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24 December 2006, Volume 22 Issue 6

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Content of Chemical Research in Chinese Universities Vol.22 No.6(2006)

2006, 22(6):  0-0.  doi:

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Preparation and Luminescence Behavior of CaSiO₃:Eu³⁺(Bi³⁺)

YANG Jing-hai, LIU Wen-yan, YANG Li-li, ZHANG Yong-jun, WANG Ya-xin, FAN Hou-gang

2006, 22(6):  671-674. 

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CaSiO₃:Eu_0.08³⁺Bi_0.002³⁺ with a monoclinic perovskite structure was synthesized by using sol-gel method, and its luminescence characteristics were investigated. From the excitation spectrum, it can be seen that the main peaks located at238, 396, 415, 437 and 359 nm correspond to the charge-transfer band of Eu³⁺-O^2- , the absorption transitions of ⁷F_0,1→⁵L₆,⁷F₀→⁵D₃,⁷F₁→⁵D₃ of Eu³⁺ ions, and ³P₁→¹S₀ of Bi³⁺ ions, respectively. When the samples were excited with a light of wavelength 359 or 395 nm, it can be seen from the emission spectrum that the electronic dipole transition located at 609 nm corresponding to ⁵D₀ →⁷F₂ of Eu³⁺ ions was stronger than the magnetic dipole transition located at 587 nm corresponding to ⁵D₀ →⁷F₁ of Eu³⁺ ions, which shows that more Eu³⁺ ions were located in nonreversion center lattices. The energy transfer from Bi³⁺ ions to Eu³⁺ ions in the phosphor was also discussed. The results show that Eu³⁺ ions could be well sensitized by Bi³⁺ ions, and the energy-transfer pattern between Bi³⁺ ions and Eu³⁺ ions was resonance energy transfer.

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Volume Contents of Chemical Research in Chinese Universities to Vol. 22(2006)

2006, 22(6):  0-0.  doi:

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Synthesis and Characterization of ZnS:Ag Nanocrystals Surface-capped with Thiourea

HUANG Feng-hua, PENG Yi-ru, LIN Cheng-fang

2006, 22(6):  675-678. 

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Ag⁺-doped ZnS nanocrystals surface-capped with thiourea(expressed as ZnS:Ag/thiourea) were synthesized through sol-gel method with thiourea as a surface modifier and characterized by X-ray diffraction(XRD), transmission electron microscope(TEM), X-ray fluorescence spectrum(XRF), infrared spectrum(IR), UV-Vis absorption spectrum(UV-Vis), and photoluminescence spectrum(PL). The results show that Ag⁺ ions are doped in ZnS nanocrystals, and the sulfur atoms in thiourea molecules coordinate with metal ions on the surface of the nanocrystals. The spherical ZnS:Ag/thiourea nanocrystals with an average diameter of 5 nm have good fluorescent characteristics, and therefore have great potential for use in molecular assembly and novel luminescence materials.

Preparation and Luminescence Behavior of CaSiO₃∶Eu³⁺(Bi³⁺)

YANG Jing-hai , LIU Wen-yan, , YANG Li-li, , ZHANG Yong-jun , WANG Ya-xin , FAN Hou-gang

2006, 22(6):  671-674.  doi:

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CaSiO₃:Eu³⁺_0.08Bi³⁺_0.002 with a monoclinic perovskite structure was synthesized by using sol-gel method, and its luminescence characteristics were investigated. From the excitation spectrum, it can be seen that the main peaks located at 238, 396, 415, 437 and 359 nm correspond to the charge-transfer band of Eu³⁺—O^2-, the absorption transitions of ⁷F_0,1→⁵L₆, ⁷F₀→⁵D₃, ⁷F₁→⁵D₃ of Eu³⁺ ions, and ³P₁→¹S₀ of Bi³⁺ ions, respectively. When the samples were excited with a light of wavelength 359 or 395 nm, it can be seen from the emission spectrum that the electronic dipole transition located at 609 nm corresponding to ⁵D₀→⁷F₂ of Eu³⁺ ions was stronger than the magnetic dipole transition located at 587 nm corresponding to ⁵D₀→⁷F₁ of Eu³⁺ ions, which shows that more Eu³⁺ ions were located in nonreversion center lattices. The energy transfer from Bi³⁺ ions to Eu³⁺ ions in the phosphor was also discussed. The results show that Eu³⁺ ions could be well sensitized by Bi³⁺ ions, and the energy-transfer pattern between Bi³⁺ ions and Eu³⁺ ions was resonance energy transfer.

Hydrothermal Synthesis and Thermal Stability of Natural Mineral Lindgrenite

BAO Ren-lie, KONG Zu-ping, GU Min, YUE Bin, WENG Lin-hong, HE He-yong

2006, 22(6):  679-683. 

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A natural mineral, lindgrenite Cu₃(MoO₄)₂(OH)₂ , was synthesized from a mixture of sodium molybdate, copper sulfate, and morpholine in water under autogenous pressure at 170 ℃. The crystal structure of the mineral was determined and the final refinement for 791 observed reflections with I＞2σ(I) gave R₁ =0.0205 and wR₂=0.0496. The thermal stability of the mineral was investigated by using TG-DTA and variable-temperature in situ X-ray diffraction(XRD) techniques. The crystalline Cu₃Mo₂O₉ was obtained when the mineral underwent thermal dehydration at a temperature ranging from 300 to 400 ℃, and the mixture of MoO₃ and CuO was formed through decomposition of Cu₃Mo₂O₉ at a temperature ranging from 650 to 700 ℃. Therefore, the structure of the mineral was thermally unstable at above 300 ℃, suggesting that Lindgrenite was likely formed via the hydrothermal route occurring in the nature.

Synthesis and Characterization of ZnS:Ag Nanocrystals Surface-capped with Thiourea

HUANG Feng-hua , PENG Yi-ru , LIN Cheng-fang

2006, 22(6):  675-678.  doi:

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Ag⁺-doped ZnS nanocrystals surface-capped with thiourea(expressed as ZnS：Ag/thiourea) were synthesized through sol-gel method with thiourea as a surface modifier and characterized by X-ray diffraction(XRD), transmission electron microscope(TEM), X-ray fluorescence spectrum(XRF), infrared spectrum(IR), UV-Vis absorption spectrum(UV-Vis), and photoluminescence spectrum(PL). The results show that Ag⁺ ions are doped in ZnS nanocrystals, and the sulfur atoms in thiourea molecules coordinate with metal ions on the surface of the nanocrystals. The spherical ZnS∶Ag/thiourea nanocrystals with an average diameter of 5 nm have good fluorescent characteristics, and therefore have great potential for use in molecular assembly and novel luminescence materials.

Fluorescence Properties of Porphyrin Dimers Incorporating an Anhydride Linker

FA Huan-bao, YIN Wei, ZHENG Wen-qi, LI Di, SHAN Ning, WANG Xing-qiao

2006, 22(6):  684-687. 

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A preliminary study on a novel free base porphyrin dimer and a zinc prophyrin dimer by comparing their fluorescence properties with those of the corresponding monomers is presented. The fluorescence intensity of the free base dimer is five times higher than that of the monomer, but the fluorescence intensity of the zinc porphyrin dimer is nearly similar to that of the zinc porphyrin monomer. The emission spectra show that energy transfer occurs between the two units.

Hydrothermal Synthesis and Thermal Stability of Natural Mineral Lindgrenite

BAO Ren-lie , KONG Zu-ping , GU Min , YUE Bin , WENG Lin-hong , HE He-yong

2006, 22(6):  679-683.  doi:

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A natural mineral, lindgrenite Cu₃(MoO₄)₂(OH)₂, was synthesized from a mixture of sodium molybdate, copper sulfate, and morpholine in water under autogenous pressure at 170 ℃. The crystal structure of the mineral was determined and the final refinement for 791 observed reflections with I>2σ(I) gave R₁=0.0205 and wR₂=0.0496. The thermal stability of the mineral was investigated by using TG-DTA and variable-temperature in situ X-ray diffraction(XRD) techniques. The crystalline Cu₃Mo₂O₉ was obtained when the mineral underwent thermal dehydration at a temperature ranging from 300 to 400 ℃, and the mixture of MoO₃ and CuO was formed through decomposition of Cu₃Mo₂O₉ at a temperature ranging from 650 to 700 ℃. Therefore, the structure of the mineral was thermally unstable at above 300 ℃, suggesting that Lindgrenite was likely formed via the hydrothermal route
occurring in the nature.

12-Ring Network Coordination Polymer—— {[Cu(C₄N₂H₁₀)₄]₂·H₄V₄O₁₄}_n Formed by Linking cyclo-[H₄V₄O₁₄]^4- with Cu(C₄N₂H₁₀)₄²⁺ Cation Clusters

LI Ya-feng, ZHANG Li-mei, WU Lei-lei, WANG Sheng-hai, WANG Hai-lian, SHANG Xuan-xuan

2006, 22(6):  688-691. 

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A novel 12-ring network coordination polymer, {[Cu(C₄N₂H₁₀)₄]₂H₄V₄O₁₄}_n(denoted as QUST-4), was hydrothermally synthesized and structurally determined by X-ray single-crystal diffraction analysis. QUST-4 was crystallized in a monoclinic system with space group P2₁/n. The parameters of the unit cell are a=1.0497(2) nm, b=1.6728(3) nm, c=1.2857(3) nm, β=94.14(3)°, V=2.2517(8) nm³, Z=4, D_cal = 1.841 Mg/m³, R₁=0.1071, and wR₃=0.2703. The largest difference peak and hole were2284 and -1040 e/nm³, respectively. The SBU(secondary building unit) of QUST-4 was a new cyclo- aggregate of polyoxovanadate cyclo-[H₄V₄O₁₄]^4-, different from cyclo-[V₄O₁₂]^4-, which was condensed from two tetrahedral and two trigonal bipyramids via alternate arrangement. Cu(piper)₄(piper=piperazine) group connected the cyclo-[V₄O₁₂]^4- anions to form the 12-ring network. The adjacent layers were linked by van der Walls forces.

Fluorescence Properties of Porphyrin Dimers Incorporating an Anhydride Linker

FA Huan-bao, YIN Wei, ZHENG Wen-qi, LI Di, SHAN Ning , WANG Xing-qiao

2006, 22(6):  684-687.  doi:

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A preliminary study on a novel free base porphyrin dimer and a zinc prophyrin dimer by comparing their fluorescence properties with those of the corresponding monomers is presented. The fluorescence intensity of the free base dimer is five times higher than that of the monomer, but the fluorescence intensity of the zinc porphyrin dimer is nearly similar to that of the zinc porphyrin monomer. The emission spectra show that energy transfer occurs between the two units.

Photoluminescence Properties of Two-dimensional Planar Layer and Three-dimensional Island Layer for ZnO Films Grown Using MOCVD

HUANG Ke-ke, HOU Chang-min, GAO Zhong-min, LI Xiang-shan, FENG Shou-hua, ZHANG Yuan-tao, ZHU Hui-chao, DU Guo-tong

2006, 22(6):  692-695. 

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ZnO(002) films with different thicknesses ranging from 7 to 300 nm were grown on sapphire(006) substrates via metal-organic chemical vapor deposition(MOCVD). The two-dimensional(2D) planar layer and the three-dimensional(3D) island layer were studied by using of X-ray diffraction(XRD) rocking curves and atomic force microscopy(AFM). The room temperature photoluminescence(PL) spectra show a blue shift of the peak positions of the ultraviolet(UV) emission with increasing film thickness. The blue shift is remarkably high(393-380 nm) when an increase in film thickness(7-15 nm) is accompanied by the change of structure from a2D planar layer to a 3D island layer. The PL spectra at 77 K also indicate that there are different transition mechanisms in the film thickness from a2D planar layer to a 3D island layer near the2D layer region.

12-Ring Network Coordination Polymer——{[Cu(C₄N₂H₁₀)₄]₂·H₄V₄O₁₄}_n Formed by Linking cyclo-[H₄V₄O_14<

LI Ya-feng , ZHANG Li-mei , WU Lei-lei , WANG Sheng-hai , WANG Hai-lian , SHANG Xuan-xuan

2006, 22(6):  688-691.  doi:

Abstract ( )  

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A novel 12-ring network coordination polymer, {[Cu(C₄N₂H₁₀)₄]₂H₄V₄O₁₄}_n(denoted as QUST-4), was hydrothermally synthesized and structurally determined by X-ray single-crystal diffraction analysis. QUST-4 was crystallized in a monoclinic system with space group P2₁/n. The parameters of the unit cell are a=1.0497(2) nm, b=1.6728(3) nm, c=1.2857(3) nm, β=94.14(3)°, V=2.2517(8) nm³, Z=4, D_cal= 1.841 Mg/m³, R₁=0.1071, and wR₃=0.2703. The largest difference peak and hole were 2284 and -1040 e/nm³, respectively. The SBU(secondary building unit) of QUST-4 was a new cyclo-aggregate of polyoxovanadate cyclo-[H₄V₄O₁₄]^4-, different from cyclo-[V₄O₁₂]^4-, which was condensed from two tetrahedral and two trigonal bipyramids via alternate {arrangement.} Cu(piper)₄(piper=piperazine) group connected the cyclo-[H₄V₄O₁₄]^4- anions to form the 12-ring network. The adjacent layers were linked by van der Walls forces.

Application of Short Sequential Extraction Procedure(SSEP) for the Determination of Zn, Cu, and Cd Contents in Riverbed Sludge in Hejiagou, Harbin, China

LI Yu, WANG Zhe, ZHAO Wen-Jin

2006, 22(6):  696-702. 

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A short sequential extraction procedure(SSEP) was applied to the determination of more readily available metal fractions of Zn, Cu, and Cd in the riverbed sludge in Hejiagou, Harbin, China. From the results, a potential order of metal availability in seven sludge samples was proposed: Cd＜Cu＜Zn, and samples S₁,S₂, and S₄ were used for the determination of total Zn content, and sample S₃ used for the determination of total Cu content in the mobile and the mobilizable fractions showed the highest pollution risk. The results with regard to metal mobility in sludge samples were confirmed by the individual and global contamination factors that were calculated from the nonresidual and resi-dual metal contents. The results obtained from metal-release experiments after exposure of sludge to environmental conditions agreed well with those obtained from both SSEP and the individual and global contamination factors, indicating that the maximum metal release could be an additional factor to evaluate the heavy metal availability in contaminated sludge. A substantial time saving was achieved by using the metal-release method in the present study.

Photoluminescence Properties of Two-dimensional Planar Layer and Three-dimensional Island Layer for ZnO Films Grown Using MOCVD

HUANG Ke-ke , HOU Chang-min , GAO Zhong-min , LI Xiang-shan , FENG Shou-hua , ZHANG Yuan-tao , ZHU Hui-chao , DU Guo-tong

2006, 22(6):  692-695.  doi:

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ZnO(002) films with different thicknesses ranging from 7 to 300 nm were grown on sapphire(006) substrates via metal-organic chemical vapor deposition(MOCVD). The two-dimensional(2D) planar layer and the three-dimensional(3D) island layer were studied by using of X-ray diffraction(XRD) rocking curves and atomic force microscopy(AFM). The room temperature photoluminescence(PL) spectra show a blue shift of the peak positions of the ultraviolet(UV) emission with increasing film thickness. The blue shift is remarkably high(393—380 nm) when an increase in film thickness(7—15 nm) is accompanied by the change of structure from a 2D planar layer to a 3D island layer. The PL spectra at 77 K also indicate that there are different transition mechanisms in the film thickness from a 2D planar layer to a 3D island layer near the 2D layer region.

Study of Spectral Character of Alkali Metals Using Microwave Plasma Torch Simultaneous Spectrometer

FENG Guo-dong, WAN Yi, HUAN Yan-fu, JIANG Jie, LI Ming, CAO Yan-bo, YU Ai-min, JIN Qin-han

2006, 22(6):  703-707. 

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A microwave plasma torch(MPT) simultaneous spectrometer was used to study the spectral character and the matrix effect on alkali metal ions in solution. The main parameters were optimized. The microwave forward power was 100 W. The argon flow rate that was used to sustain the Ar-MPT included the flow rate of carrier gas and the flow rate of support gas, which were 0.8 and 1.0 L/min, respectively. The HCl concentration in the solution was 0.02 mol/L. The observation height was 9.0 mm. The detection limits of Li, Na, K, Rb, and Cs were 0.0003, 0.0004, 0.009, 0.07 and2.4 mg/L, respectively, and the results obtained by the Ar-MPT were compared with those obtained by argon inductively coupled plasma(Ar-ICP) and argon microwave induced plasma(Ar-MIP). The interference effects of several matrix elements were also studied.

Application of Short Sequential Extraction Procedure(SSEP) for the Determination of Zn, Cu, and Cd Contents in Riverbed Sludge in Hejiagou, Harbin, China


LI Yu , WANG Zhe , ZHAO Wen-Jin

2006, 22(6):  696-702.  doi:

Abstract ( )  

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A short sequential extraction procedure(SSEP) was applied to the determination of more readily available metal fractions of Zn, Cu, and Cd in the riverbed sludge in Hejiagou, Harbin, China. From the results, a potential order of metal availability in seven sludge samples was proposed: Cd<Cu<Zn, and samples S₁, S₂, and S₄ were used for the determination of total Zn content, and sample S₃ used for the determination of total Cu content in the mobile and the mobilizable fractions showed the highest pollution risk. The results with regard to metal mobility in sludge samples were confirmed by the individual and global contamination factors that were calculated from the nonresidual and resi-dual metal contents. The results obtained from metal-release experiments after exposure of sludge to environmental conditions agreed well with those obtained from both SSEP and the individual and global contamination factors, indicating that the maximum metal release could be an additional factor to evaluate the heavy metal availability in contaminated sludge. A substantial time saving was achieved by using the metal-release method in the present study.

Structural Analysis of Water-soluble Polysaccharide PIP₁ Extracted from the Cultured Mycelium of Phellinus igniarius

WU Ming-jiang, JIANG De-zhi, LIU Tie-mei, ZHANG Li-ping

2006, 22(6):  708-711. 

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Water-soluble crude polysaccharide(PIP) was extracted from cultured mycelium of the fungus Phellinus igniarius . After ethanol precipitation and sepharose CL-6B gel filtration, the fraction of PIP₁ was obtained, which was shown to be a homogeneous polysaccharide by means of high-performance liquid chromatography. The structure of PIP₁ was determined by using several methods. GC analysis indicates that PIP₁ is composed of the monosaccharides of glucose, galactose, and mannose. Their molar ratio is 3.70:4.06:1.00. The molar weight was estimated to be 17 kd via HPLC. IR, GC, partial hydrolysis with acid, periodate oxidation, Smith degradation, methylation, and GC-MS analysis were used for the structural analyses of PIP₁. The results show that PIP₁ has a small quantity of branch structure. The main glycosidic linkage of PIP₁ has a β -configuration. The main chain is made up of a large mass of glucose(1→3 ) and few mannose(1→4); the side chain is composed of glucose(1→3) and galactose(1→6); the nonreduced end is composed of galactose and glucose. The side chains are branched at 6-O of glucose(1→3,6) and mannose(1→4,6). On an average, there are three branches among20 residues. It is presumable that the existence of 1,3-linked Glc in the main and side chains is the main reason for its higher antitumor activity.

Study of Spectral Character of Alkali Metals Using Microwave Plasma Torch Simultaneous Spectrometer

FENG Guo-dong, WAN Yi, HUAN Yan-fu, JIANG Jie, LI Ming, CAO Yan-bo, YU Ai-min , JIN Qin-han

2006, 22(6):  703-707.  doi:

Abstract ( )  

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A microwave plasma torch(MPT) simultaneous spectrometer was used to study the spectral character and the matrix effect on alkali metal ions in solution. The main parameters were optimized. The microwave forward power was 100 W. The argon flow rate that was used to sustain the Ar-MPT included the flow rate of carrier gas and the flow rate of support gas, which were 0.8 and 1.0 L/min, respectively. The HCl concentration in the solution was 0.02 mol/L. The observation height was 9.0 mm. The detection limits of Li, Na, K, Rb, and Cs were 0.0003, 0.0004, 0.009, 0.07 and 2.4 mg/L, respectively, and the results obtained by the Ar-MPT were compared with those obtained by argon inductively coupled plasma(Ar-ICP) and argon microwave induced plasma(Ar-MIP). The interference effects of several matrix elements were also studied.

Fusion Proteins Cpn10-E^rns with Properties of Generating CSFV-Neutralized Antibodies

CHEN Yue, WANG Xuan-jun, CONG Xian-ling, ZHANG Pei-yin, WU X iu-li, WE IHong-fei, WANG Li, WAN Min, WANG Li-ying, YU Yong-li

2006, 22(6):  712-716. 

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When pigs are infected with classical swine fever virus (CSFV), the antibody primarily targets the structural glycoprotein E^rns of the virus. Previous investigations have demonstrated that E^rns has low or no virus neutralizing capacity. In this study, candidate subunit marker vaccine, chaperonin 10(Cpn10)-E^rns, which possess the property of generating neutralized antibodies against lethal challenge of virulent CSFV was developed. The gene of E^rns was isolated from Hog cholera lapinized virus (HCLV)-infected spleen cells of rabbits via RT-PCR method and fused to the downstream region of the cpn10 gene; the products of recombinant fusion protein (cpn10-E^rns) induced expression in Escherichia coli, and the products were purified by affinity chromatography. During the course of vaccination, the candidate vaccines cpn10-E^rns were used for the immunization of guinea pigs, and they induced a strong antibody response against cpn10-E^rns. The antibodies can be immobilized by coating inactivated CSFV particles, indicating that these antibodies can recognize CSFV. Neutralization assay was carried out on rabbits according to National Regulations on Veterinary Drug. The results clearly indicate that the typical fever of rabbits induced by the live attenuated HCLV could be inhibited by preincubation with the antisera (dilution 1:4) induced by cpn10-E^rns, but not inhibited by preincubation with the antisera induced only by E^rns. Analogous results were observed for the group of the rabbits immunized with cpn10-E^rns, which were protected against the typical fever induced by the challenge with HCLV. The findings of this study formed the basis of a new means for developing subunit marker vaccine against CSFV.

Structural Analysis of Water-soluble Polysaccharide PIP₁ Extracted from the Cultured Mycelium of Phellinus igniarius

WU Ming-jiang , JIANG De-zhi , LIU Tie-mei , ZHANG Li-ping

2006, 22(6):  708-711.  doi:

Abstract ( )  

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Water-soluble crude polysaccharide(PIP) was extracted from cultured mycelium of the fungus Phellinus igniarius. After ethanol precipitation and sepharose CL-6B gel filtration, the fraction of PIP₁ was obtained, which was shown to be a homogeneous polysaccharide by means of high-performance liquid chromatography. The structure of PIP₁ was determined by using several methods. GC analysis indicates that PIP₁ is composed of the monosaccharides of glucose, galactose, and mannose. Their molar ratio is 3.70∶4.06∶1.00. The molar weight was estimated to be 17 kd via HPLC. IR, GC, partial hydrolysis with acid, periodate oxidation, Smith degradation, methylation, and GC-MS analysis were used for the structural analyses of PIP₁. The results show that PIP₁ has a small quantity of branch structure. The main glycosidic linkage of PIP₁ has a β-configuration. The main chain is made up of a large mass of glucose(1→3) and few mannose(1→4); the side chain is composed of glucose(1→3) and galactose(1→6); the nonreduced end is composed of galactose and glucose. The side chains are branched at 6-O of glucose(1→3,6) and mannose(1→4,6). On an average, there are three branches among 20 residues. It is presumable that the existence of 1,3-linked Glc in the main and side chains is the main reason for its higher antitumor activity.

Synthesis and Characterization of Novel 4-Methyl-3-isoxazolidinone Derivatives

GAO Fei-fei, ZHANG Guang-liang, ZHENG Liang-yu, LI Yao-xian, ZHANG Suo-qin

2006, 22(6):  717-720. 

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A novel type of acetohydroxyacid synthase inhibitors, 4-methyl-3-isoxazolidinone derivatives of sulfonylurea, was designed and synthesized. The structures of these compounds were confirmed by using MS, NMR, and elemental analysis. The results of preliminary active tests indicate that the compounds show a herbicidal activity.

Fusion Proteins Cpn10-E^rns with Properties of Generating CSFV-Neutralized Antibodies

CHEN Yue, , WANG Xuan-jun , CONG Xian-ling, , ZHANG Pei-yin , WU Xiu-li , WEI Hong-fei , WANG Li , WAN Min , WANG Li-ying , YU Yong-li

2006, 22(6):  712-716.  doi:

Abstract ( )  

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When pigs are infected with classical swine fever virus (CSFV), the antibody primarily targets the structural glycoprotein E^rns of the virus. Previous investigations have demonstrated that E^rns has low or no virus neutralizing capacity. In this study, candidate subunit marker vaccine, chaperonin 10(Cpn10)-E^rns, which possess the property of generating neutralized antibodies against lethal challenge of virulent CSFV was developed. The gene of E^rns was isolated from Hog cholera lapinized virus (HCLV)-infected spleen cells of rabbits via RT-PCR method and fused to the downstream region of the cpn10 gene; the products of recombinant fusion protein (cpn10-E^rns) induced expression in Escherichia coli, and the products were purified by affinity chromatography. During the course of vaccination, the candidate vaccines cpn10-E^rns were used for the immunization of guinea pigs, and they induced a strong antibody response against cpn10-E^rns. The antibodies can be immobilized by coating inactivated CSFV particles, indicating that these antibodies can recognize CSFV. Neutralization assay was carried out on rabbits according to National Regulations on Veterinary Drug. The results clearly indicate that the typical fever of rabbits induced by the live attenuated HCLV could be inhibited by preincubation with the antisera (dilution 1∶4) induced by cpn10-E^rns, but not inhibited by preincubation with the antisera induced only by E^rns. Analogous results were observed for the group of the rabbits immunized with cpn10-E^rns, which were protected against the typical fever induced by the challenge with HCLV. The findings of this study formed the basis of a new means for developing subunit marker vaccine against CSFV.

Chemoenzymatic Synthesis of Cellular Adhesion Tripeptide RGD Precursor in Organic Media

WANG Hua, ZHAO Mi-feng, PU Li-mei, DING Wei, HUANG Yi-bing, HOU Rui-zhen, ZENG Hong-bin, XU Li, ZHANG Xue-zhong

2006, 22(6):  721-726. 

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Chemoenzymatic synthesis of tripeptide Bz-RGD-(OEt)₂ was conducted in this study. First, the free dipeptide Gly-Asp was synthesized via a novel chemical method, wherein only L-aspartic acid was used and was followed by the esterification of Gly-Asp. The formation of the linkage between the third amino acid Bz-Arg-OEt and Gly-Asp-(OEt)₂ was completed by using the enzymatic method in organic media. The effects of several factors such as pH, the water content, triethylamine(TEA), the molar ratio of the substrates, and the reaction time on the yield of Bz-RGD-(OEt)₂ were examined. It was obtained that the optimum conditions for Bz-RGD-(OEt)₂ synthesis in an ethanol/Tris-HCl buffer system(volume ratio 93:7) were as follows; pH=8.0; temperature, 30 ℃; reaction time, 7 h. The tripeptide yield was 75.2%.

Synthesis and Characterization of Novel 4-Methyl-3-isoxazolidinone Derivatives

GAO Fei-fei , ZHANG Guang-liang , ZHENG Liang-yu , LI Yao-xian , ZHANG Suo-qin

2006, 22(6):  717-720.  doi:

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A novel type of acetohydroxyacid synthase inhibitors, 4-methyl-3-isoxazolidinone derivatives of sulfonylurea, was designed and synthesized. The structures of these compounds were confirmed by using MS, NMR, and elemental analysis. The results of preliminary active tests indicate that the compounds show a herbicidal activity.


20(S)-20-O-Camptothecin β-Aminopropionate: Novel Synthesis and Antitumor Activity in vitro

LI Yu-yan, YOU Qi-dong, WANG Lei, CHEN Sheng, CHEN Xiao-guang, LI Yan, LI Hong-yan

2006, 22(6):  727-731. 

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To improve the biological anticancer activity of 20(S)-camptothecin, a novel class of 20(S)-20-O-camptothecin β-aminopropionates were designed and synthesized with camptothecins as the starting materials, through acylation with acryloyl chloride followed by Michael′s addition. Twelve esters, 1a-1d, 4a-4d and 5a-5d, were synthesized and evaluated by using MTT assay method. The results demonstrate that all these compounds show a potential cytotoxicity on KB, HT-29, HCT-8, and Bel7402 tumor cell lines. Some compounds, 1d, 4c, 5b, 5c and 5d, show a higher cytoto-xicity on KB and HCT-8 compared with camptothecin.

Chemoenzymatic Synthesis of Cellular Adhesion Tripeptide RGD Precursor in Organic Media


WANG Hua , ZHAO Mi-feng , PU Li-mei , DING Wei , HUANG Yi-bing , HOU Rui-zhen , ZENG Hong-bin , XU Li , ZHANG Xue-zhong

2006, 22(6):  721-726.  doi:

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Chemoenzymatic synthesis of tripeptide Bz-RGD-(OEt)₂ was conducted in this study. First, the free dipeptide Gly-Asp was synthesized via a novel chemical method, wherein only L-aspartic acid was used and was followed by the esterification of Gly-Asp. The formation of the linkage between the third amino acid Bz-Arg-OEt and Gly-Asp-(OEt)₂ was completed by using the enzymatic method in organic media. The effects of several factors such as pH, the water content, triethylamine(TEA), the molar ratio of the substrates, and the reaction time on the yield of Bz-RGD-(OEt)₂ were examined. It was obtained that the optimum conditions for Bz-RGD-(OEt)₂ synthesis in an ethanol/Tris-HCl buffer system(volume ratio 93∶7) were as follows: pH=8.0; temperature, 30 ℃; reaction time, 7 h. The tripeptide yield was 75.2%.

Electrospray Ionization Mass Spectra of Amino Acid Methyl Ester 5′-Phosphoramidates of 2′,3′-Isopropylideneuridine

CHEN Wei-zhu, GAO Yu-xing, BAI Yong-gang, HAN Da-xiong, ZHAO Yu-fen

2006, 22(6):  732-737. 

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Amino acid methyl ester phosphates were synthesized and determined by using positive-ion mode electrospray ionization mass spectrometry(ESIMS) in combination with multistage tandem mass spectrometry. The fragmentation pathways were investigated, and it was observed that most fragment ions contained the phosphoryl group. It was interesting to observe that the fragmentation pathways of the protonated molecule show some differences when compared with those of the sodium ion adduct. The methoxy group of amino acid methyl ester can migrate from the carbonyl group to the phosphoryl group in the sodium ion adduct.

20(S)-20-O-Camptothecin β-Aminopropionate: Novel Synthesis and Antitumor Activity in vitro

LI Yu-yan , YOU Qi-dong , WANG Lei , CHEN Sheng , CHEN Xiao-guang , LI Yan , LI Hong-yan

2006, 22(6):  727-731.  doi:

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To improve the biological anticancer activity of 20(S)-camptothecin, a novel class of 20(S)-20-O-camptothecin β-aminopropionates were designed and synthesized with camptothecins as the starting materials, through acylation with acryloyl chloride followed by Michael′s addition. Twelve esters, 1a—1d, 4a—4d and 5a—5d, were synthesized and evaluated by using MTT assay method. The results demonstrate that all these compounds show a potential cytotoxicity on KB, HT-29, HCT-8, and Bel7402 tumor cell lines. Some compounds, 1d, 4c, 5b, 5c and 5d, show a higher cytotoxicity on KB and HCT-8 compared with camptothecin.

Synthesis and Characterization of Novel Thiosemicarbazones Bearing Sugar Moieties

YANG Bo, ZHANG Shu-sheng, LI Hui-xiang

2006, 22(6):  738-741. 

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Six novel thiosemicarbazones containing sugar and thiosemicarbazide moieties were synthesized by a five-step procedure using D-galactose and D-xylose as the starting materials and the corresponding glycosyl isothiocyanates as the intermediates. The target compounds were characterized by IR, ¹H NMR, and elemental analysis. The coupling constants between H1 and H2 in the sugar rings, all fall within the range of J=9.2-10.0 Hz, confirming the β-configuration of the compounds.

Electrospray Ionization Mass Spectra of Amino Acid Methyl Ester 5'-Phosphoramidates of 2',3'-Isopropylideneuridine

CHEN Wei-zhu, , GAO Yu-xing , BAI Yong-gang , HAN Da-xiong , ZHAO Yu-fen

2006, 22(6):  732-737.  doi:

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Amino acid methyl ester phosphates were synthesized and determined by using positive-ion mode electrospray ionization mass spectrometry(ESIMS) in combination with multistage tandem mass spectrometry. The fragmentation pathways were investigated, and it was observed that most fragment ions contained the phosphoryl group. It was interesting to observe that the fragmentation pathways of the protonated molecule show some differences when compared with those of the sodium ion adduct. The methoxy group of amino acid methyl ester can migrate from the carbonyl group to the phosphoryl group in the sodium ion adduct.

Synthesis of Hydroxystilbene Derivatives and their Antioxidant Activity by DPPH Method

LI Yue-qing, SONG Qi-ling, CHEN Ping-ping, ZHAO Wei-jie, WANG Shi-sheng

2006, 22(6):  742-746. 

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Five hydroxystilbene derivatives were synthesized and their structures were determined using high-resolution mass spectrometry, ¹H NMR, and IR. In this study, the antioxidant activities of eight hydroxystilbenes(five synthesized hydroxystilbene derivatives and three other compounds) were evaluated with the free radical scavenging model 1,1-diphenyl-2-picrylhydrazyl. It was observed that there exists a very significant linear relationship between the reciprocal of the EC₅₀ value of each of the compounds and the maximum wavelength of the ultraviolet absorption peaks. It is believed that this result will be helpful for the further synthesis of such antioxidants.

Synthesis and Characterization of Novel Thiosemicarbazones Bearing Sugar Moieties

YANG Bo, ZHANG Shu-sheng , LI Hui-xiang

2006, 22(6):  738-741.  doi:

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Six novel thiosemicarbazones containing sugar and thiosemicarbazide moieties were synthesized by a five-step procedure using D-galactose and D-xylose as the starting materials and the corresponding glycosyl isothiocyanates as the intermediates. The target compounds were characterized by IR, ¹H NMR, and elemental analysis. The coupling constants between H1 and H2 in the sugar rings, all fall within the range of J=9.2—10.0 Hz, confirming the β-configuration of the compounds.

Synthesis, Structure Characterization, and Cu²⁺ Recognition of 3-{[3-(Phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one

LI Xue-mei, ZENG Cheng-chu, NIU Li-ting, YAN Hong, ZHENG Da-wei, ZHONG Ru-gang

2006, 22(6):  747-752. 

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Aryl diketo acid derivatives are one of the most promising HIV-1 integrase(IN) inhibitors. With a view to substitute the critical diketo acid pharmacophore with the diketo benzimidazole unit, the coupling reaction of compound 4 with o-phenylenediamine was carried out. However, the reaction product, compound 5, was confirmed to be 3-{[3-(phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one rather than the2-benzimidazole derivative by using X-ray diffraction. Owing to its low solubility in water, the evaluation of the anti-HIV IN activity of the synthesized compound 5 could not be carried out. Consequently, the ion-binding properties of compound 5 in the absence of HIV-1 IN were investigated with UV-Vis spectroscopy in organic solvents. The results show that such a compound can selectively recognize Cu²⁺ .

Synthesis of Hydroxystilbene Derivatives and their Antioxidant Activity by DPPH Method

LI Yue-qing, SONG Qi-ling, CHEN Ping-ping, ZHAO Wei-jie , WANG Shi-sheng

2006, 22(6):  742-746.  doi:

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Five hydroxystilbene derivatives were synthesized and their structures were determined using high-resolution mass spectrometry, ¹H NMR, and IR. In this study, the antioxidant activities of eight hydroxystilbenes(five synthesized hydroxystilbene derivatives and three other compounds) were evaluated with the free radical scavenging model 1,1-diphenyl-2-picrylhydrazyl. It was observed that there exists a very significant linear relationship between the reciprocal of the EC₅₀ value of each of the compounds and the maximum wavelength of the ultraviolet absorption peaks. It is believed that this result will be helpful for the further synthesis of such antioxidants.

Mass Spectrometric Fragmentation of 1,8-Bis[4-substituted-(oxazolin-2-yl)] anthracenes: Ring-contraction Rearrangement of Oxazoline Ring under Electron-Impact Ionization Conditions

JIAO Peng, MA Lin-ge, ZHANG Qi-han, XU Jia-xi

2006, 22(6):  753-755. 

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The mass spectrometric fragmentation of 1,8-bis[4-substituted(oxazolin-2-yl)] anthracenes(AnBOXes) was investigated by using mass-analyzed ion kinetic energy spectrometry under electron-impact ionization conditions. All the compounds could undergo a ring contraction by the loss of an RCH=CH₂ molecule to form 1-oxazirinyl-8-(oxazolin-2-yl) anthracene ions, which could further lose an R radical, followed by the loss of oxazoline. These ions could also eliminate an R radical and subsequently undergo ring-contraction rearrangements to lose a CHCH₂O fragment and an epoxide molecule, respectively. The ions that are formed could further lose CHCH₂O and CH₂=CH fragments. Several ring-contraction rearrangements of the oxazoline ring were observed under electron-impact ionization conditions.

Synthesis, Structure Characterization, and Cu²⁺ Recognition of 3-{[3-(Phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one

LI Xue-mei, ZENG Cheng-chu, NIU Li-ting, YAN Hong, ZHENG Da-wei , ZHONG Ru-gang

2006, 22(6):  747-752.  doi:

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Aryl diketo acid derivatives are one of the most promising HIV-1 integrase(IN) inhibitors. With a view to substitute the critical diketo acid pharmacophore with the diketo benzimidazole unit, the coupling reaction of compound 4 with o-phenylenediamine was carried out. However, the reaction product, compound 5, was confirmed to be 3-{[3-(phenylsulfonamido)benzoyl]methylidene}-3,4-dihydroquinoxaline-2(1H)-one rather than the 2-benzimidazole derivative by using X-ray diffraction. Owing to its low solubility in water, the evaluation of the anti-HIV IN activity of the synthesized compound 5 could not be carried out. Consequently, the ion-binding properties of compound 5 in the absence of HIV-1 IN were investigated with UV-Vis spectroscopy in organic solvents. The results show that such a compound can selectively recognize Cu²⁺.

Mass Spectral Fragmentation of (S,S)-N,N′-Bis [1-(hydroxymethyl)alkyl]anthracene/Naphthalene-1,8-dicarboxamides under Electron Impact Ionization Conditions

JIAO Peng, ZHANG Qi-han, XU Jia-xi

2006, 22(6):  756-759. 

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The mass spectrometric fragmentation of(S,S)-N,N′-bis[1-(hydroxymethyl)alkyl]anthracene/naphthalene-1,8-dicarboxamides was investigated with the aid of mass-analyzed ion kinetic energy spectrometry and the elemental compositions of important fragment ions were determined by accurate mass measurement under electron impact ionization conditions. All the compounds could eliminate formaldehyde. The [M-CH₂O] ions could also eliminate imine, aziridine, aziridinone,2-amonoalkan-1-ol, water, and other fragments. Several cyclizations were observed under electron impact ionization.

Mass Spectrometric Fragmentation of 1,8-Bis[4-substituted-(oxazolin-2-yl)] anthracenes: Ring-contraction Rearrangement of Oxazoline Ring under Electron-Impact Ionization Conditions

JIAO Peng, MA Lin-ge, ZHANG Qi-han , XU Jia-xi

2006, 22(6):  753-755.  doi:

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The mass spectrometric fragmentation of 1,8-bis[4-substituted(oxazolin-2-yl)] anthracenes(AnBOXes) was investigated by using mass-analyzed ion kinetic energy spectrometry under electron-impact ionization conditions. All the compounds could undergo a ring contraction by the loss of an RCH—CH₂ molecule to form 1-oxazirinyl-8-(oxazolin-2-yl) anthracene ions, which could further lose an R radical, followed by the loss of oxazoline. These ions could also eliminate an R radical and subsequently undergo ring-contraction rearrangements to lose a CHCH₂O fragment and an epoxide molecule, respectively. The ions that are formed could further lose CHCH₂O and CH₂==CH fragments. Se-veral ring-contraction rearrangements of the oxazoline ring were observed under electron-impact ionization conditions.

Synthesis and Crystal Structure of 5-N-#em/em#-Propyl-2-(2′-nitrobenzenesulfonyl)-glutamine

XIAO Yong-jun, WANG Jian-guo, WANG Bao-lei, LI Zheng-ming, SONG Hai-bin

2006, 22(6):  760-762. 

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The title compound, 5-N-#em/em#-propyl-2-(2′-nitrobenzenesulfonyl)-glutamine, was synthesized and its structure was confirmed by IR, MS, ¹H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P2(1), with α=0.69281(11) nm,b=0.76508(12),c=1.5843(3) nm,α=90°,β=90.941(3)°,γ=90°,V=0.8397(2) nm³,Z=2,Dc=1.477 g/cm³,μ=0.236 mm^-1 , F(000)=392, R=0.0297, and wR=0.0664.

Mass Spectral Fragmentation of (S,S)-N,N'-Bis[1-(hydroxymethyl)alkyl]anthracene/Naphthalene-1,8-dicarboxamides under Electron Impact Ionization Conditions

JIAO Peng, ZHANG Qi-han , XU Jia-xi

2006, 22(6):  756-759.  doi:

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The mass spectrometric fragmentation of (S,S)-N,N’-bis[1-(hydroxymethyl)alkyl]anthracene/naphthalene-1,-8-dicarboxamides was investigated with the aid of mass-analyzed ion kinetic energy spectrometry and the elemental compositions of important fragment ions were determined by accurate mass measurement under electron impact ionization conditions. All the compounds could eliminate formaldehyde. The [M-CH₂O] ions could also eliminate imine, aziridine, aziridinone, -2-amonoalkan-1-ol, water, and other fragments. Several cyclizations were observed under -electron Impact ionization.

Synthesis and Crystal Structure of 2-tert-Butyl-5-(4-tert-butylbenzylthio)-4-chloropyridazin-3(2H)-one

XU Liang-zhong, YU Guan-ping, XU Zhong-jie, ZHANG Gong-sheng, ZHAI Zhi-wei

2006, 22(6):  763-764. 

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The title compound,2-tert-butyl-5(4-tert-butylbenzylthio)-4-chloropyridazin-3(2H)-one, was synthesized from 1-tert-butylhydrazine, (Z)-2,3-dichloro-3-formylacrylic acid and (4-tert-butylphenyl)methanethiol in several steps. It crystallized in an orthorhombic space group Pnma with M_r=364.93(C₁₉H₂₅CN₂OS), a=1.0091(2) nm, b=0.7076(2) nm, c=2.8103(5) nm, V=2.0066(6) nm³, Z=4, D_c=1.192 g/cm³ , F(000)=765, μ=0.301 mm^-1 , final R₁=0.0665, and wR=0.1913 for 1927 unique reflections. Inter-and intramolecular hydrogen bond C-H…O interactions stabilize the structure.

Synthesis and Crystal Structure of 5-N-i-Propyl-2-(2'-nitrobenzenesulfonyl)-glutamine

XIAO Yong-jun, WANG Jian-guo, WANG Bao-lei, LI Zheng-ming , SONG Hai-bin

2006, 22(6):  760-762.  doi:

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The title compound, 5-N-i-propyl-2-(2’-nitrobenzenesulfonyl)-glutamine, was synthesized and its structure was confirmed by IR, MS, ¹H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P2(1), with a=0.69281(11) nm, b=0.76508(12), c=1.5843(3) nm, α=90°, β=90.941(3)°, γ=90°, V=0.8397(2) nm³, Z=2, D_c=1.477 g/cm³, μ=0.236 mm^-1, F(000)=392, R=0.0297, and wR=0.0664.

Synthesis, Crystal Structure, and Biological Activities of 2-Oxo-2-aryl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate

XU Liang-zhong, ZHOU Kai, HU Zhi-qiang, BI Wen-zhao

2006, 22(6):  765-767. 

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The two title compounds,2-oxo-2-p-tolyl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate(compound 3a) and2-oxo-2-p-biphenyl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate(compound 3b), were synthesized and identified by IR, EA and ¹H NMR spectra. The crystal structure of compound 3b was determined by X-ray diffraction analysis. The compound crystallized in a monoclinic system of space group P2₁/c with M_r =398.47(C23H18N4OS),a=0.8769(2) nm,b=1.1924(2) nm, c=2.0440(6) nm,β=109.66(3)°,V=2.0126(8) nm³,Z=4, D_c=1.315 g/cm³, F(000)=832,μ=0.183 mm^-1, final R₁ =0.0819. The biological test result shows that the two title compounds exhibit certain fungicidal activities.

Synthesis and Crystal Structure of 2-tert-Butyl-5-(4-tert-butylbenzylthio)-4-chloropyridazin-3(2H)-one

XU Liang-zhong, YU Guan-ping, XU Zhong-jie, ZHANG Gong-sheng , ZHAI Zhi-wei

2006, 22(6):  763-764.  doi:

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The title compound, 2-tert-buty-5(4-tert-butylbenzylthio)-4-chloropyridazin-3(2H)-one, was synthesized from 1-tert-butylhydrazine, (Z)-2,3-dichloro-3-formylacrylic acid and (4-tert-butylphenyl)methanethiol in several steps. It crystallized in an orthorhombic space group Pnma with M_r=364.93(C₁₉H₂₅ClN₂OS), a=1.0091(2) nm, b=0.7076(2) nm, c=2.8103(5) nm, V=2.0066(6) nm³, Z=4, D_c=1.192 g/cm³, F(000)=765, μ=0.301 mm^-1, final R₁=0.0665, and wR=0.1913 for 1927 unique reflections. Inter- and intramolecular hydrogen bond C―H…O interactions stabilize the structure.

Synthesis, Dimeric Crystal Structure, and Biological Activities of N-(4-Methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N-(2-trifluoromethyl-phenyl)-guanidine

HE Feng-qi, WANG Bao-lei, LI Zheng-ming

2006, 22(6):  768-771. 

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The title compound, N-(4-methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N′-(2-trifluoromethyl-phenyl)-guanidine, was synthesized and its structure was confirmed by using IR, MS, ¹H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has a weak herbicidal activity.

Synthesis, Crystal Structure, and Biological Activities of 2-Oxo-2-aryl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate

XU Liang-zhong, ZHOU Kai, HU Zhi-qiang , BI Wen-zhao

2006, 22(6):  765-767.  doi:

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The two title compounds, 2-oxo-2-p-tolyl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate(compound 3a) and 2-oxo-2-p-biphenyl-1-(1,2,4-triazol-1-yl)ethyl phenylcarbamodithioate(compound 3b), were synthesized and -identified by IR, EA and ¹H NMR spectra. The crystal structure of compound 3b was determined by X-ray diffraction analysis. The compound crystallized in a monoclinic system of space group P2₁/c with M_r=398.47(C₂₃H₁₈N₄OS), a=0.8769(2) nm, b=1.1924(2) nm, c=2.0440(6) nm, β=109.66(3)°, V=2.0126(8) nm³, Z=4,D_c=1.315 g/cm³, F(000)=832, μ=0.183 mm^-1, final R₁=0.0819. The biological test result shows that the two title compounds exhibit certain fungicidal activities.

Apoptotic Effects of Hypocrellin A on HeLa Cells

FEI Xiao-fang, CHEN Jie, ZHENG Ke-yan, WU Wei, SUN Su-juan, WANG Li, MA Lan, LI Cong, TENG Li-rong

2006, 22(6):  772-775. 

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Hypocrellin A(HA), a photosensitive perylenequinone compound of Hypocrella bambusae , inhibited the proliferation of several tumor cell lines. Human cervical cancer cells, HeLa cells, were used as a model to elucidate the molecular mechanisms of HA-induced tumor cell death. The results show that HA can induce the oligonucleosomal fragmentation of DNA in HeLa cells and also can increase the expression of apoptosis inducer Bax mRNA and that it decreases the expression of apoptosis suppressor, Bcl-2 mRNA, in mitochondria. It can be concluded from the data that HA-induced apoptosis is related to the balance between Bcl-2 and Bax gene expressions.

Synthesis, Dimeric Crystal Structure, and Biological Activities of N-(4-Methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N’-(2-trifluoromethyl-phenyl)-guanidine

HE Feng-qi, WANG Bao-lei , LI Zheng-ming

2006, 22(6):  768-771.  doi:

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The title compound, N-(4-methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N’-(2-trifluoromethyl-phenyl)-guanidine, was synthesized and its structure was confirmed by using IR, MS, ¹H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has a weak herbicidal activity.

Interactions Between Surface Reactions and Gas-phase Reactions in Catalytic Combustion and Their Influence on Ignition of HCCI Engine

ZENG Wen, XIE Mao-zhao, JIA Ming

2006, 22(6):  776-782. 

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The catalytic combustion of methane in a microchannel whose surface was coated with platinum(Pt)catalyst was studied by numerical-simulation. The effects of gas-phase reactions on the whole catalytic combustion process were analyzed at a high inlet pressure. A sensitivity analysis of the detailed mechanisms of the surface reaction of methane on Pt revealed that the most sensitive reactions affecting the heterogeneous ignition are oxygen adsorption/desorption and methane adsorption, and the most sensitive reactions affecting the homogeneous ignition are OH and H₂O adsorption/desorption. The combustion process of the homogeneous charge compression ignition(HCCI) engine whose piston face was coated with Pt catalyst was simulated. The effects of catalysis and the most sensitive reactions on the ignition timing and the concentration of the main intermediate species during the HCCI engine combustion are discussed. The results show that the ignition timing of the HCCI engine can be increased by catalysis, and the most sensitive reactions affecting the ignition timing of the HCCI engine are OH and H₂O adsorption/desorption.

Apoptotic Effects of Hypocrellin A on HeLa Cells

FEI Xiao-fang , CHEN Jie , ZHENG Ke-yan , WU Wei , SUN Su-juan , WANG Li5 , MA Lan6 , LI Cong7 , TENG Li-rong

2006, 22(6):  772-775.  doi:

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Hypocrellin A(HA), a photosensitive perylenequinone compound of Hypocrella bambusae, inhibited the proliferation of several tumor cell lines. Human cervical cancer cells, HeLa cells, were used as a model to elucidate the molecular mechanisms of HA-induced tumor cell death. The results show that HA can induce the oligonucleosomal fragmentation of DNA in HeLa cells and also can increase the expression of apoptosis inducer Bax mRNA and that it decreases the expression of apoptosis suppressor, Bcl-2 mRNA, in mitochondria. It can be concluded from the data that HA-induced apoptosis is related to the balance between Bcl-2 and Bax gene expressions.

Self-assembling Process of Alkanethiol Monolayers on Gold Surface via Underpotential Deposition

HAN Dong-xue, XU Xiao-yu, HOU Peng, YANG Gui-fu, NIU Li, ZHAO Jian-wei

2006, 22(6):  783-786. 

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It was demonstrated feasible that underpotential deposition(UPD) of copper on a monolayer-modified gold substrate can be used to determine the gold electrode area. The deposition and stripping of a Cu adlayer can take place reversibly and stably at a bared or a self-assembled monolayer modified gold electrode. The growth kinetics of decanethiol/Au was also investigated via Cu UPD. The difference between the assembling kinetics determined by UPD and that by quartz crystal microbalance measurements reveals the configuration transmutation of the assembled molecules from a disordered arrangement to an ordered arrangement during the self-assembling processes.

Interactions Between Surface Reactions and Gas-phase Reactions in Catalytic Combustion and Their Influence on Ignition of HCCI Engine

ZENG Wen, XIE Mao-zhao , JIA Ming

2006, 22(6):  776-782.  doi:

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The catalytic combustion of methane in a microchannel whose surface was coated with platinum(Pt)catalyst was studied by numerical-simulation. The effects of gas-phase reactions on the whole catalytic combustion process were analyzed at a high inlet pressure. A sensitivity analysis of the detailed mechanisms of the surface reaction of methane on Pt revealed that the most sensitive reactions affecting the heterogeneous ignition are oxygen adsorption/desorption and methane adsorption, and the most sensitive reactions affecting the homogeneous ignition are OH and H₂O adsorption/desorption. The combustion process of the homogeneous charge compression ignition(HCCI) engine whose piston face was coated with Pt catalyst was simulated. The effects of catalysis and the most sensitive reactions on the ignition timing and the concentration of the main intermediate species during the HCCI engine combustion are discussed. The results show that the ignition timing of the HCCI engine can be increased by catalysis, and the most sensitive reactions affecting the ignition timing of the HCCI engine are OH and H₂O adsorption/desorption.

Effects of Sequence Distribution and Physical Aging on Physical Properties of PES/PEES Random, Block, and Alternative Copolymers

ZHOU Xiao-ming, JIANG Zhen-hua

2006, 22(6):  787-791. 

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The random, block, and alternative copolymers of poly ether sulfone(PES) and poly ether ether sulfone(PEES) were synthesized via three kinds of methods. The chemical structures of the three kinds of copolymers were characterized by ¹³C NMR. Three kinds of PES/PEES copolymers(T_g=215 ℃), which were almost identical in composition but different in sequence distribution, were used. Their physical aging process was studied by differential scanning calorimetry(DSC) at three aging temperatures ranging between T_g-15 ℃ and T_g-25 ℃. The experimental results reveal that the alternative copolymer shows a lower enthalpy relaxation time<т>and apparent activation energy when compared with the random and block copolymers. The result of the electron-microscopy investigation of the three copolymers that were treated at 200 ℃ for 96 h indicates that the molecular aggregation of the copolymers changed from a randomly coiled amorphous phase to an ordered phase, and the ordered structure of the alternative copolymer was more distinct than that of the random phase. The experimental results of this study suggest that the motion of the segments is affected by the different molecular-chain sequence distribution.

Self-assembling Process of Alkanethiol Monolayers on Gold Surface via Underpotential Deposition

HAN Dong-xue , XU Xiao-yu , HOU Peng , YANG Gui-fu , NIU Li , ZHAO Jian-wei

2006, 22(6):  783-786.  doi:

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It was demonstrated feasible that underpotential deposition(UPD) of copper on a monolayer-modified gold substrate can be used to determine the gold electrode area. The deposition and stripping of a Cu adlayer can take place reversibly and stably at a bared or a self-assembled monolayer modified gold electrode. The growth kinetics of decanethiol/Au was also investigated via Cu UPD. The difference between the assembling kinetics determined by UPD and that by quartz crystal microbalance measurements reveals the configuration transmutation of the assembled molecules from a disordered arrangement to an ordered arrangement during the self-assembling processes.

Biomimetic Preparation of Magnetite/Chitosan Nanocomposite via In Situ Composite Method——Potential Use in Magnetic Tissue Repair Domain

HU Qiao-ling, WU Jia, CHEN Fu-ping, SHEN Jia-cong

2006, 22(6):  792-796. 

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This study focused on the preparation of magnetic chitosan nanocomposite that has a potential application to bone repair and regeneration using an in situ composite method where chitosan membrane was used as the template and NaOH was used as the precipitant. X-ray diffraction analysis results show the formation of magnetite in the chitosan matrix. From the magnetic measurement, it could be concluded that the magnetic chitosan rods were superparamagnetic,and that this is the unique property of nanomagnetite. Macroscopical layer structure of the magnetic chitosan rods was observed from the photographs after mechanical test, and the microlayer structure of the rods was observed from the images of scanning electron microscopy. The mechanism for preparing the rods was discussed in detail. Transmission electron microscope was used to investigate the magnetite particles in the chitosan matrix and from the images it was concluded that the magnetite particles dispersed well in chitosan matrix with particle size of about 10 nm. The mechanical properties of the magnetic chitosan rods were measured and the blending strength was found to be 98.8 MPa. The mechanical properties did not decline when compared with those of the pure chitosan materials.

Effects of Sequence Distribution and Physical Aging on Physical Properties of PES/PEES Random, Block, and Alternative Copolymers


ZHOU Xiao-ming , JIANG Zhen-hua

2006, 22(6):  787-791.  doi:

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The random, block, and alternative copolymers of poly ether sulfone(PES) and poly ether ether sulfone(PEES) were synthesized via three kinds of methods. The chemical structures of the three kinds of copolymers were characterized by ¹³C NMR. Three kinds of PES/PEES copolymers(T_g=215 ℃), which were almost identical in composition but different in sequence distribution, were used. Their physical aging process was studied by differential scanning calorimetry(DSC) at three aging temperatures ranging between T_g=-15 ℃ and T_g=-25 ℃. The experimental results reveal that the alternative copolymer shows a lower enthalpy relaxation time〈τ〉and apparent activation energy when compared with the random and block copolymers. The result of the electron-microscopy investigation of the three copolymers that were treated at 200 ℃ for 96 h indicates that the molecular aggregation of the copolymers changed from a randomly coiled amorphous phase to an ordered phase, and the ordered structure of the alternative copolymer was more distinct than that of the random phase. The experimental results of this study suggest that the motion of the segments is affected by the different molecular-chain sequence distribution.

Synthesis and Characterization of Polystyrene/Nanosilica Organic-Inorganic Hybrid

YUAN Wang-zhang, PENG Mao, YU Qiu-ming, TANG BEN-zhong, ZHENG Qiang

2006, 22(6):  797-802. 

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A polystyrene(PS)/nanosilica organic-inorganic hybrid material was prepared from styrene monomer and commercial aqueous silica sol containing large amounts of Si-OH by means of emulsion polymerization. The nanosilica sol was modified by the addition of the reactive coupling agent methacryloxy propyltrimethoxysilane(MPS), and the resulting latex particles were protected by surfactants such as sodium dodecyl sulphonate(SDS), hydroxypropyl methyl cellulose(HMPC), and poly(vinylpyrrolidone)(PVP). The effects of the type of surfactant, the amount of surfactant, and the coupling agent on the shape and stability of the resulting latex particles were investigated. The TEM observation indicates that among SDS, HMPC, and PVP, SDS is the best surfactant. When the content of SDS is 0.5% and the amount of MPS is 7% in the system, the latex with obvious core-shell structure could be obtained. The average diameters of the monodispersed particles range from 182 to278 nm, and the average number of silica beads for each composite are 1325 and 4409, respectively. The FTIR analysis shows that PS was chemically linked to silica through MPS. The thermal gravimetric analysis shows that when there is a higher silica content, the hybrid composites have a better heat resistance.

Biomimetic Preparation of Magnetite/Chitosan Nanocomposite via In Situ Composite Method——Potential Use in Magnetic Tissue Repair Domain

HU Qiao-ling, WU Jia, CHEN Fu-ping , SHEN Jia-cong

2006, 22(6):  792-796.  doi:

Abstract ( )  

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This study focused on the preparation of magnetic chitosan nanocomposite that has a potential application to bone repair and regeneration using an in situ composite method where chitosan membrane was used as the template and NaOH was used as the precipitant. X-ray diffraction analysis results show the formation of magnetite in the chitosan matrix. From the magnetic measurement, it could be concluded that the magnetic chitosan rods were superparamagnetic，and that this is the unique property of nanomagnetite. Macroscopical layer structure of the magnetic chitosan rods was observed from the photographs after mechanical test, and the microlayer structure of the rods was observed from the images of scanning electron microscopy. The mechanism for preparing the rods was discussed in detail. Transmission electron microscope was used to investigate the magnetite particles in the chitosan matrix and from the images it was concluded that the magnetite particles dispersed well in chitosan matrix with particle size of about 10 nm. The mechanical properties of the magnetic chitosan rods were measured and the blending strength was found to be 98.8 MPa. The mechanical properties did not decline when compared with those of the pure chitosan materials.

Molecular Recognition Based on Hydrogen-bonding in the Coliposomes of Phosphatidylcholine and Amphiphiles Using Nucleobases

SONG Li-ming, ZHU Tao, WANG Qiu-sheng, ZHANG Xiao, LI Guo-wen

2006, 22(6):  803-807. 

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A functional amphiphile, N⁶-myristoyl-9-[8-(1-trimethylamino)octyl] adenine bromide(MTOAB), was used to form coliposomes of phosphatidylcholine(PC), PC/thymine, and PC/TOTB using sonication . The morphologies of the coliposomes were characterized using TEM(transmission electron microscopy). The UV-Vis spectroscopic beha-vior of PC/MTOAB/thymine(molar ratio=5:1:1) and PC/MTOAB/TOTB(molar ratio=5:1:1) of coliposomal solutions showed that as a result of base pairing, absorption intensity showed a decrease at263 nm with increase of time. The decrease of absorption intensity is ascribed to the hypochromic effect, which is because of the formation of hydrogen bonds between adenine and thymine in the coliposomes. The same effect was also observed for the mixture of aqueous PC/MTOAB liposomes and PC/TOTB liposomes after fusion, whereas the nocomplementary coliposomes formed from PC/MTOAB and PC/TOTB did not show these spectroscopic changes. The molecular recognition through hydrogen interactions between adenine and thymine is very slow because of the possible occurrence of molecular lateral diffusion and exchange of amphiphile before recognition progresses in coliposomes. These results provide useful information for the design of supramolecular devices such as vesicles and liposomes,which can be used to mimic primitive recognition processes observed in biological systems.

Synthesis and Characterization of Polystyrene/Nanosilica Organic-Inorganic Hybrid

YUAN Wang-zhang , PENG Mao , YU Qiu-ming , TANG BEN-zhong, , ZHENG Qiang

2006, 22(6):  797-802.  doi:

Abstract ( )  

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A polystyrene(PS)/nanosilica organic-inorganic hybrid material was prepared from styrene monomer and commercial aqueous silica sol containing large amounts of Si—OH by means of emulsion polymerization. The nanosilica sol was modified by the addition of the reactive coupling agent methacryloxy propyltrimethoxysilane(MPS), and the resulting latex particles were protected by surfactants such as sodium dodecyl sulphonate(SDS), hydroxypropyl methyl cellulose(HMPC), and poly(vinylpyrrolidone)(PVP). The effects of the type of surfactant, the amount of surfactant, and the coupling agent on the shape and stability of the resulting latex particles were investigated. The TEM observation indicates that among SDS, HMPC, and PVP, SDS is the best surfactant. When the content of SDS is 0.5% and the amount of MPS is 7% in the system, the latex with obvious core-shell structure could be obtained. The average diameters of the monodispersed particles range from 182 to 278 nm, and the average number of silica beads for each composite are 1325 and 4409, respectively. The FTIR analysis shows that PS was chemically linked to silica through MPS. The thermal gravimetric analysis shows that when there is a higher silica content, the hybrid composites have a better heat resistance.

Research Notes

Calix[4]arene Polyaza Derivatives: Novel Effective Neutral Receptors for Cations and (a)-Amino Acids

YANG Fa-fu, JI Yan-qing, GUO Hong-yu, LIN Jian-rong, PENG Qi

2006, 22(6):  808-810. 

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Articles

Molecular Recognition Based on Hydrogen-bonding in the Coliposomes of Phosphatidylcholine and Amphiphiles Using Nucleobases

SONG Li-ming, ZHU Tao, WANG Qiu-sheng, ZHANG Xiao , LI Guo-wen

2006, 22(6):  803-807.  doi:

Abstract ( )  

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A functional amphiphile, N⁶-myristoyl-9-[8-(1-trimethylamino)octyl] adenine bromide(MTOAB), was used to form coliposomes of phosphatidylcholine(PC), PC/thymine, and PC/TOTB using sonication . The morphologies of the coliposomes were characterized using TEM(transmission electron microscopy). The UV-Vis spectroscopic behavior of PC/MTOAB/thymine(molar ratio=5:1:1) and PC/MTOAB/TOTB(molar ratio=5:1:1) of coliposomal solutions showed that as a result of base pairing, absorption intensity showed a decrease at 263 nm with increase of time. The decrease of absorption intensity is ascribed to the hypochromic effect, which is because of the formation of hydrogen bonds between adenine and thymine in the coliposomes. The same effect was also observed for the mixture of aqueous PC/MTOAB liposomes and PC/TOTB liposomes after fusion, whereas the nocomplementary coliposomes formed from PC/MTOAB and PC/TOTB did not show these spectroscopic changes. The molecular recognition through hydrogen interactions between adenine and thymine is very slow because of the possible occurrence of molecular lateral diffusion and exchange of amphiphile before recognition progresses in coliposomes. These results provide useful information for the design of supramolecular devices such as vesicles and liposomes，which can be used to mimic primitive recognition processes observed in biological systems.

Research Note

Calix[4]arene Polyaza Derivatives: Novel Effective Neutral Receptors for Cations and α-Amino Acids

YANG Fa-fu , JI Yan-qing , GUO Hong-yu , LIN Jian-rong , PENG Qi

2006, 22(6):  808-810.  doi:

Abstract ( )  

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In this article, the interesting results of these complexation experiments were reported.