Complexes with Mesoporous Silica MCM-48 and Oxygen Sensing Properties

HUO Cheng, ZHANG Hong-Yu, ZHANG Ping, SONG Wei-Feng, ZHANG Hui-Dong, WANG Yue

2007, 28(1):  71-74.  doi:

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A series of palladium meso-tetrakis[3-methoxy-4-(N-carbazyl)n-alkyloxyphenyl]porphyrin(Pd-4Cn-TPP, n=4, 6, 8) were synthesized. Pd-4C4-TPP, Pd-4C6-TPP and Pd-4C8-TPP exhibit similar luminescent properties in solution and solid state. Three protonated palladium(Ⅱ) porphyrins Pd-4Cn-TPP⁴⁺ are assembled with mesoporous silica MCM-48, respectively, resulting in the assembly materials Pd-4Cn-TPP⁴⁺/MCM-48(n=4, 6, 8). The luminescence of Pd-4Cn-TPP⁴⁺/MCM-48 can be extremely quenched by molecular oxygen. Even the volume fraction of oxygen is 0.1%, the luminescence intensity of Pd-4Cn-TPP⁴⁺/MCM-48 can be quenched over 50%. The high sensitivity(I₀/I₁₀₀>38) and rapid response time(t_↓≤0.08 s) were achieved.

Purification and Properties of a Novel Se-containing Protein from Se-enriched Ganoderma lucidum and Its Antioxidant Activity

DU Ming^1,2, ZHAO Lei¹, LI Chao-Rui¹, ZHAO Guang-Hua¹, HU Xiao-Song¹

2007, 28(1):  75-78.  doi:

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A novel water-soluble fungi Se-containing protein, named as Se-GL-P, was purified for the first time from Se-enriched GL to establish the relationship between the antioxidant activity of protein and its Se content. This protein was isolated and purified to homogeneity by using ammonium sulfate precipitation followed by two consecutive anion exchange chromatography and size exclusion chromatography. This protein in its native state was identified as a monomer of 36600 estimated by 19.8% weight carbohydrate. The protein is acidic and the N-terminal shows a sequence of DINGGGATLPQKLYLTPDVL, suggesting that this protein belongs to a family of DING protein. The Se content of this protein is 4.87 mg/g protein, and the protein has stronger scavenging activities on superoxide and hydroxyl radicals. It is found that the increasing antioxidant property of this protein depends quantitatively on the increase of its Se content.

Design and Synthesis of a Novel Fluorescent Peptide Substrate of SARS-CoⅤ 3CL^pro and Studies on Its Enzymatic Kinetics

WAN Hui-Xin, CHEN Li-Li, LI Xin, WANG Xin, HU Ding-Yu, SHEN Xu, SHEN Jing-Kang

2007, 28(1):  79-82.  doi:

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A novel fluorescent peptide substrate, H₂N-E(Eddnp) STLQSGLK(Abz)-CONH₂, based on fluorescence resonance energy transfer(FRET) technique, was designed and synthesized by solid-phase peptide synthesis. Abz/Eddnp was used as the fluorescence donor and quenching pair. The highly fluorescent Abz group was efficiently quenched by energy transfer to the Eddnp group. The fluorescent substrate was specifically hydrolyzed by SARS-CoⅤ 3CL^pro between QS with 15-fold increase in fluorescence and the cleavage site was determined by HPLC-MS. The studies on its enzymatic kinetics(K_m= 525.5 μmol/L and K_cat=1.29 min^-1) elucidate that the synthetic fluorescent peptide substrate is suited to be used as a fluorescent probe in determination of the activity of SARS-CoⅤ 3CL^pro and screening assays for its inhibitors.


Anion Recognition of 2-(2'-Hydroxy-3-methoxy phenyl)-5,6-dinitrobenzimidazole

YU Ming¹, LIN Hai², LIN Hua-Kuan¹

2007, 28(1):  83-86.  doi:

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The design and synthesis of functionalized receptors for the development of potential chemosensors is an increasingly topical field in anion recognition chemistry. The incorporation of chromophores into the receptor, which are sensitive to the interactions between the host and guest molecules, has recently gained considerable attention due to their low detection limit. In this article a benzimidazole-based anion receptor 1 was designed and synthesized. The structure of compound 1 was confirmed through single crystal X-ray diffraction analysis. Anion binding studies carried out by using ¹H NMR and UV-Visible reveal that this compound exhibited the recognition towards AcO^-, H₂PO₄^-, OH^- in DMSO solutions. Receptor 1 showed dramatic color changes from light-yellow to red in the presence of AcO^-, H₂PO₄^-, OH^-. The intermolecular interactions between compound 1 and anions could be easily monitored by anion complexation-induced changes in UV-Vis absorption and by the “naked eye”.

Preparation and Structure Characterization of an Alkali-soluble Polysaccharide from Grifola frondosa Mycelium

YU Guang-Li, WANG Ying, ZHAO Xia, GAO Hao-Dong, GUAN Hua-Shi

2007, 28(1):  87-91.  doi:

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An alkali-soluble polysaccharide(GFM2A)was extracted by cold sodium hydroxide and further purified by column chromatography from fermented Grifola frondosa mycelium. The structural characterization of GFM2A was confirmed by NaIO₄ oxidation, Smith degradation, acetolysis, GCMS, IR and NMR techniques. The results showed that GFMZA contain glucose(Glc),mannose(Man)and xylose(Xyl), and their molar ratio was 9∶2∶1. There are six α-1,3-D-Glc and two α-1,3-D-Man in the backbone, and there are two branches in the main chain, and both of them linked to α-1,3-D-Glc residue, one branch contains three β-1,4-D-Glc, another branch contains one α-1,4-D-Xyl.

Characterization of Linear Epitope of the β₂-Microglobulin via Combination of MALDI-TOF-MS with Immunoaffinity

LI Gen^1,2, LIU Ning¹, LIU Zhi-Qiang¹, LIU Shu-Ying¹

2007, 28(1):  92-96.  doi:

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Matrix-assisted laser desorption ionization time-of-flight mass spectrometry(MALDI-TOF-MS), in combination with immunoaffinity provided a powerful tool for determining epitope(antigenic determinant) in protein. The linear epitope of the β₂-microglobulin was characterized in the paper. The method as follows: at first β₂-microglobulin was digested by a proteolytic enzyme to produce an appropriate set of peptide fragments, then peptide fragments containing the linear epitope were selected and separated from the pool of peptide fragments by immunoprecipitation with the monoclonal antibody. The agarose beads were collected carefully after the reaction. Unbound peptides would be washed away, while the peptides containing the epitope would remain bound to the immobilized antibody after the beads were washed several times with appropriate buffer. At last the masses of the bound peptides were identified directly by MALDI-TOF MS. Using Endoproteinase Glu-C Endoproteinase Lys-C and Trypsin in the experiment, the linear epitope of β₂-microglobulin was located within peptide fragment 59—69, that is, DWSFYLLYYTE.


研究简报

Determineation of DNA Cleavage Site Sequence Using Fluorescence Labeled Primer and DNA Sequencer

ZHENG Wei-Juan¹, CHEN Yuan¹, SHAO Ying², TANG Zhong-Hua³, GUO Zi-Jian², HUA Zi-Chun¹

2007, 28(1):  97-99.  doi:

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Determining the base sequence of DNA broken site is quite crucial for the study on the cleavage site specificity and mechanism of various natural or synthetic DNA cleavage regents, and on developing novel therapeutic drugs targeting at DNA. The most frequently used method depending on chemical reactions of the Maxam-Gilbert procedure, and the late arising methods used by Rui Ren et al. which were based on Sanger's DNA sequencing strategy, all had some deficiencies, either the pollution of radioactive materials, or really complicated and difficult to operate. In the present paper, a new method for DNA cleavage site sequence determination was developed. The fluorescence FAM-labeled primer was annealed to the DNA fragments, which has been cleaved by restriction enzymes or other regents, and extended along the template sequence. The products then loaded onto the polyacrylamide electrophoresis gel of ABI 377 DNA Sequencer. Data was collected and analyzed by using ABI PRISM Data Collection Software and ABI PRISM Sequencing Analysis Software. It is proved to be a credible and simple new approach to determine the base sequence of DNA broken sites.

研究论文

New Diterpenoid Compound from Rabdosia macrocalyx


SHI Hao¹, HE Shan¹, HE Lan², PAN Yuan-Jiang¹

2007, 28(1):  100-102.  doi:

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On the basis of the investigation on natural product antitumor agents, a new diterpenoid named macrocalyxin J was isolated from the leaves of Rabdosia macrocalyx(Dunn) Hara by silica gel column chromatography. Based on IR, MS, ¹H NMR, ¹³C NMR and 2D NMR spectroscopies, the structure of macrocalyxin J was determined as (1α,6β,11β,14α)-1,7∶6,20-diepoxy-6,11-dihydroxy-6,7-seco-ent-kaur-16-ene-7,15-dione-14-acetate. The antitumor activity of the compound was assayed by MTT method. Macrocalyxin J was shown to have a potency in vitro against the cultures of Hela cells.

研究简报

Tryptophan Modification and Fluorescence Spectrum of Inulinase

LIU Xian, GAO Guo-Fen, YANG Li, HE Xiao-Xiao, MENG Zhe, TENG Li-Rong

2007, 28(1):  103-105.  doi:

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Tryptophan(Trp) residues in inulinase were modified by chemical reagent N-bromossuccinimide(NBS). The results of Spande's method indicate that there were seventeen Trp residues in inulinase and five of them were located on the surface of the enzyme. Three of these Trp residues were none-essential residues which showed the fastest rate by Zhou's plot. Two relative faster reacting residues were both essential for the activity of the enzyme. The other twelve were the slowest or none-reactive residues for the reaction. The study on fluorescence quenching of inulinase shows that KI could not quench all of the fluorescence from Trp residues in inulinase which indicate that there are two kinds of Trp residues in inulinase acrylamide(Acr), a polarized quencher without electronic charge could quench almost all of the fluorescence from Trp residues in inuoinase while there are still seventy percernt of the activity of the enzyme left. The collisional quenching constants(K_D) of inulinase at different concentrations of Acr were calculated in terms of Stern-Volmer equation.

Synthesis and Electrochemical Properties of Lithium Bis(heptafluoroisopropyl)tetrafluorophosphate

GUO Ai-Hong^1,2, BI Cheng-Liang^1,3, JIAO Li-Fang³, ZHANG Bao-Gui¹

2007, 28(1):  106-108.  doi:

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Lithium-ion secondary cell has a high energy desity, stable and high working voltage, wide working temperature and long working term. It is a safe and clean energy resource without pollution. At present, lithium hexafluorophosphate is used as a conducting electrolyte lithium salt in lithium-ion secondary batteries. But lithium hexafluorophosphate as conducting electrolyte lithium salt has some disadvantages such as hydrolysis and instability. Lithium bis(heptafluoroisopropyl) tetrafluorophosphate Li[(C₃F₇)₂PF₄] was received by Simons process from diisopropylchlorophosphane in this paper. As an electrolyte of Li ion secondary cell, Li[(C₃F₇)₂PF₄] had lower vapor pressure than LiPF₆ in the solvent at the same temperature, comparable conductivity and oxidation stability in the same concentration at room temperature. It was worth mentioning that Li[(C₃F₇)₂PF₄] has an excellent stability towards hydrolysis. The synthesis process is safe and easily controlled.

研究论文

Synthesis of Polypyrrole and Electrochemical Performance of Doual-ion Battery

XIE Hai-Ming^1,2, HAN Ming-Juan¹, YU Hai-Ying¹, YANG Gui-Ling¹, CHU Ying¹, WANG Rong-Shun¹

2007, 28(1):  109-112.  doi:

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Conducting DBSA-PPy was fabricated by reverse microemulsion polymerization. DBSA increase the conductivity of PPy when it is used as the dopant and was surfactant, since the W/O microemusion can supply nano-reactor. The electrochemical performance of dual ion battery with graphite as the anode and DBSA-PPy as the cathode materials was tested, the result shows that the battery has as good electrochemical characteristics as traditional lithium-ion battery, due to the high conductivity and doped structure of the prepared DBSA-PPy, which indicates that conducting polymer as positive materials of electrode is hopeful for the application.

Constant Temperature Oxidation Behavior of a High-temperature-cast Ni-base Superalloy K52 at 900 ℃


LI Yun^1,2,3, XU Ning¹, GUO Jian-Ting², YUAN Chao², YANG Hong-Cai³

2007, 28(1):  113-116.  doi:

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The isothermal oxidation behavior of a cast Ni-base superalloy K52 at 900 ℃, which compared with Ni-base superalloy ЧC104-Bи, was investigated. The bases of the experiment and theory were provided for designing and applying superalloy K52. The results indicate that oxidation kinetics obeyed parabolic law for the two kinds of superalloys. The resistance oxidation belongs to Ⅰgrade for K52 and ЧC104-Bи superalloys at 900 ℃.The scales on the surface were determined by X-ray diffraction, scanning electron microscopy(SEM), and EPMA equipped with an EDAX unit. The results show that oxidation scales of K52 superalloy is similar to that of ЧC104-Bи one, and the oxidation scales consisted of three parts: which the external layer without protective discrete is mainly formed with TiO₂, and a protective continuous compact Cr₂O₃ layer with a certain amount of NiCr₂O₄ is intermediate layer, as well as the internal layer is mainly Al₂O₃ with a small amount of TiO₂. The oxidation resistance of the superalloy K52 is superior to that of the superalloy ЧC104-Bи.

QSAR Study of Acute Toxicities of Phenylsulfonyl Carboxylate Compounds

LI Ji-Lai¹, HANG Ye-Chao², GENG Cai-Yun¹, HUANG Xu-Ri¹, LI Fang-Shi², SUN Chia-Chung¹

2007, 28(1):  117-120.  doi:

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Based on the theoretical linear solvation energy relationship(LSER) parameters, a new QSAR model was established to correlate the acute toxicities of 56 phenylsulfonyl carboxylate compounds. All the descriptors were derived from quantum chemical computation at B3LYP/6-31G(d) level of theory. Compared with the model from TLSER, the new model has a better expression and prediction because more samples have been used. The model is shown below and its adequacy is R=0.94, R²_adj=0.88, F=61.62, q²=0.83.
-lgEC₅₀=a×E_HOMO+b×P+c×q₁₀+d×q₁+e×μ+f×q_H+costant
The computation results show that the smaller of the hydrophilicity of the substituent at the ester group, the bigger the acute toxicity; the bigger the hydrophilicity of the substitute attached to the benzene ring, the bigger the acute toxicity; the bigger the volume of the molecule, the smaller the toxicity; the bigger the ability of the molecule to form H-bonding, the smaller the toxicity; the higher the energy of HOMO, the bigger the toxicity. The present study may be helpful for probing the mechanism of action in acute toxicity of phenylsulfonyl carboxylate compounds and understanding the phenylsulfonyl carboxylate chemistry.


SERS Spectroscopy Studies on the Self-assembled Films of Metalloporphyrin Based Axial Ligation

CHENG Yu-Chuan, WANG Yun-Xin, SONG Wei, YU Miao, XU Wei-Qing, ZHAO Bing

2007, 28(1):  121-124.  doi:

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We select a [5-para-alkyloxyphenyl-10, 15, 20-tri(m-ethoxyphenyl)]porphyrin hydroxy rare earth complexes(HoOH) and 4, 4'-bipyridine(44BPY) as the blocking units, and successfully assemble a HoOH monolayer on the 44BPY-modified silver surface based on axial ligation. The structure and orientation of the SAMs were studied by UV-Vis and SERS spectroscopy. The results reveal that 44BPY is assembled onto the silver surface with an end-on adsorption via 4-position nitrogen. The other side pyridine groups coordinate into the central metal ions of HoOH. Therefore, a HoOH monolayer is ligated to the underlying 44BPY layer along its axial direction, forming new alternative films. In the alternative films, the oblique angle between the molecular long axis of 44BPY and the normal of the substrate increased, while the molecular plane of HoOH was nearly parallel to the substrate.

Studies on Isomerization of Homoallylic Alcohol in Water over the Nanostructured Mesoporous Ru-PPh₂-SBA-16 Catalyst

ZHANG Fang, WAN Ying, LI He-Xing

2007, 28(1):  125-128.  doi:

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Based on the self-assembly of F127, a new SBA-16-like mesoporous silica modified with diphe-nylphosphine group(PPh₂-SBA-16) was synthesized by extend co-condensation with tetraethoxysilane(TEOS) and 2-(diphenylphosphino)ethyltriethoxysilane(DPPTS) as the mixed silicon source. The PPh₂-SBA-16 was used as a support to immobilize the Ru(Ⅱ) ions through strong coordination between PPh₂-group and Ru(Ⅱ), denoted as Ru-PPh₂-SBA-16. The characterizations demonstrate that the Ru-PPh₂-SBA-16 still remained ordered mesoporous structure. During the isomerization of homoallylic alcohols carried in water as a environmentally friendly medium, the as-prepared Ru-PPh₂-SBA-16 catalyst exhibited an excellent selectivity, almost the same as the corresponding homogeneous catalyst [RuCl₂(PPh₃)₃]. Although its activity was slightly lower than that of RuCl₂(PPh₃)₃, the Ru-PPh₂-SBA-16 could be considered more suitable for industrial application based on the following benefits: (1) The catalyst could be easily separated from the reaction products. (2) The catalyst could be used repetitively at least for 3 times without significant activity decrease. (3) The Ru(Ⅱ) was strongly immobilized on the support which could effectively inhibit the leaching of active sites and protect the environmental pollution from heavy metals.

A Density Function Theory Investigation on Sandwich-type Heavy Transition Metal Complexes(B₆C)₂M Containing Planar Hexacoordinate Carbons

LI Si-Dian, REN Guang-Ming, MIAO Chang-Qing, LI Dong-Dong

2007, 28(1):  129-131.  doi:

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A density functional theory(DFT) investigation on ⅧB second- and third-row transition metal complexes(B₆X)₂M(X＝C, N; M=Ru, Rh, Pd, Os, Ir, Pt) containing quasi-planar hexacoordinate carbon(PhC) or nitrogen(PhN) was presented in this work. The 6π B₆C^2- and B₆N^- units turned out to be effective aromatic ligands to coordinate ⅧB transition metal centers to form 18-electron staggered sandwich-type complexes, in which the colinear terminal PhCs(or PhNs) and the transition metal center M form the six-fold molecular axes of the systems. The planar hexacoordinate nonmetal centers X carrying approximately unitary negative charges follow the octet rule, with the Wiberg bond orders of WBI_PhC≈4 and WBI_PhN≈3. These theoretical predictions are expected to be confirmed in experiments to open a new branch of chemistry on planar hexacoordinate carbons and other nonmetals.

Theoretical Studies on Some Important Reactions of N₃O₂ Ion and Neutral Molecule

ZHANG Hao, SUN Yan-Bo, LI Ze-Sheng, SUN Chia-Chung


2007, 28(1):  132-135.  doi:

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In this article, some important characters about neutral N3O2 molecule such as its dissociations and the key reaction NO+N₂O←→N₂+NO₂ were investigated at CCSD(T)/6-311G(d,p)//B3LYP/6-311 G(d,p)+ZPE levels. The optimized geometries of neutral N₃O₂ are W shape and five-membered ring isomer. However, the energies of the two isomers are so high that they would rather dissociate to some other small molecules. In the photolysis of the N₃O₂ negative ion, such a process is confirmed as N₃O₂^-+hν→TS1(W shape neutral N₃O₂ molecule with C_2v symmetry)+e^-→m1(W shape neutral N₃O₂ molecule with C_s symmetry)+e^-→TS2+e^-→ N₂O+NO+e. Because the barrier near TS2 is very low(only 5.96 kJ/mol), the life of m1 is so short that it can hardly be detected in the experiments. In the key reaction NO+N₂O←→N₂+NO₂, both barriers of multicomponent reaction and elementary reaction are high. But the elementary reaction is easier than the multicomponent reaction.

Preparation and Properties of LiFePO₄/C Composite Materials with Fe₂O₃ as Starting Reactant

WANG Guan, SU Gang, YAN Man-Ming, CAI Wen-Bin, JIANG Zhi-Yu

2007, 28(1):  136-139.  doi:

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LiFePO₄ was considered as a new kind of cathode material candidate for lithium ion batteries due to its advantages. LiFePO₄/C composites were successfully prepared from Fe₂O₃ via solid state reaction by a thermal reduction method in Ar+5%(volume fraction) H₂ atmosphere. The crystal structure and electrochemical behavior of the materials were investigated using XRD, SEM, CV and charge/discharge cycle measurements. Based on the results of TGA-DTA, LiFePO₄/C composites were synthesized at different temperatures, and it was found that the LiFePO₄/C composites synthesized at 700 ℃ with 8.76% mass fraction carbon content presented the initial discharge capacity of 144.8 mA·h/g at 0.1C, and after 160 cycles, the capacity remained as 141.4 mA·h/g. The method is available due to the low cost of Fe₂O₃ instead of using bivalent ferrous compound.

Electrooxidation of 2-Methylpyridine at PbO₂-SPE Composite Electrodes

LI Fei, CAO Xue-Jing, ZHANG Heng-Bin, ZHANG Yu-Min, LI Ke-Chang

2007, 28(1):  140-144.  doi:

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The PbO₂-SPE composite electrodes were prepared by hot press and hot-pressed electroplating methods. The electrocatalytic activity of the PbO₂-SPE composite electrode to the electrooxidation reactions of 2-methylpyridine were studied with the cyclic voltammetry and steady state polarization curves. The relationships between the current density and overpotential and between the overpotential and cell voltage were examined in different electrolytes of the counter electrode, as well as the relationship between the current density and potential was also examined in the solution of the working electrode in the presence of or in the absence of the liquid supporting electrolyte. Also the relationships between the current density and overpotential and between the current density and cell voltage were compared between common PbO₂ electrode and PbO₂-SPE composite electrode prepared by hot press electroplating method. It was found that the latter possesses a high current density at the same overpotential or a low cell voltage at the same current density.

Effects of Proton Exchange Membranes on Performance of Vanadium Redox Flow Battery

Lü Zheng-Zhong^1,2, HU Song-Lin^1,2, LUO Xuan-Li¹, WU Zeng-Hua^1,2, CHEN Li-Quan^1,2, QIU Xin-Ping^1,2

2007, 28(1):  145-148.  doi:

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The poly(vinylidene fluoride)-graft-poly(styrene sulfonic acid) (PVDF-g-PSSA) membrane was prepared by a solution-grafting method for vanadium redox flow battery (VRB)as the separator. The ion exchange capacity (IEC), conductivity of PVDF-g-PSSA, Nafion 117 and PE01 homogeneous membranes were investigated contrastively. The electrochemical performance of VRB with PVDF-g-PSSA, Nafion 117 and PE01 homogeneous membranes as the separator, respectively, was studied. The results show that PVDF-g-PSSA membrane possessed a high conductivity and excellent IEC with a value 3.22×10^-2 S/cm and 1.13 mmol/g respectively, at room temperature. PVDF-g-PSSA membrane showed dramatically lower vanadium ion permeability compared to Nafion 117, its coulombic efficiency and energy efficiency of VRB with PVDF-g-PSSA as the separator being higher notablely than that of VRB with Nafion 117 and PE01 homogeneous membranes as the separator.

A Preliminary Study on Fabrication and Electronic Measurements of a Ag₂S Nanoelectrochemical Switch

KONG De-Sheng^1,2, TIAN Jing-Hua¹, LIU Bo¹, LIU Hai-Lin¹, CHEN Zhao-Bin¹, MAO Bing-Wei¹, TIAN Zhong-Qun¹

2007, 28(1):  149-152.  doi:

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Nanoelectronics is an important area of research in nanotechnology and nanoscience, in which nano structures with electronics functionality are designed and fabricated. In this paper, a Au/Ag/Ag₂S/Au solid-state electrochemical nanoswitch was constructed by using electrochemical methods from the “bottom-up” approach. The Ag₂S nanoelectrochemical switch fabricating procedure includes three steps: (1) A silver layer was electrodeposited on one of a pair of facing Au electrodes which was separated with about 2 μm gap width; (2) the surface of the silver layer was then converted to Ag₂S by electrochemical oxidation in a basic Na₂S solution; (3) the gap was narrowed down to about 1 nm by electrodepositing Au atoms on to the other one of the facing pair electrodes. It is demonstrated that such a device can switch between “on” and “off” states at room temperature and in air. A gap of 1 nm is the key structure of the switch. The Ag₂S switch works by controlling the formation and annihilation of an atomic Ag-bridge at the tip point between two electrodes. The reversibility and stability of the switch is satisfactory with a current difference between “on” and “off” states more than three orders of magnitude.

研究简报

Modulation Effect of Sucrose in the Assembly Nanometer Se⁰ Particles and Their Stability in Liquid Phase

BAI Yan¹, LI Wei-Jia¹, WU Ya-Qin^1,2, ZHENG Wen-Jie¹, ZHOU Yan-Fen¹

2007, 28(1):  153-155.  doi:

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The effect of sucrose on nanometer Se⁰ in liquid phase was reported. Transmission electron microscope(TEM), laser light scattering image and Resonance Rayleigh Scattering(RRS) were used to study the configuration and stability of nanometer Se⁰ particles. The results show that sucrose solution modulated the assemble of nanometer Se⁰ particles and stabilized the Se⁰ particles in liquid phase. From the concentration of 1.07 to 42.8 μmol/L, the diameter of Se⁰ particles were 47—600 nm. However, in the presence of 1.0% sucrose solution, the major distribution range of Se⁰ diameter was 20—80 nm. Furthermore, the nanometer Se⁰ sol-gel could be preserved stably in sucrose solution at least for 2 months at 2—10 ℃.

Photocatalytic Hydrogen Generation Using Glucose and Sucrose as Electron Donors over Pt/TiO₂

LI Yue-Xiang¹, XIE Yan-Zhao¹, PENG Shao-Qin¹, L<SPAN lang=EN-US style=

2007, 28(1):  156-158.  doi:

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Using glucose and sucrose as the electron donors, the photocatalytic hydrogen evolution over Pt/TiO₂ was investigated. Glucose and sucrose enhance notably the activity for hydrogen generation. The amounts of produced H₂ increase almost proportionally to time within 5 h irradiation in the reaction systems of the two electron donors. The effect of the initial concentration of glucose and sucrose on the reaction rate is consistent with the Langmuir-Hinshelwood kinetic model. After 5 h irradiation, the COD(chemical oxygen demand) in the reaction system of glucose and in that of sucrose decrease by 33.2%, 11.4% respectively. The effect of electron donors on the flat-band potential of conduction band of TiO₂ electrode was investigated. The flat-band potential of conduction band of TiO₂ electrode in the presence of the electron donors shifts negatively, and the shift in the presence of glucose is larger than that in the presence of sucrose due to glucose having a larger adsorption amount on TiO₂.

研究论文

Effects of the Chemical Structure Changes on Phase Behavior, Thermal and Mechanical Properties of Rigid Rod Epoxy Resins

REN Shao-Ping^1,2,3, LIANG Li-Yan^1,2,3, LAN Yan-Xun², ZHOU Jiang-Min⁴, L 2007, 28(1):  159-163.  doi:

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Phenol novolac resins(PN) and sulphanilamide(SAA) were used to cure rigid rod epoxy resins, namely DGEBP, DGETMBP and traditional epoxy resin(DGEBA). The effects of chemical structure of epoxy resins on the thermal, mechanical, and phase behavior were studied. The results show that rigid rod epoxy resins exhibited better physical properties than DGEBA. The epoxy networks which contain oriented domains showed high thermal properties and toughness. SEM was conducted to investigate the morphology of fracture surface. The fractography of unisotropic rigid rod epoxy networks exhibited an extremely rough and highly deformed fracture surface. The fracture surfaces of the isotropic epoxy networks were smooth, which was the character of fragile materials.

Modification of Carbon Nanotubes with Surface Hyperbranched Poly(p-chloromethyl stryrene)

WANG Guo-Jian, DONG Yue, LIU Lin, XU Qian-Wei

2007, 28(1):  164-168.  doi:

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Hyperbranched poly(p-chloromethyl stryrene)(PCMS) was prepared by combining atom transfer radical polymerization(ATRP) and self-condensing vinyl polymerization(SCVP). The branches of the hyperbranched PCMS was ended with halogen atoms, which were transferred into azide groups. Then PCMS was connected to the surface of carbon nanotube by the reaction of azide group with single walled carbon nanotube(SWNT) or multi-walled carbon nanotube(MWNT) and the chemical modification of CNT was realized. The results from FTIR, XPS, Raman spectra and TEM show that PCMS was combined with carbon nanotube by the covalent bond. According to the results of TGA mensuration, the modification density was calculated and it can be confirmed that massive functional groups from hyperbranched polymer is favorable for improving the effect of modification of carbon nanotubes.

Preparation of Water-soluble Quantum Dots and Their Self-assembly with Chitosan Derivatives

XU Hai-E, YAN Cui-E

2007, 28(1):  169-172.  doi:

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Water-soluble CdTe quantum dots(QDs) were prepared by using 3-mercaptopropionic acid as the stabilizer, and their preparation parameters were optimized. Self-assembling of QDs with chitosan and folic acid(FA) and poly(ethylene glycol)(PEG) modified chitosan via electrostatic interaction was also investigated. The results demonstrate that fluorescence intensity of chitosan/QDs complex was much higher than that of QDs themselves. The complex shows a clear core/shell structure, and QDs were located in the core. The modified chitosan/QDs complexes were smaller and more uniform than those of unmodified chitosan.

Synthesis and Partial Properties of Naphthalene and Phthalazinone-based Sulfonated Copolyimides for Proton Exchange Membrane in Fuel Cells

PAN Hai-Yan, LIANG Yong-Fang, ZHU Xiu-Ling, ZHANG Shou-Hai, JIAN Xi-Gao

2007, 28(1):  173-176.  doi:

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A new sulfonated copolyimides(SPIs) containing both of naphthalene and phthalazinone moieties in polymer's main chain were successfully synthesized from 4,4'-diaminophenyl ether-2,2' disulfonic acid(ODADS), 1,2-dihydro-2-(4-aminophenyl)-4-[4-(4-aminophenoxy)phenyl]-phthalazin-1-one(DHPZ-DA) and 1,4,5,8-naphthalenetetracarboxylic dianhydride(NTDA) via direct polymerization, which are potentially utilized in proton exchange membrane in PEMFC. The obtained sulfonated polymers(SPIs) have a molecular weight with the inherent viscosity range from 0.55 to 1.47 dL/g. The chemical structure of the SPIs was carefully characterized by FTIR and ¹H NMR. The yellow transparent and tough membranes cast from m-cresol solution of SPIs were obtained, which were utilized to investigate the physicochemical properties of new copolymers. The data demonstrate that the membrane's water uptake, swelling ratio, ion exchange capacities(IEC), as well as the resistance to both of water and oxidation varied accordingly with the increase of sulfonation degree of the new SPIs. The introduction of DHPZ-DA improved the SPIs' solubility. Meanwhile, the thermic stability of copolymers by TGA was also investigated.

Photochemical Synthesis and Characterization of Amine-functionalized Superparamagnetic Nanogel for α-Chymotrypsin Immobilization

HONG Jun, XU Dong-Mei, SUN Han-Wen, GONG Pei-Jun, DONG Li, YAO Si-De

2007, 28(1):  177-182.  doi:

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In this paper, amine-functionalized superparamagnetic nanogel was obtained by Hoffman degradation of the PAM-coated Fe₃O₄ nanoparticles prepared by photochemical in situ polymerization. α-Chymotrypsin was successfully bound to the magnetic nanogel with amino groups in the presence of 1-ethyl-3-(3-dimethylaminepropyl) carbodiimide(EDC). The immobilized enzyme was characterized by using photo correlation spectroscopy(PCS), transmission electron microscopy(TEM), X-ray diffraction(XRD) analysis, thermogravimetric-differential scanning calorimetry(TG-DSC) and Fourier transform infrared spectroscopy. Mean particle size of the immobilized enzyme was measured to be 31 nm by PCS; the binding capacity was 69 mg enzyme/g nanogel determined by TG analysis, 61 mg enzyme /g nanogel determined by standard BCA. The crystalline structure of Fe₃O₄ was affected by xenon lamp irradiation and enzyme immobilization. Magnetic content of the immobilized enzyme was as high as 88%. Specific activity of the immobilized α-chymotrypsin was 0.93 U/(min·mg), 59.3% of free form. It can be expected that the immobilized α-chymotrypsin has a potential in the fast detection and separation, as well as the reuse of immobilized enzymes.

Synthesis and Characterization of N-(2-Sulfobenzyl)chitosan and pH Sensitivity of Its Hydrogel

LIN You-Wen , CHEN Qing, LUO Hong-Bin

2007, 28(1):  183-187.  doi:

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By two steps of reaction, a novel water-soluble chitosan derivative[N-(2-sulfobenzyl) chitosan, SBCS] was synthesized. The chemical structure of SBCS was characterized by FTIR, ¹H NMR, UV-Vis spectra. Degree of substitution(DS) of N-2-sulfobenzyl was determined by colloid titration. In the buffer solutions with different pH values the swelling characteristics of hydrogels based on SBCS(SBCSG) prepared by cross-linking with glutaraldehyde were studied. The results show that the swelling ratio(SR) of SBCSG was decreased with increasing the dosage of glutaraldehyde. The SBCSG swelled more significantly in alkaline solution than in acidic medium and showed the lowest SR at pH=5.0. In alkaline solution, the SR of SBCSG was increased with raising the DS of N-2-sulfobenzyl of SBCS, but no significant change in acidic environment. The SBCSG showed swelling reversibility when soaked in pH=1.0 and pH=7.4 buffer solutions alternately. The results imply that SBCS could be potential pH sensitive carrier for colon-specific drug delivery system.

Preparation and Properties of a Novel Poly(ether sulfone) Microcellular Material

WEI Hong^1,2, GUAN Shao-Wei¹, GUO Mei-Mei¹, MA Xiao-Ye¹, JIANG Zhen-Hua¹

2007, 28(1):  188-192.  doi:

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A modified poly(ether sulfone)(PES) was prepared by introducing diallyldihydroxybiphenyl(DA-DHBP) unit into the main chain of PES and microcellular foams of the modified PES were prepared by using supercritical carbon dioxide as the foaming agent. Before radiation crosslinking, the influence of foaming temperature, saturation pressuse, foaming time and transfer time on the microcellular morphology was investigated. The results suggest that the cell diameter increased with increasing the foaming temperature and the cell density reached the maximum at 140 ℃, when the foaming temperature ranged from 110 ℃ to 170 ℃; the cell diameter decreased and the cell density increased with saturation pressuse increased; the foaming time and transfer time almost haven't influenced on the cell diameter and cell density. After radiation crosslinking, the influence of radiation dosage on the microcellular morphology was investigated. The results suggest that the content of gelation increased gradually with the increase of radiation dosage and the radiated sample can remain the microcelllar structure well, even though the radiated sample was heat-treated at 265 ℃ for 10 min.

Preparation of Monodisperse Polyacrylamide Microspheres with Submicrometer Size in Ethyl Acetate/Ethanol Media by Dispersion Polymerization

CAO Kang-Li, SHI Tie-Jun, ZHAI Lin-Feng, CAO Jin-Yan, WANG Hua-Lin

2007, 28(1):  193-198.  doi:

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Using PVP as the stabilizer and AIBN as the initiator, monodisperse PAM microspheres sized in submicrometer were prepared in ethyl acetate/ethanol media by dispersion polymerization method. In the early period of the dispersion polymerization, auto-accelerate phenomenon was observed, and molecular weight gradually increased with the increase of the conversion because of the gel effect. The study on the FTIR spectrum of PAM and the effects of the concentrations of stabilizer on final increment ratio reveal that adsorption stabilization mechanism and graft stabilization mechanism are concurring in this system and the latter is dominant. The influences of polymerization parameters, such as concentration of stabilizer, initiator, monomer and solvent composition on the particle size and size distribution were also investigated. The size distribution is narrow when the volume ratio of ethyl acetate to ethanol ranges from 5∶5 to 7∶3. Particle size decreases with the increase of the concentration of stabilizer and the decrease of the concentration of initiator, moreover, monodisperse microspheres cannot be obtained when the concentration of monomer is too high or too low.