Table of Content

10 June 2006, Volume 27 Issue 6

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高等学校化学学报2006年第27卷第6期目次

2006, 27(6):  0.  doi:

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研究论文

Structural Investigation of Layered Aluminophosphate UT-4 by Solidstate NMR

ZHOU Dan¹, CHEN Lei², YU Ji-Hong1*, DENG Feng², XU Ru-Ren¹

2006, 27(6):  991-994.  doi:

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Pure UT-4 crystalline phase was synthesized by using pyridine as the solvent instead of TEG in the system of Al₂O₃-H₃PO₄-C₆H₁₁NH₂-Py. ²⁷Al MAS NMR, ³¹P MAS NMR, ¹H→¹P cross-polarization(CP) and ²⁷Al-³¹P heteronuclear correlation(HETCOR) experiments were employed to investigate the framework of UT-4, a two-dimensional layer aluminophosphate, which was first synthesized in the system of TEG, coexisting with UT-5. In the assignment of two fourcoordinated Al atoms, two methods were used. The assignment of ³¹P signals is based on the ²⁷Al-³¹P HETCOR spectrum.

Effects of Ray Irradiation on KMgF₃ and KMgF₃∶Eu²⁺ Crystal

MO Feng-Shan^1,3, ZHU Guo-Xian^1,3, XIA Chang-Tai², SHI Chun-Shan^3*

2006, 27(6):  995-998.  doi:

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The conversion of Eu³⁺ →Eu²⁺ in KMgF₃∶Eu is almost 100% at the low dopant concentration and the saturant dopant is 0.29% molar fraction. The irradiation damage of KMgF₃ crystal by 1 h X-ray irradiation can recover in about 100 h under experimental condition. After KMgF₃∶Eu²⁺ crystal was irradiated by X-ray, the sharp peak emission intensity at about 360 nm cuts down slightly and the stimulated spectrum was not observed. The changes are obviously different for all thetemperature peak intensities of TLS glow curves of KMgF₃ crystal irradiated by γ-ray of different dosages, even if the damage caused by a little dosage irradiation is relatively hard to recover, for example, if the dosage of γ-ray irradiation is 103 Gy, the recovery time of irradiation damage is about 30 d. The sharp peak emission intensity at 360 nm drops linearly with the growth of γ-ray irradiation dosage.

Effects of Lanthanide Ions(La³⁺, Gd³⁺, Yb³⁺) on Production of Reactive Oxygen Species in Mitochondria

LIU Hui-Xue, YANG Xiao-Da*, WANG Kui

2006, 27(6):  999-1002.  doi:

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The effects of lanthanides(Ln) on the production of reactive oxygen species(ROS) in isolated mitochondria were investigated by fluorescence assays upon incubation with Ln³⁺. The results show that Ln³⁺(La³⁺, Gd³⁺, Yb³⁺) could reduce the rates of overall ROS production. The results obtained from experiments on xanthine/xanthine oxidative enzyme system suggest that Ln³⁺ ions can reduce the formation of ·O^-₂, but H₂O₂ did not react with Ln³⁺. The influences of Ln³⁺ on the activities of metabolize enzymes(GSH-Px and Mn-SOD) indicate that Ln³⁺ could decrease the activity of Mn-SOD, but could not affect the activity of GSH-Px. The effects of Ln³⁺ on cellular H₂O₂ level are discussed.

Effect of PVA on Ferric Oxide Coated on Carbon Nanotubes

YU Hua-Rong, CHENG Rong-Ming*, XU Xue-Cheng, CHEN Yi-Wei

2006, 27(6):  1003-1006.  doi:

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Fe₂O₃ coated on CNTs were prepared by adding CNTs in liquid-disposition process. The TEM images show that CNTs and Fe₂O₃ would be separated from each other without the PVA and be connected well when the PVA was absorbed on the surface of CNTs. The PVA could help CNTs weltering the aquatic phase and enhance the stability of their dispersion. The PVA had bifunctional bridges, with hydrophilic groups jointed with the Fe₂O₃ film, and hydrophobic chains adhered to the surface of the carbon nanotubes, so the Fe₂O₃ were supported on the surface of the carbon nanotubes through the surfactant. When the sample was calcined at 350 ℃, the PVA melted and coated on the external suface of CNTs to prevent the Fe₂O₃ from seperating from the CNTs′ external suface. The XRD patterns of the Fe₂O₃ film coated on CNTs reveal that the coating was α-Fe₂O₃ and γ-Fe₂O₃.

Preparation and Characterization of Threedimensionally Ordered SiC Hollow Spheres

WANG Hao¹*, LI Xiao-Dong¹, XIAO Jia-Yu¹, KIM Dong-Pyo²

2006, 27(6):  1007-1011.  doi:

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Three-dimensionally long range ordered SiC hollow spheres were prepared for the first time by infiltrating polymethylsilane(PMS) into three-dimensionally ordered sacrificial porous carbon templates produced from the ordered silica spheres as the original templates, curing and pyrolysis of PMS, and the removal of the porous carbon templates. It was found that the outer diameter(135-896 nm), the wall thickness(14-79 nm), BET specific surface area(50.8-5.0 m²/g) and micropore volume(0.265-0.038 cm³/g) of the achieved SiC hollow spheres can be tailored by utilizing carbon templates with different pore sizes or PMS solutions with different concentrations. In addition, the produced SiC hollow spheres were packed as a hcp structure to be a long range ordered assembly.

Optical Properties of a-C and a-C∶H Diamond-like Films Prepared by High Power Excimer Laser Ablation

CHEN Bao-Ling¹; ZHAO Li-Xin²; ZHANG Bing¹; CHEN Yu-Qiang1; YANG Xin-Hui¹; PENG Hong-Yan^1*; JIN Zeng-Sun³

2006, 27(6):  1012-1015.  doi:

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The amorphous carbon films have many superior properties such as high hardness, high wear resistance, low coefficient of friction, etc., making them suitable for many applications so that many studies have focused on the synthesis and characterization of carbon coatings in the past years. The films can be prepared by different techniques, among them was pulsed laser deposition(PLD) which has attracted much attention mainly due to the good quality film it produces. In this work amorphous carbon(a-C) and a-C∶H films were deposited by high frequency and high power pulsed XeCl excimer laser ablation of pyrolytic graphite targets at room temperature. The effect of the laser power density and the pressure of hydrogen atmosphere on the optical properties of the films were studied by setting the laser peak power density on the target at 10⁸, 10⁹ and 10¹⁰ W/cm², respectively, and the pressure of the hydrogen was 0, 2, 20 and 50 Pa while the laser density at 10¹⁰ W/cm². Raman spectra as well as the UV and IR transparency were used for film analysis. The results indicate that the optical property of the films was improved with the increase of the laser power density and the hydrogen pressure, respectively. The reason was demonstrated according to the pulsed laser deposition mechanism.

Novel ^99mTc-nitride Heterocomplexes as Potential Myocardial Perfusion Imaging Agents

CHU Jin-Feng¹, KONG De-Jing², LI Bin², WANG Xue-Bin^2*, LU Jie ² , WANG Jin-Cheng³, MI Hong-Zhi³, ZHAO Jian-Dong³

2006, 27(6):  1016-1019.  doi:

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To develop a new potential myocardial imaging agent, [^99mTcN(PNP5)(DEDC)]⁺ and [^99mTcN(PNP5)(DPODC)]⁺ were prepared through ligand exchange reaction. Their radiochemical purities were over 90%. The results of biodistribution in mice indicate that they possessed a high myocardial uptake, rapid clearance from nontarget tissues and good ratios of target to nontarget. And [^99mTcN(PNP5)\5(DEDC)]⁺ is superior. SPECT imaging in dog shows that its properties were similar to those of ^99mTc-tetrofosmin. Based on its promising characters, it may be suitable for myocardial perfusion imaging.

研究简报

Synthesis, Structure of a Novel Two-dimensional Inorganic-organic
Framework Ni(PDC)(H₂O)₂ with Double Helical Chains

TIAN Ge, ZHU Guang-Shan, FANG Qian-Rong, XIN Ming-Hong, GUO Xiao-Dan, XUE Ming, QIU Shi-Lun*

2006, 27(6):  1020-1022.  doi:

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A novel coordination polymer [Ni(PDC)(H₂O)₂] was synthesized under solvothermal conditions and characterized by means of single- crystal X-ray diffraction(XRD) analysis, elemental analysis, IR analysis, TG analysis. Crystal data for C₇H₇NO₆Ni were obtained, i.e., monoclinic P2₁/c(No.14), a=0.720 2(3) nm, b=0.917 2(4) nm, c=0.128 79(4) nm, β=90.46(3)°, Z=4. The compound was a 2D layered coordination polymer with helical chains. In the compound, there are two helical Ni-O-C and Ni-pdc chains in one layer, and the opposite orientation of the helical chains in the adjacent layers. The layers are connected via hydrogen bonds into 3D supramolecular framework.

研究论文

Rapid and Sensitive Detection and Characterization of Saccharomyces
cerevisiae by Light Scattering Method

CHEN Shao-Fen; HUANG Cheng-Zhi*; TAN Ke-Jun

2006, 27(6):  1023-1027.  doi:

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The light scattering(LS) spectra of Saccharomyces cerevisiae was studied. The results show that the LS intensities were in proportion to the concentrations of Saccharomyces cerevisiae at peak 308.0 nm in the concentration range of 2.0×10⁴-2.0×10⁶ Cell/mL. The detection limit(3σ) was 4.94x10² Cell/mL. The present new method was successfully applied to the rapid, sensitive determination and characterization of Saccharomyces cerevisiae biomass in suspensions.

Studies on Determination of Percentage Bound of Eight Antibiotics by Using a New Home-made Surface Plasomon Resonace Sensor

ZOU Xiang-Yu, ZHOU Jian-Guang, XIE Ping, ZHANG Lei, WANG Shu-Hua,
FENG Guo-Dong, JIN Qin-Han*

2006, 27(6):  1028-1031.  doi:

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Based on surface plasmon resonance (SPR), a novel optical chemical sensor was developed. Traditionally, wavelength modulation SPR sensing method adapted tungsten lamp as the light source with an expensive and complicated apparatus. The device presented here is a relatively simple and inexpensive one. It was designed using a white LED with a 5 V battery as the light source. The percentage bound of 8 antibiotics with BSA was studied by this setup. The results were compared with the reliable percentage bound data obtained by standard equilibrium dialysis and a relative good agreement was achieved.

An Amplified Piezoelectric Immunosensor Based on Amplification of Enzyme-catalyzed Precipitation Mass

FU Ting, WANG Hua, SHEN Guo-Li*, YU Ru-Qin

2006, 27(6):  1032-1035.  doi:

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In this paper, an amplified immunosensor with highly sensitivity has been proposed based on precipitation of an insoluble product on functionalized electrode. Anti-hIgG was immobilized onto the surface of gold electrode modified with 1,6-hexanedithiol and colloidal Au interface. It was proved that the amount of immobilized antibody and the immunoactivity of bound antibodies could be well improved by colloidal Au. HRP labeled antibody reacted with antigen, then HRP biocatalyzed DAB (3,3′-diaminobenzidine) in the presence of H₂O₂, resulting in an insoluble product on the electrode surface, to achieve an obviously decreased frequency. Comparing with the direct detection of antigens, the immunosensor with the proposed amplified procedure shows improved sensitivity due to the significantly extended detection range. Analytical results indicate that the developed amplified procedure is a promising alternative for biorecognition element on the electrode surface showing an improved performance in terms of the magnitude of the response and sensitivity. The proposed immunosensor in optimal conditions has a linear range of 16 ng/mL-100 μg/mL for hIgG detection with a detection limit of 10 ng/mL. The immunosensor can be used to quantitatively determine hIgG in the sample of human serum.

Post Chemiluminescence Reaction of Dipyridamole in Luminol in Luminol-potassium Ferricyanide System and Its Application in Analysis
-----The Molecular Imprinting-post Chemiluminescene Method for the Determination of Dipyridamole

LIU Qing-Hui; LU Jiu-Ru*; FENG Na

2006, 27(6):  1036-1041.  doi:

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In this work, a new post chemiluminescence(PCL) reaction of the Dipyridamole in the potassium ferricyanide-luminol system was found. A possible PCL mechanism was proposed based upon the studies of the kinetics characteristics, the CL spectra, fluorescence spectra of some relative reactions and other series of experiments. At the same time, Dipyridamole-imprinted polymer(MIP) was synthesized. Using the MIP as the recognition material and employing potassium ferricyanide-luminol-Dipyridamole PCL system, a new molecular imprinting-post-chemiluminescence(MIP-PCL) method for the determination of Dipyridamole was established. The linear range of this method was 1.0×10^-8-1.0×10^-6 g/mL with a linear correlation coefficient of 0.999 2, the detection limit was 3×10^-9 g/mL and the relative standard deviation for the determination of 1.0×10^-7 g/mL Dipyridamole solution was 2.7%(n=11). This method was successfully applied to the determination of Dipyridamole in human urine with a satisfactory result.

In Vivo Rat Metabolism Studies of Ginsenoside-Rb₁

YANG Liu, XU Shun-Jun, ZENG Xing, WU Zhi-Feng, DENG Yuan-Hui, LIU Yi-Ming

2006, 27(6):  1042-1044.  doi:

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The major metabolites of ginsenoside-Rb₁ in rats urine were described. Urine samples were collected before and after 24 h of single oral administration of 150 mg and intravenous administration of 60 mg Rb₁ to four rats, respectively. The samples were purified by SPE column and then were analyzed by liquid chromatography-ESI-mass spectrometry for potential metabolites. Parent drug and its fourteen metabolites were identified in rat urine based on the comparison of total ion chromatograms of the blank with the metabolic urine as well as mass spectra. Its main metabolic pathways and possible structures are analyzed in detail.

研究简报

Molecular Size Distribution Characteristics of the Element-DOM Complexes in Nature Waters by HPSEC-UV-ICP-MS

WANG Zheng, JIANG Miao, Frank S. C. Lee, WANG Xiao-Ru*

2006, 27(6):  1045-1047.  doi:

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The complexation of the elements P, S, Cr, Ni, Cu, Zn, Fe, Hg, Pb, Cd and As with different molecular size fractions of dissolved organic matter in one river water sample and two sea water samples were investigated by coupling size-exclusion chromatography sequentially with UV-Vis and inductively coupled plasma mass spectrometric detectors. It can provide quantitative information regarding the distribution of both DOM and its element-bound complexes. This information would be helpful in understanding of the speciation, mobility and bio-accessibility of elements in the environment and further elucidation of the dissolved organic matter structure.

Simultaneous Kinetic-spectrophotometric Determination of Three Organophosphorus Pesticides with Multivariate Calibration Methods

NI Yong-Nian*; CAO Dong-Xia

2006, 27(6):  1048-1050.  doi:

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A kinetic-spectrophotometric method for the determination of parathion, methyl-parathion and fenitrothion was developed. It was based on the kinetic reaction of these compounds with H2O2 in alkaline medium. Under the optimal conditions, quantitative analysis for each compound in mixtures was investigated with the aid of multivariate calibration methods. The proposed method was applied to several water samples spiked with known amounts of the pesticides with satisfactory results.

研究论文

Purification and Preparation of Active Subunits of C-phycocyanin by a Protocol of Liquidphase Isoeletric Focusing

HUANG Zhi^1,2, YANG Fang¹, ZHENG Wen-Jie¹, GUO Bao-Jiang^2*

2006, 27(6):  1051-1054.  doi:

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A process of liquidphase isoeletric focusing(LP-IEF) was developed and conducted in a 8.0 mol/L urea medium in Rotofor system for isolation, purification and preparation the α and β subunits of C-PC(αβ)3 purified from Spirulina platensis. After two steps of pre- and re- fractionating, collected fractions with α or β subunit were identified and characterized by SDSPAGE and slab ultra thin IEF. Its absorption and fluorescence spectra were determined. The results show that the α and β subunits were concentrated at about pH=4.9 and pH=4.1 respectively and the total recovery of α and β subunits was 392%. The α and β subunits of C-PC with a high purity as well as activity maintaining were obtained easily by this LP-IEF protocol, suggesting that it should be an ordinary but effective method for purification and preparation of protein subunits with different pI values.

Total Synthesis of (±)Caulilide(Ⅱ)

YAN Ri-An^1*, SU Jing-Yu²

2006, 27(6):  1055-1057.  doi:

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The Caulilide which shows a potent cytotoxicity was synthesized from 2,6,6trimethylcyclohex2ene1,4dione via selective ketalization, Wittig reaction, deprotection, hydrolysislactonization and reduction in 60% total yield, in which wittig reaction was the key step. The difficulty of this reaction came from the strong blocking effect, many reaction conditions were optimized, a better yield of this reaction was gained in 578%. The synthesis of caulilide was completed by reduction of a lactone with NaBH4, the crude product was separated by high performance liquid chromatography to give the target compound.

Syntheses and Fluorescent Property of 5-(2-Phenyl-1,2,3-triazoly)-3-aryl Pyrazoline Derivatives

LI Fang¹,XIE Zheng-Feng1, LIU Fang-Ming^1,2*

2006, 27(6):  1058-1061.  doi:

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Four chalcones were synthesized by aldol condensation reaction of acetophenone or parasubstituted acetophenones with 2-phenyl-1,2,3triazol-4-carboxaldehyde, which reacted with three hydrazines in glacial acetic acid under refluxing to give a series of pyrazoline derivatives. The structures wer confirmed by means of IR spectrum, ¹H NMR and element analyses. The fluorescent spectra of twelve compounds were detected. The results show that the compounds have fluorescence. The fluorescence emission wavelength of compounds 3a—3d is about 380 nm. The effect of diffient substituents on the fluorescence intensity was investigated.

Design and Synthesis of Photolabeling Probes for the Study of Antiviral Mechanism of Ribavirin

ZHU Xun^1,2*, QU Fan-Qi³

2006, 27(6):  1062-1065.  doi:

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The photolabeling probes for the study of antiviral mechanism of ribavirin were designed, and the synthesis experiments were carried out by using 1,2,3,5-tetra-O-acetyl-β-D-ribofuranose and methyl 3-bromo-1,2,4-triazole-5-carboxylate as the raw materials. Two photolabeling probes for the study of antiviral mechanism of ribavirin, 5-azido-1-(β-ribofuranosyl)-1,2,4-triazole-3-carboxamide and 3-azido-1-(β-ribofuranosyl)-1,2,4-triazole-5-carboxamide were synthesized, and characterized by IR, MS and 1H NMR, etc.. The design of the photolabeling probes and their structures were discussed.

Studies on Adsorption Mechanisms of Adsorbents for Endotoxin

LI Ji-Hong¹, YU Meⁱ¹, WANG Hui-Yan¹, YUAN Zhi^1*, MA Yi²

2006, 27(6):  1066-1069.  doi:

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It had been reported that a novel molecular recognition, in which there was a hydroxyl group at β site, had excellent adsorption capacity of endotoxin. In this work, the computer simulation method was used to investigate the interaction mechanism between the adsorbents and the endotoxin. The computer simulation showed that the hydroxyl group at β site of adsorbent with dimethylamine ligand could form H bond with endotoxin, as a result an eightmembered ring was formed. The electrostatic interaction, hydrogen bond and cooperative effect of the eightmembered ring were formed simultaneously. The interaction between a series of adsorbents model with hydroxyl group at different sites and endotoxin were investigated by computer simulation, too. The result indicated that electrostatic interaction was the main interaction force, and the site of hydroxyl group could affect the adsorption capacity of adsorbents obviously.

Studies on ESI-MS of Mannosyl-1-phosphoramidates

SUN Qi¹, MA Qiang¹, HE Li¹, JU Yong ^1,2* , ZHAO Yu-Fen ¹

2006, 27(6):  1070-1074.  doi:

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Phosphoglycoproteins are a kind of compounds that have many important biological functions. In order to study the relationship between the structure and the biological functions of these compounds, some core structures(glycosyl-1-phosphoramides) of these compounds were synthesized. Electrospray ionization mass spectrometry(ESI-MS) was used to study the fragmentation characteristics of various types of acetyl protecting mannosyl-1-phosphoramidates. The results show that there are very different characteristics between α- and β- anomeric isomers. The ESI-MS² spectra of the quasi\|molecular ion ［M+Na］⁺ of β-anomeric isomers show characteristic fragment ions at m/z 433, 391 and 371; and the relative abundance of fragment ion ［M-CH₂CHCH₃+Na］⁺ peak is much higher than that of αanomeric isomers. That this characteristic fragmentation should be due to the interaction of the phosphoramide group at the anomeric carbon and the acetyl protecting groups of the hydroxyl groups, especially the acetyl protecting group at C2. Meanwhile, the ESI-MS³ spectrum of fragment ion ［sugar+Na］⁺ m/z 353 of different isomers of acetyl protecting glycosyl-1-phosphoramidates shows the same fragmentation pattern including the loss of molecules of CH_2⁼C=O and AcOH and is not effected by the other position configuration.

Elemental Analysis of Human Bones in Xigongqiao Site

HU YaoWu1*, HE DeLiang2, LIU XinYi3, DONG Yu3, WANG ChangSui1,
GAO MingKui2, LAN YuFu2

2006, 27(6):  1075-1079.  doi:

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Palaeodietary reconstruction through elemental analysis has been of great concern in bioarchaeology. However, bone diagenesis, or bone contamination, during long\|term burial would have great impact on the elemental contents of bones. Therefore, identification and exclusion of contaminated bones become a prerequisite before elemental analysis. In this paper elemental contents of 18 human bones in Xigongqiao Site, Tengzhou, Shangdong, were analyzed to monitor bone diagenesis. The Ca/P ratios and contents of Ca and P in XM29, XM 34, XM48, XM38, XM49, XM22, XM41, XM28, XM8 and XM42 indicated the loss of hydroxylapatite integrity. Contents of Al and Fe and their correlation, correlation of Ba and Mn and correlation of lg(Sr/Ca) and lg(Ba/Ca) in the left samples showed that they were contaminated by attack of soil and microorganism. So systematic indicators of bone diagenesis were set up and implied that all the samples were contaminated to some extents and can not be used for palaeodietary study.

Effects of Temperature on Adsorption Behavior of Synthesis Gas and Stability for Co/SiO₂ as Catalyst in Fischer-Tropsch Synthesis

ZHOU Wei, FANG Ke-Gong, CHEN Jian-Gang, SUN Yu-Han*

2006, 27(6):  1080-1085.  doi:

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The effects of temperature on adsorption behavior of synthesis gas and stability for Co/SiO₂ catalyst in FischerTropsch synthesis(FTS) were studied by using FTIR, TPSR, XRD, BET, HTPD and TPR technologies. It was found that the CO adsorption was active on the surface of the catalyst and that was still stable at 270 ℃. With the reaction temperature increasing, the main reaction changed from the CO hydrogenation reaction to the Boudouard reaction, and the latter became overwhelming beyond 350 ℃. Besides, cobalt sintering became more evident accompanied with the formation of cobalt silicates and/or hydrosilicates species on the catalyst with the increase of the reaction temperature. It was also proved that sintering was the dominant reason for the catalyst deactivation at higher reaction temperature.

Preparation of V(Ⅴ)Promoting SO^2-₄/ZrO₂ Solid Superacid and Its Catalytic Activity

ZHENG Ming-Dong¹, CHEN Tong-Yun^1*, HU Ke-Liang²

2006, 27(6):  1086-1090.  doi:

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The V(Ⅴ)-promoting SO^2-₄/ZrO₂ solid superacid samples were prepared by the method of ageing at a low temperature. The acidities of the samples were determined with flow indicator method, and the characterizations of the samples were performed by IR, XRD and XPS. The samples were used in the esterification of acetic acid and glycerol. The results show that the catalysts calcined at 600—650 ℃ and aged at a low temperature have a better performance comparing with other samples aged at ambient temperature, the flexible vibration peak of SO bond was strengthened remarkably in IR spectra, XRD patterns of aged samples at a low temperature and containing V(Ⅴ) additive indicate that metastable ZrO₂ cubic crystals formed which were baked at 600—650 ℃. The peak position of Zr_3d has a bigger chemical shift in XPS patterns.

Theoretical Studies on the Ground State and Excited State of 7-Azaindole Derivatives

FAN Jian-Xun¹, REN Ai-Min¹, FENG Ji-Kang^1,2*, Bo Dong-Sheng¹

2006, 27(6):  1091-1095.  doi:

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7-Azaindole derivatives: 1,3-di(N-7-azaindolyl)benzene(1), 1,3,5-tri(N-7-azaindolyl)benzene(2) and 4,4′-di(N-7-azaindolyl)biphenyl(3) were optimized with ab initio-HF and density functional theory-B3lyp and calculated I_P, E_A and other energies. Absorption spectra are obtained by using ZINDO and TDDFT. CIS method was used to calculate the S₁ excited states of the three compounds and to analyze the relation ship between their energies and emission spectra; the absorption and emission spectra were calculated in solvent and compared with the experimental data. The results indicate that the abilities for accepting holes from 7-azaindole to the three derivatives upwards are strengthened in turn, and that absorption and emission spectra are red-shifted.

Synthesis, Crystal Structures and Quantum Chemistry Study of Scorpionates Oxovadium Complexes

XING Yong-Heng^1*, SUN Zheng², GE Mao-Fa², BAI Feng-Ying¹, NIU Shu-Yun¹, YANG Guang-Di³, YE Ling³

2006, 27(6):  1096-1100.  doi:

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Two new complexes of VO(acac)[HB(pz)₃](1) and VO(acac)[HB(3,5-Me₂pz)₃]·CH₃CN(2) were synthesized by using tripyrazolylborate ligand. Both complexes were characterized by element analysis, IR spectra, UV-Vis spectra and their crystal structures were determined by X-ray diffraction. The electronic structure and the bonding characters of the two complexes were calculated with ab initio and Natural Bonding Orbital analysis.

Absorption Properties of Ordered Cu/AAO Nano-array Composite Structures

LI Yan¹; WANG Cheng-Wei^1,2*; ZHAO Xin-Hong¹; WANG Jian¹

2006, 27(6):  1101-1105.  doi:

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Ordered Cu/AAO nano-array composite structures were fabricated by the electrodeposition method within the cylindrical pores of anodic aluminum oxide(AAO) membranes and their optical properties were characterized by absorption spectrum in the range of 200-1000 nm. The experiments show that the surface plasma resonance(SPR) peak appeared around a wavelength of 570 nm, which had a little blue shift and strengthened with the increase of Cu deposition, and gradually disappeared with a larger red shift of the absorption edge over 500 nm. These interesting phenomenon can be well qualitatively described in the framework of the Maxwell-Garnett(M-G) theory. Here, the theoretically analyzed modulation mechanism of the composites′absorption edge expatiates the absorption peak disappearance with the increase of Cu deposition.

Ab initio Study of Fullerenelike Structures of Si₆₀

GAN Li-Hua, SHU Chun-Ying, WANG Chun-Ru*

2006, 27(6):  1106-1108.  doi:

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Ab initio calculations were performed on Si₆₀(I_h) and its several lower symmetrical structures. Five stable structures of spherical Si₆₀ with T, C_i, C₁, C_s and C₂ symmetries were found by following the imaginary frequency vibrations of Si₆₀(I_h), Si₆₀(D_3d) and Si₆₀(T_h). The calculated results demonstrate that some silicon atoms pop out and some shrink inward in the five favored structures of Si60, leading to form sp3 hybridization of silicon. These results will provide insight into the formation and stability of nanoscale silicon clusters.

Heat Capacity and Thermodynamic Properties of Crystalline Pyrimethanil Phenoxyacetate(C₂₀H₂₁N₃O₃)

SUN Xiao-Hong^1*; LIU Yuan-Fa²; TAN Zhi-Cheng³; JIA Ying-Qi²; WANG Mei-Han³

2006, 27(6):  1109-1112.  doi:

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Low-temperature heat capacities of Pyrimethanil phenoxyacetate(C₂₀H₂₁N₃O₃) were precisely measured with a high-precision automated adiabatic calorimeter over the temperature range between 81 to 380 K. The compound was observed to melt at(349.38±0.04) K. The molar enthalpy Δ_fusH_m, and entropy of fusion, Δ_fusS_m of the compound were determined to be (34.279±10) J/mol, (98.13±0.05) J/(mol•K), respectively. The thermodynamic function data relative to the reference temperature(298.15 K) were calculated based on the heat capacities measurements in the temperature range from 80 K to 325 K.

Kinetics of Adsorption of Disperse Dyes at Cationic Bentonites

LI Qian, YUE Qin-Yan*, GAO Bao-Yu, LIU Li-Li

2006, 27(6):  1113-1117.  doi:

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Kinetics of adsorption of each of disperse dyes, namely, Disperse Yellow Brown S-2RFL(DYB S-2RFL), Disperse Red S-R(DR S-R), Disperse Blue SBL(DB SBL) and Disperse Yellow SE-6GFL(DY SE-6GFL) onto cationic bentonites(EPI-DMA/Bt, PD/Bt, CTMAB/Bt) were studied. The results show that the adsorption processes follow a two-step first-order kinetic rate equation with two different rate constants(k₁, k₂), energies of activation(E_a1, E_a2), enthalpies of activation(ΔH^*₁, ΔH^*₂) and entropies of activation(ΔS^*₁, ΔS^*₂). With the increasing of the alkyl of cationic intercalary reagents, the kinetic rate constants also increase, which indicate that the large space between layers, more hydrophobic interlayer environment and more positive charges of cationic bentonites are important influence factors to accelerate adsorption. It has been found that for both the adsorption kinetic steps, ΔH^*₁＜-T_avΔS^*₁ ,ΔH^*₂＜-T_avΔS^*₂ and ΔG^*＞0, which means that the influence of the entropy is more remarkable than the enthalpy in the activation reaction.

Effects of Acetic Acid on Product Selectivity in Gas Phase Oxidative Dehydrogenation of Cyclohexane

ZHU Yu-Jun^1,2, LI Jing¹, YANG Xiang-Guang^1*, WU Yue¹

2006, 27(6):  1118-1120.  doi:

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The effect of adding acetic acid on the product distribution in gas phase oxidative dehydrogenation of cyclohexane over α₁-VOPO₄ catalyst was investigated. The role of acetic acid in the reaction process was put forward. The proposed mechanism is that acetic acid take precedence of cyclohexane adsorbing on the active sites of α₁-VOPO₄ catalyst to form isolated active site. Thus, cyclohexene species can desorb quickly from the active sites, avoiding its deep oxidation dehydrogenation. Almost 100% selectivity to cyclohexene could be obtained when the molar ratio of acetic acid to cyclohexane was 12.9∶1 at 450 ℃, the conversion of cyclohexane was 6.9%.

Preparation of DTMS Films on LY12 Aluminum Alloys via Electrochemical
Deposition and Their Anti\|corrosive Performance

HU Ji-Ming^1*; LIU Liang¹; ZHANG Jian-Qing^1,2; CAO Chu-Nan^1,2

2006, 27(6):  1121-1125.  doi:

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Dodecyltrimethoxysilane(DTMS) films were prepared on LY12 aluminum alloys by electrochemical deposition. FTIR-RA tests showed that the DTMS films were successfully deposited through the chemical bonding between silane agent and Al alloys, i.e., by the formation of Si—O—Al bond. The corrosion inhibition of silane covered alloys was characterized by electrochemical impedance spectroscopy(EIS) measurements in NaCl solutions with a mass fraction of 3.5%. The results show that in comparison with those prepared at open\|circuit potential(OCP), the DTMS films deposited at cathodic potentials displayed an enhancement in protectiveness. Furthermore, a “critical potential”were observed, at which the films prepared showed the highest barrier performance. Scanning electron microscopy(SEM) image indicated a potential dependence of surface morphology of silane films. The highest compactness was obtained at the“critical potential”. The impedance models of DTMS covered Al alloys in corrosive solutions were also proposed in the present work.

Fabrication of Linear Aniline-DNA Complex Nanowires and DNA-templated Polyaniline Nanowires

YANG Tao; WEI Gang; NIU Li*; LI Zhuang

2006, 27(6):  1126-1130.  doi:

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In the present work, we developed a simple method for fabricating conducting polymer nanowires and characterized the resulted nanostructures mainly by atomic force microscopy(AFM). With DNA as templates, aniline-DNA complex nanowires were first produced in solution via a self-assembled process in which aniline monomers assembled on the entire DNA molecule surface from any direction. Compressed gas flow was then used to stretch the obtained aniline-DNA complex nanowires onto mica substrate. The linear aniline-DNA complex nanowire arrays can be directly observed from the AFM images. Finally, we got the polyaniline(PAn) nanowires based on the precursor of aniline-DNA complex nanowires through further chemical oxidative polymerization. The aniline-DNA complex nanowires and the polyaniline(PAn-DNA) nanowires both exhibit a low background on the unmodified mica substrates. This strategy can be adopted for constructing other conducting polymer nanowires.

Electrocatalytic Reduction of Carbon Monoxide on Cu, Fe, Brass Electrode in Solid Electrolyte Cells

HAO Jin-Ku*, CAO Ying-Yu, SHEN Yong-Li, ZHUGE Shang-Qi, BAI Dong-Hua

2006, 27(6):  1131-1134.  doi:

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A new electrolysis system was developed for the conversion of CO to formaldehyde and ethylene, in which the electrochemical reduction took place at the two-phase(gas/solid) interface on Cu, Fe and Brass electrodes with α-Zr(HPO₄)₂H₂O(ZrP) used as proton-conducting solid electrolyte at room temperature and atmospheric pressure. The products for eletroreduction of CO depended on the different metal electrodes and the current densities. Considerable faradic efficiency was observed for HCHO at Cu/ZrP cathode electrode over a wide range of current density. And the faradic efficiency of HCHO increased with the increase of the current density and approached 29.0% at a current density of 100 mA·cm^-2. The Cu/ZrP cathodic surface reaction mechanism was proposed, i.e., oxygencon-taining Cu…HCO was formed and the fine product HCHO was obtained. The faradic efficiency of C₂H₄ increased with the increase of the current density and approached 15.0% at a current density of 100 mA·cm^-2 on Fe/ZrP cathode electrode. The Fe/ZrP surface reaction mechanism was proposed, that was, radical coordinate Fe…H₂ was formed and the product C₂H₄ was obtained.

研究简报

Electroreduction Behavior of Coumarin in an Ionic Liquid(BMIMBF₄)

WANG Huan; XUE Teng; ZHANG Ai-Jian; ZHANG Li; LU Jia-Xing*

2006, 27(6):  1135-1137.  doi:

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The electrochemical reduction of coumarin at GC electrode in 1-n-butyl-3-methylimidazolium tetrafluoroborate(BMIMBF₄) room temperature ionic liquid is reported. Coumarin exhibits a one-electron, irreversible reduction to caroanion radical, and the latter species undergoes fast dimerization to dihydrodimer. The influences of scan rate, concentration and temperature were studied by cyclic voltammetry. The results show that the reaction is diffusion controlled. The diffusion coefficient D of coumarin in BMIMBF₄ from Chronocoulometry is 5.066×10^-7 cm²/s. Furthermore, the influences of water and substituting group during the electroreduction are discussed. These preliminary electrochemical experiments show encouraging results for the use of ionic liquids in a "green" electrochemistry.

Preparation of Porous Nano-nickel Oxide by Fast Precipitation and Its Capacitance Characteristics

ZHENG Ming-Bo¹; CAO Jie-Ming^1*; CHEN Yong-Ping¹; HE Ping¹;
TAO Jie¹; LIANG Yan-Yu²; LI Hu-Lin^1,2

2006, 27(6):  1138-1140.  doi:

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Ni(OH)₂ with a high specific surface area was synthesized by a facile fast precipitation method. Porous nano-NiO was obtained by calcining Ni(OH)₂ at 300 ℃. The NiO sample possesses a fine porous distribution at around 3-10 nm. The BET specific surface area and pore volume of this sample are 218.1 m²/g and 0.31 cm³/g, respectively. The electrochemical characteristics of the samples were studied by cyclic voltammetry and constant current charge/discharge. The specific capacitance of the NiO sample is about 255 F/g in the 2.0 mol/L KOH solution. The sample also has a fine electrochemical stability.

研究论文

Synthesis and Characterization of Novel Sulfonated Poly(arylene ether
ketone) as Proton Exchange Membrane for PEM Fuel Cell Application

KONG Ling-Huan^2,3, XIAO Min¹, WANG Lei^2,3, MENG Yue-Zhong^1,2*

2006, 27(6):  1141-1144.  doi:

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A novel sulfonated poly(arylene ether ketone) was successfully synthesized by the sulfonation of the polymer with chlorosulfonic acid. It was confirmed by ¹H NMR spectra that the sulfonic acid group had beenintroduced onto the para-position of the pendant phenyl rings. The sulfonated polymers are very soluble in DMSO and other organic solvents, and can be readily cast into tough and transparent film. The results show that the membrane derived from the as-prepared polymers exhibits higher water absorption, superior thermal stability and higher proton conductive property than Nafion. The mechanical strength, oxidative stability and hydrolytic stability were tested and compared with those of Nafion.

Synthesis and Luminescent Property of a Novel Fluorescent Dual Sensitive Chitosan

GUAN Xiao-Lin, LIU Xing-Yu, SU Zhi-Xing*

2006, 27(6):  1145-1148.  doi:

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A novel method for attaching 3-epoxypropoxy fluorescein(EPF) to water soluble chitosan(GCS) and its dual sensitive quality of fluorescence were investigated. GCS bearing EPF was characterized by the methods of IR, ¹H NMR, UV and fluorescence spectra, respectively. The chemiluminescent and photophysical behavior of GCS-EPF were studied, and the pH and temperature dependences of fluorescence of GCS-EPF were investigated in detail. From the results, we found that the emission wavelengths of GCS-EPF in solid and film states were larger than that in solution state, which may be due to the formation of an excimer between chromophore moieties on a chitosan chain. At 0-60 ℃, the maximum fluorescence intensity of GCS-EPF decreased on heating and the relationship between fluorescence intensity and the change of temperature was linear; At pH=0-13.5, its fluorescence intensity increased with basification and completely disappeared at very acidic pH.

Preparation of Rhombohedral CdCO₃@SiO₂ Core-shell Particles and Hollow Rhombohedral SiO₂ Particles

HAN Kun, ZHAO Zhi-Hui, XIANG Zheng, WANG Yan-Ping, ZHANG Jun-Hu, YANG Bai*

2006, 27(6):  1149-1152.  doi:

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We report a facile method to coat rhombohedra CdCO₃ microparticles with SiO₂ directly by Stber seed growth method. CdCO₃@SiO₂ core-shell colloid particles were obtained, and the thickness of the SiO₂ shell can be modulated in a certain range by adjusting the amount of tetraethyl orthosilicate(TEOS) which was added into the system. As a result, a new species was found which can be coated with SiO₂ without surface modification. Furthermore, after removal CdCO₃ particles with hydrochloric acid, hollow rhombohedra SiO₂ particles were obtained which can be further used as microreactors and so on.

Preparation of Novel Naphthalenic Sulfonated Polyimide Proton Conductive Membrane

SHANG Yu-Ming^1_; XIE Xiao-Feng^1*; LIU Yang¹; XU Jing-Ming¹; MAO Zong-Qiang¹; ZHOU Qi-Feng²

2006, 27(6):  1153-1156.  doi:

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To prepare proton conductive membrane for DMFC, a novel sulfonated diamine 1,4-bis(4-amino-2-sulfonic-phenoxy)-benzene(DS-TBDA) was synthesized and polymerized with a non-sulfonated diamine(ODA) and naphthalene-1,4,5,8-tetracaboxylic dianhydride(NTDA) to get a series of naphalenic sulfonated polyimides(S-PI). The sulfonation degree of the polymers was controlled by changing the molar ratio of the monomers. The obtained SPI membrane was characterized by FTIR and the properties, such as water uptake, proton conductivity and methanol permeability, were investigated. With the increase of sulfonation degree, the proton conductivity and methanol permeability raise gradually. The proton conductivities of the SPI membranes are in a range of from 0.007 9 to 0.072 S/cm and the methanol permeability is less than 2.85×10^-7 cm²/s. The experiment result indicats they are great potential candidates for fuel cell applications.

Studies on Carbon Nanotube Surface Modified with Polystyrene

WANG Guo-Jian*; DONG Yue; QIU Jun; LIU Lin

2006, 27(6):  1157-1161.  doi:

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Polystyrene with a halogen atom at the chain end was prepared by means of atom transfer radical polymerization(ATRP). Then polystyrene with an azide group at the chain end was obtained through the azidization reaction. Finally, PSt 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 characterizing results of FTIR, XPS, UV, Raman spectrum and TEM show that the PSt was combined assuredly with carbon nanotube by the covalent bond. According to the results of TGA mensuration, the content of PSt on the surface of SWNT and MWNT is respectively estimated and more defects in structure of MWNT are favorable for chemical modification of CNTs.

Nonisothermal Crystallization Behavior of Poly(L-lactide)-Poly(ethylene glycol) Diblock Copolymer

YANG Jun-Liang; ZHAO Ting; CUI Ji-Jun; LIU Lei-Jing; ZHOU Yun-Chun;
LI Gao*; ZHOU En-Le; CHEN Xue-Si

2006, 27(6):  1162-1166.  doi:

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The nonisothermal crystallization behavior of poly(L-lactide)-poly(ethylene glycol)(PLLA-PEG) diblock copolymer was studied by means of real-time WAXD, DSC and POM, and Ozawa equation was used to analyze the kinetics of PLLA\|PEG under nonisothermal crystallization conditions. During the crystallization of the high-Tm block (PLLA), the low-Tm block(PEG) acts as a noncrystalline diluent, and the crystallization behavior of PLLA obeys the Ozawa theory. When the PEG block begins to crystallize, the PLLA phase is always partially solidified and the presence of the spherulitic microstructure of PLLA profoundly restricts its crystallization behavior, which results in that the overall crystallization process does not obey the Ozawa equation. Furthermore, the study of the crystalline morphology of PLLA-PEG at different cooling rates indicates that when the cooling rate is from low to high, the crystalline morphology undergoes a transformation from the ring-banded spherulites to the typical Maltese cross spherulites, which experiences the mixed crystalline morphologies of ring\|banded and typical Maltese cross spherulites, and the spherulitic size becomes smaller.

Preparation and Characters of Novel Support PEI/SiO₂ for the Immobilization of Penicillin Acylase

WANG Xu-Peng; GAO Bao-Jiao*; GUO Jian-Feng; ZHANG Li-Ping

2006, 27(6):  1167-1172.  doi:

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Polyethyleneimine(PEI) was coupled chemically to the surface of silica gel particles through the intermedium effect of γ\|chloropropyltrimethoxysilane, novel complex carrier PEI/SiO₂ for immobilizing penicillin acylase was prepared, and finally an immobilized penicillin acylase with a higher activity and stability was obtained. The influences of various factors on the preparation of the carrier were examined via measuring coupling amount of PEI on the compisite carrier. The chemical composition and structure of the surface of the composite carrier were characterized via IR and conductimetric titration. In order to explore the immobilization mechanism of the complex carrier for the penicillin acylase, the ζ potential of the support was determined before the enzyme was immobilized. The results show that the polyamine PEI can fully be coupled chemically to the surface of silica gel particles by the agency of γ-chloropropyltrimethoxysilane, and the linkage amount can reach 15%. The favorable reaction conditions are the reaction temperature is 90-94℃, the reaction time 5 h and the mass concentration 45-50 g/100 mL for PEI. Owing to a large quantity of amido contained on the macromolecular chains of PEI, there is not only chemical linkage, but also a great deal of physical adsorption during enzyme immobilization on the surface of PEI/SiO₂. The combination of a spot of chemical covalent linkage and a great deal of physical adsorption results in fast and stable immobilization, and excellent maintenance of constellation for penicillin acylase, so that the activity and activity recovery ratio of the immobilized enzyme are all higher. Moreover, the immobilized enzyme has a better continuous operating stability and its activity can keep at a level of 87.5% of fresh one all along after having been used for fifteen time repeatedly.

Sudies on Non-isothermal Melt Crystallization Kinetics in PET/PEN/DBS Blends

LI Gui-Juan^1,2*; XU Xiao-Duo¹; XU Xue-Li¹; YU Bao-Jie¹; LI Yi¹; ZHOU En-Le²

2006, 27(6):  1173-1177.  doi:

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Macrokinetic models, namly the modified Avrami, Ozawa and Zibicki models, were applied to study the non-isothermal melt crystallization process of PET/PEN/DBS blends by DSC measurement. The modified Avrami model was found to describe the experimental data fairly well. With the cooling rates in the range from 5 to 20 K/min, Ozawa model could be well used to describe the early stages of crystallization. However, Ozawa model did not fit the polymer blends during the late stages of crystallization, because it ignored the influence of secondary crystallization. The crystallization ability of the blends decreases with increasing the DBS content from analysis by using Ziabicki kinetic model, which is similar to the results based on calculation of the effective energy barrier of the blends.

Preparation of PVP Helical Fibres by Electrospinning and Study on the Mechanism of Helix Formation

DU Jian-Shi¹; YANG Qing-Biao¹; WANG Yong-Zhi¹; YANG Song-Tao¹; BAI Jie¹; WANG Shu-Gang¹; SONG Yan¹; LI Yao-Xian^1*; WANG Ce^2*

2006, 27(6):  1178-1181.  doi:

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Helical fibres of PVP were fabricated by electrospinning. The morphologies of helical fibre were observed by Scanning Electron Microscopy. PVP ethanol solutions with different mass fractions(12%, 14%, 16%, 20% and 24%) were electrospun at the voltage of 9 kV. With increase of PVP mass fraction, the morphologies of PVP fiber changed from straight, helical, folded to disordered form. Helical fibres were obtained when the mass fractions of PVP solution changed in the range of 16%-20%. The solutions were also electrospun at different voltages from 6 kV to 13 kV, respectively. The result show those regular helical fibres could be obtained in a wide voltage range when PVP solution with a mass fration of 20% was electrospun. The mechanism of the formation of helical fibre was discussed. Coulomb excluding force between static charge carried by fibres during the process of electrospinning was the main factor to form helical fibre.

Preparation and Characteristics of Floating-bioadhesive Microcapsules Containing Clarithromycin

ZHENG Jian-Hua¹; LIU Chao-Wu¹; BAO De-Cai^1,2; ZHAO Yan-Jun¹; MA Xiao-Jun^1*

2006, 27(6):  1182-1185.  doi:

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Floating-bioadhesive microcapsules containing clarithromycin were prepared by a combined method of emulsion solvent diffusion and internal/ion gelation for the treatment of Helicobacter pylori. Ethylcellulose microsphers(EMs) were prepared by the emulsion solvent diffusion method. EMs were coated with alginate and chitosan by the internal/ion gelation method to get alginate-ethylcellulose microcapsules(AEMs) and chitosan-alginate-ethylcellulose microcapsules(CAEMs). The drug efficiency and drug content of clarithromycin in CAEMs were determined to be 72.3%—78.2% and 7.1%—12.7%, respectively. CAEMs showed an obviously sustaining effect for more than 6h in vitro, and more than 70% of CAEMs floated in acetate buffer solution for 8 h in vitro. Furthermore, the in vitro remaining percentage of CAEMs in the stomach 4 h after the administration was 60.5%. The results suggest that floating-bioadhesive microcapsules might be a promising drug delivery system for the treatment of Helicobacter pylori infection.

研究简报

Microstructure of the Hybrid Core-shell Latex Synthesized by Emulsion
Copolymerization of 3-Trimethoxysilyl Propyl Methacrylate and Styrene

NI Ke-Fan; SHAN Guo-Rong*; WENG Zhi-Xue

2006, 27(6):  1186-1188.  doi:

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The microstructures of the hybrid core-shell latex synthesized by emulsion copolymerization of 3-trimethoxysilyl propyl methacrylate(MPS) and styrene were investigated. The polymers obtained under different operating conditions were characterized by 29Si solid state NMR, FTIR, DSC and elemental analysis.