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25 March 2010, Volume 26 Issue 2

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Content of Chemical Research in Chinese Universities Vol.26 No.2(2010)

2010, 26(2):  0. 

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Articles

Facile Approach to Conductive Diamond Submicro-rods Arrays and Their Field Emission Properties

ZHAO Tian-yi, LIU Hui-biao, WANG Chun-ru, LI Yu-liang, LIU Huan* and JIAN Lei

2010, 26(2):  165-169. 

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The authors presented a facile approach to prepare highly-ordered sub-micrometer scaled cylindrical  diamond arrays based on a chemical vapor deposition method, where the accurate control of the style of crystal seeds dispersion and the growth time are very crucial. The as-prepared diamond array showed good conductivity which was originated from the proper boron doping, and moreover, it exhibited good field emission property with low turn-on field and high emission current. Importantly, this approach can be easily applied to the preparation of various    micro-patterned one-dimensional diamond arrays.

Synthesis, Crystal Structure and Magnetic Behavior of a NovelCd(II) Complex with Four Nitroxide Radicals

GAO Dong-zhao*, ZHANG Guo-ying, XU Yan-yan and SUN Ya-qiu

2010, 26(2):  170-173. 

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A novel diamagnetic-metal Cd(II) complex with four nitroxide radicals [Cd(IM4Py)₄Cl₂](IM4Py= 2-(4'-pyridinyl)-4,4,5,5-tetramethylimidazoline-1-oxyl) was synthesized and characterized by elemental analyses, IR spectra, UV-Vis spectra and X-ray single crystal diffraction. The complex crystallized in triclinic space group P1 with a=0.93285(14) nm, b=1.16827(18) nm, c =1.3660(2) nm, α =112.759(2)°, β =104.524(2)°, γ =92.008(3)°, V=1.3143(3) nm³, Z=1, D_c =1.335 g/cm³, the final R₁ =0.0423 and wR₂ =0.1009. In the title complex, each Cd(II) ion adopting a distorted octahedral geometry is coordinated by two Cl^– anions and four pyridyl-N atoms from four IM4Py ligands. The magnetic measurements show the weak antiferromagnetic interactions between the nitroxide radicals.

Three-dimensional 3d-4d Heterometallic Coordination Polymer——Synthesis, Structure, Magnetic and Luminescent Properties

CHEN Rui-xin, LUO Yan-ling and WANG Ming-hui*

2010, 26(2):  174-177. 

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A new three-dimensional 3d-4d heterometallic coordination polymer, [Cd₂Mn(H₂O)₄(BTC)₂]·2H₂O(BTC=1,3,5-benzenetricarboxylate) was prepared under hydrothermal conditions and characterized by single crystal X-ray diffraction. This compound crystallized in the monoclinic space group C2/c, with cell parameters a=1.9452(4) nm, b=0.7094(2) nm, c=1.8064(4) nm, β=118.02(3)°, V=2.2004(8) nm³ and Z=4. Its structure contains trinuclear mixed metal clusters, which are further connected by BTC to form a three-dimensional framework. The compound exhibits intense photoluminescence at room temperature. Magnetic studies of the compound show a dominant antiferromagnetic exchange between the Mn(II) ions.

Synthesis of KNiF₃ with Lower Oxygen Content by Refluxing Method

SHEN Hai-yun, YANG Qiu-hua*, ZHAO Shao-jing and WANG Dan

2010, 26(2):  178-180. 

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The complex fluoride, KNiF₃, with perovskite structure was synthesized by refluxing KF and Ni(NO₃)₂·6H₂O in ethanediol. The samples were characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM), X-ray photoelectron spectroscopy(XPS), and ultraviolet-visible diffuse reflectance spectroscopy(UV-Vis DRS). The results indicate that the mean diameter of KNiF₃ particles is about 30―60 nm and the oxygen content in the samples is ≤5%. The prepared KNiF₃ shows obvious absorption peaks at 400―830 nm.

Synthesis and Structure of a Novel Chain-like Inorganic-organic Hybrid Constructed from Isopolyanion and Oxalato-bridged Dinuclear Copper Complex

LIN Hong-yan, WANG Xiu-li*, XU Lin* and LIU Guo-cheng

2010, 26(2):  181-184. 

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A novel inorganic-organic hybrid based on isopolyanion, {[Cu₂(phen)₂(μ-ox)][H₂Mo₈O₂₆]}·4EtOH·Et₂O(1)(phen=phenanthroline, ox=oxalate), was synthesized under open-air mild reaction conditions, and characterized by elemental analysis, IR, ICP, TG and single crystal X-ray diffraction analysis. The crystal structure belongs to triclinic system with space group Pī and cell parameters: a=1.1075(5) nm, b=1.1608(5) nm, c=1.3333(5) nm, α=91.683(5)°, β=113.996(5)°, γ=112.170(5)°, V=1.4159(10) nm³, M_r=2017.44, Z=1, D_c=2.366 g/cm³ and F(000)=980.0. The structure of hybrid 1 is a 1D chain constructed of alternating octamolybdate isopolyanions [β-(Mo₈O₂₆)^4–] and oxalato- bridged dinuclear copper complex cations [Cu₂(phen)₂(μ-ox)]²⁺. Ultimately, a 3D supramolecular network was formed by hydrogen bond interactions among the adjacent chains. The result shows that hybrid 1 is the first example of inorganic-organic hybrid constructed from isopolyanion and oxalato-bridged dinuclear copper complex fragment (CCDC No. 665101).

Synthesis and Characterization of Cubic Zinc Titanate Doped with Lithium

YU Ran-bo, ZHENG Ming-zhen, CHEN Jun, DENG Jin-xia, LIU Gui-rong, ...

2010, 26(2):  185-188. 

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Cubic (Zn,Li)TiO₃ powders were synthesized through a modified sol-gel route including the Pechini process via a three-step heat treatment. The as-synthesized (Zn,Li)TiO₃ could be stable up to 1000 °C. The dielectric constant and dielectric loss tangent of all the synthesized (Zn,Li)TiO₃ samples at different measurement frequencies showed the similar tendency. At the same frequency, the dielectric constant and the dielectric loss tangent of (Zn,Li)TiO₃ samples decreased and increased, respectively, with the lithium doping content increase. The as-prepared (Zn,Li)TiO₃ showed improved microwave dielectric properties, and its maximum value of quality factor could reach 34000 GHz.

Determination of Protein via Resonance Light Scattering Technique with (NH₄)₂SO₄

WU Li-hang, MU Dan, LIANG Fang-hui, TIAN Yuan, ZHANG Han-qi, YU Ai-min, ...

2010, 26(2):  189-193. 

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Be able to form large particles with protein via electrostatic force to enhance the intensity of resonance light scattering(RLS), (NH₄)₂SO₄ was used as a RLS probe to determine bovine serum albumin(BSA), human serum albumin(HSA) and ovum albumin(OVA). The experimental conditions were investigated, including the acidity and saturation degree of (NH₄)₂SO₄. Under the optimum conditions, the enhanced RLS intensity is proportional to the concentration of BSA, HSA and OVA in the ranges of 5×10^–8―1×10^–6, 2.5×10^–8―8×10^–7 and 5×10^–8―1.5×10^–6 mol/L, respectively. The detection limits for BSA, HAS and OVA are 6.6×10^–9, 3.8×10^–9 and 7.4×10^–9 mol/L, respectively. The effects of foreign substances were also examined. The practical and synthetic samples were analyzed with satisfactory results.

Gold Nanoparticle-based Colorimetric Assay for Determination ofLead(II) in Aqueous Media

LI Xiao-kun and WANG Zhen-xin*

2010, 26(2):  194-197. 

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The authors presented a simple colorimetric assay for the detection of toxic heavy metal lead(II) ion(Pb²⁺). Pentapeptide, cysteine-alanine-leacine-asparagine-asparagine(CALNN), functionalized gold nanoparticles(GNPs) were aggregated in the presence of the divalent metal ion in solution by an ion-templated chelation process, which caused an easily measurable change in the absorption spectrum of the particles. Typically, mono-dispersing GNPs exhibit an absorption band at 522 nm, corresponding to a red color solution, while aggregated GNPs have it at longer wavelengths, corresponding to a purple or blue color solution. The chelation/aggregation process is reversible via the addition of a strong metal ion chelator such as EDTA. Highly selective and sensitive detection of Pb²⁺ in aqueous solution is thus provided. A detection limit of 0.1 μmol/L of Pb²⁺ was demonstrated.

Pyrolysis-GC/MS of Menthyl Esters of N-Benzoxycarbonyl Amino Acid

MAO Mao, GU Cheng-zhi, YIN Hao, SONG Qin-hua and LI Qian-rong*

2010, 26(2):  198-203. 

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With the aid of a Pyrolysis-GC/TOF MS technique, the pyrolysis behaviour of two menthyl esters of N-benzoxycarbonyl amino acid was investigated. A clear pattern emerges involving the cleavage of the bond linking the menthyl ring to the carboxy group, followed by further degradation of the fragments. The major pyroproducts were p-menth-1-ene pyrolysed at a higher temperature or p-menth-2-ene pyrolysed at a lower temperature, and various derivatives of cyclohexene pyrolyzed from the menthyl ring. In addition, some of the products were also iden- tified as derivatives of benzene from the pyrolysis of benzyloxyl moiety.

Effects of Nitrobenzene on Liver Antioxidant Defense System of Carassius auratus

SHAO Peng, YUAN Xing*, LIU Rui* and CAO Jian-ping

2010, 26(2):  204-209. 

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With superoxidedismutase(SOD), catalase(CAT), glutathione S-transferase(GST) and malondialdehyde (MDA) as characteristic indexes, the effects of nitrobenzene(NB) on the liver antioxidant defense system of Carassius auratus were studied under the indoors stimulant conditions, and the toxic mechanisms were discussed. The exposure concentrations of NB were 0.5, 1.0, 5.0 and 10.0 mg/L, and the exposure time was 5, 10 and 15 days, respectively. The results show that the stress responses of four antioxidant indexes in the fish liver to nitrobenzene were different. The SOD activity was firstly inhibited and then induced. The CAT and GST activities were mainly induced. The MDA content in the high concentration group showed a significant time-effect relationship. In addition, the changes of CAT and SOD activities were not synchronous, and GST played an important part in the detoxification process of nitrobenzene.

Formation of Struvite Crystals in a Simulated Food Waste Aerobic Composting Process

DU Xian-yuan, LIU Jian-lin, HUANG Guo-he and LI Yu*

2010, 26(2):  210-216. 

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Bench-scale treatments with three mixtures of Mg and P salts, including K₃PO₄+MgSO₄, K₂HPO₄+MgSO₄, and KH₂PO₄+MgSO₄ as additives in a simulated food waste aerobic composting process, were conducted to test   the magnesium ammonium phosphate(MAP) formation, and the compost products were analyzed by X-ray diffraction(XRD), Scanning electron microscopy(SEM), and Energy dispersive X-ray spectroscopy(EDS) analyses. The comparison results between XRD, SEM, and EDS analyses of MAPs in the dried compost and synthesized MAPs confirm the formation of MAP crystals in the simulated food waste aerobic composting process. The analysis of the compost also indicates that the addition of all the three mixtures of Mg and P salts in the aerobic composting process can increase nitrogen conservation and decrease nitrogen loss because of the formation of MAPs. The mechanism of MAP formation was verified as the reaction of ammonium(NH₄⁺) with magnesium(Mg²⁺) and phosphate[H_nPO₄^(3–n)–, n=0, 1, and 2).

Remarkably Decreased CD11b Positive Splenocytes in Aquaporin 3-Null Mice

ZHU Na, QIAO Ying, ZHANG Di, WANG Wen-juan, LIU Jia, LIU Tian-zhou, ...

2010, 26(2):  217-220. 

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Aquaporins(AQPs) are molecular water channels that play important physiological roles in fluid transporting organs. The expression and function of AQPs in the immune system are largely unknown. CD11(a―d)/CD18 integrins are adhesion molecules expressed on leukocytes, which play a critical role in leukocyte adhesion, migration and host defense. In the present study, we discovered the expression of aquaporin-3(AQP3) on spleen CD11b positive cells, and the content of CD11b positive splenocytes in aquaporin 3-null mice is significantly decreased. Further analysis suggested remarkably decreased monocyte/macrophage subpopulation and significantly decreased granulocyte subpopulation. It is the first report suggesting an important role of AQP in the development and maturation of immunocytes.

Expression and Activities Experiment of DNA Transduction Motif Based on GAL4 in Pichia Pastoris

XU Xiao-hong, CHI Bao-rong*, LI Xiao, YANG En-cheng, GAO Peng, LIU Yan, ...

2010, 26(2):  221-224. 

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The genes encoding DNA-binding domain(BD) designed based on the yeast transcriptional activator GAL4 and protein transduction domain of HIV-1 Tat protein were fused via soft linker peptide sequence, and cloned into yeast expression vector pPIC9k. The resulted plasmid pTG was linearized and transfected into Pichia pastoris strains GS115 by electroporation. High copies of transformants were obtained with Mut^s and HIS⁺ phenotype identification, PCR amplification and screening of G418. After flask culture and expression induced by methanol, the target protein named TG was well expressed and analyzed by SDS-PAGE and Western blot. Under optimized conditions, the yield of soluble recombinant protein was approximately 39.7 mg/L. DNA binding activity and cell transduction  property of TG were analyzed by gel electrophoresis and fluorescent microscopy. The results show that the recombinant protein could bind strongly to the plasmid containing upstream activating sequence(UAS). The cell experiments revealed that TG could deliver the binding plasmid into HEK-293 cells effectively. In summary, the work presented here suggests that TG is specific toward UAS containing plasmid and has the potential for use as nonviral DNA delivery agent.

Synthesis and HIV-1 Integrase Inhibitory Activity of Furanone Derivatives

YU Sheng-hui, ZHAO Si-tai, LIU Chuan, ZHONG Yuan and ZHAO Gui-sen*

2010, 26(2):  225-229. 

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Twenty novel furanone derivatives, based on the structure of raltegravir which was the first HIV-1 integrase(IN) inhibitor approved by the United States Food and Drug Administration(US FDA), were designed, synthesized and characterized by ¹H NMR, IR and MS. The biological activities of these compounds against HIV-1 IN in vitro were evaluated. The assay results indicate that the replacement of pyrimidinone with furanone decreased the inhibitory activity of the compounds to HIV-1 IN. Compounds 3i, 3j and 3t show moderate inhibitory activity against HIV-1 IN and selectively inhibit the strand transfer reaction.

Total Fractionation and Analysis of Polysaccharides from Leaves of Panax ginseng C. A. Meyer

NI Xiu-zhen, WANG Bing-qing, ZHI Yuan, WEI Ning-ning, ZHANG Xu, LI Shan-shan,...

2010, 26(2):  230-234. 

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The water-soluble polysaccharides isolated from the leaves of Panax ginseng C. A. Meyer were totally fractionated into one neutral fraction(GLPN-1), six acidic fractions(GLPN-2, GLPA-1a, GLPA-1b, GLPA-1c, GLPA-2 and GLPA-3) by a combination of ethanol precipitation, ion-exchange and gel permeation chromatography. All the fractions were analyzed by determining monosaccharide composition, molecular weight distribution. The results show that GLPN-1 was mainly composed of Gal(38.1%) and Ara(33.6%) and presumed to be an arabinogalactan. GLPA-1a, GLPA-1b and GLPA-2 mainly contained Gal, Ara, Rha and GalA. The amount of Gal and Ara acounted for over 50% of total sugar and the amount of Rha was more than 10%. The molar ratios of Rha/GalA in GLPA-1a, GLPA-1b and GLPA-2 were 1:1, 1:2 and 1:2.7, respectively, indicating that they belong to type-I rhamnogalacturonan (RG-I)-rich pectin. GLPA-1c was mainly composed of GalA(78%), belonging to homogalacturonan(HG)-rich pectin. GLPA-3 might be a glycoprotein.

Expression and Characterization of a Recombinant Truncated Capsid Protein of Hepatitis E Virus in Pichia pastoris

YANG En-cheng, CHI Bao-rong*, LI Xiao, LIU Yan, GAO Peng, JIA Peng

2010, 26(2):  235-239. 

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Hepatitis E is an enterically transmitted viral disease caused by infection with hepatitis E virus(HEV). HEV is a nonenveloped virus that has been classified in the family of Caliciviridae. The virus appears to be a polyadenylated, positive-stranded RNA virus with three major open reading frames(ORFs). The capsid protein of HEV is encoded by the open reading frame 2(ORF2). We attempted to produce a truncated capsid protein, designed p293, in Pichia pastoris. The p293 gene encoding amino acids(aa) 382-674 of HEV ORF2 was designed based on the full length of HEV ORF2, cloned into the yeast vector pPIC9K, and expressed in P. pastoris strain GS115. SDS-PAGE and Western blotting demonstrated that the recombinant protein p293 could well be expressed in P. pastoris. Under optimized conditions (culture medium pH, 6.0―6.5; methanol concentration added daily, 3.0%; inoculum density, OD₆₀₀=60; induction time point, 72―96 h), the yield of soluble p293 was approximately 80 mg/L. We also observed p293 secretory expressed in P. pastoris to be 30 nm viral like particles by using electron microscopy. These results show that the p293 may has utility in the analysis of cell specific factors in the protein processing and assembly of HEV, and serve as a useful antigen for both diagnostic and vaccine purposes.

Expression and Characterization of an Active Chimeric Protein of Human Extracellular Superoxide Dismutase and hCuZnSOD in Pichia pastoris

QU He-zhi, DU Shan-shan, YANG Shuo, HUANG Lu, ZHANG Lei, XIAO Song, ...

2010, 26(2):  240-244. 

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Mammalian cells express two isoforms of Cu- and Zn-containing superoxide dismutases(SODs), CuZnSOD and extracellular SOD(EC-SOD), involved in the defense system against reactive oxygen species(ROS). The two SODs have structurally homologous centre domain with distinct N- and C-terminuses, resulting in the different characteristics of the structure and function of the two molecules. We generated a hybrid SOD molecule(namely hySOD) via replacing the N- and C-terminuses of hCuZnSOD with the counterparts of hEC-SOD. The hySOD was expressed in host Pichia pastoris and the purified protein was a dimer with a molecular weight of about 34000. A series of activity analyses indicates that the hySOD is similar to hEC-SOD in heat-stability, and has the activity of protec- ting the host cell against heat shock and oxidative stress. Our results show evidence for the study on the compound activity of multiple SOD molecules, and may be important for understanding the relationship between structure and function of hEC-SOD and hCuZnSOD.

Facile Synthesis of 5-Hydroxy-2-(2-phenylethyl)chromone

ZHANG Lan-ping and WANG Ya-lou*

2010, 26(2):  245-248. 

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5-Hydroxy-2-(2-phenylethyl)chromone(1) was synthesized from 2,6-dihydroxyacetophenone(7) obtained via four-steps resorcinol-reacting with phenylpropionic acid, the procedures involved are Baker-Venkataraman rearrangement and cyclization which are easy to conduct, the overall yield is 32%.

Highly Sensitive Acidic pH Fluorescent Probe Based on A Boradiaza-indacene Derivative

LIU Yang, LIU Shan-lin and WANG Yan-guang*

2010, 26(2):  249-251. 

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A pH-sensor with a pK_a value of 5.05 based on 4,4-difluoro-4-bora-3a,4a-diaza-s-indacene(BODIPY) dye was synthesized and demonstrated to be highly sensitive within a pH range of 4.0―6.0 and was highly photostable, which makes it a potential pH fluorescent probe. The new pH-sensor will find its application in studying acidic organelles in living cells.

Proteomics Approach to Investigate Impact of aFGF Antagonist on Signal Transduction Pathway

FU Yu-qin, LI Min, WANG Xu, ZHOU Guo-qiang, ZHOU Hui and CUI Yin-qiu*

2010, 26(2):  252-255. 

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Fibroblast growth factor(FGF) signal transduction pathway is correlated with many diseases, such as cancer, skeletal dysplasias, olfactory syndromes and so on. P(VYMSPF), a small peptide, is an antagonist of aFGF. In order to investigate the impact of the peptide P on aFGF signal transduction pathway, the proteomes of NIH3T3 cell stimulated under different conditions(aFGF+heparin sodium and aFGF+heparin sodium+P) were extracted and analyzed by 2DE, five differentially expressed protein spots were selected and identified via ESI-MS/MS. The result indicates that the peptide P has a great influence on the function of aFGF such as metabolism, protein translation and cytoskeleton formation; the target signal pathway of the peptide P may be MAPK pathway and the peptide P might also affect the PLCγ pathway. The article provides a new insight into the peptide P as a potential anticancer drug.

Design, Synthesis and Molecular Docking of a Novel Small-molecule Inhibitor of Caspase-3

ZHANG Jin-liang, GUO Yang-hong, GAO Chao-hui, WANG En-si, REN Zhong-yuan, ...

2010, 26(2):  256-258. 

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4,5-Dihydro-3-methylbenzo[1,2-b]furan-4,5-dione(4) was identified as a novel and potent inhibitor of caspase-3 through structural modification of an existing drug, sodium tanshinone IIA sulfonate(STS). Compound 4 showed high potency against caspase-3 in vitro(IC₅₀=0.13 μmol/L). Molecular docking study further provided an insight into the interaction of compound 4 with activated caspase-3. Hence, this small-molecule caspase-3 inhibitor could be a promising therapeutic candidate against diseases caused by abnormally up-regulated apoptosis.

Improved Allele-specific Polymerase Chain Reaction for Single Nucleotide Polymorphism Genotyping

WU Mei, DU Zhen-wu, LIU Jia-nan, SONG Yang, WANG Ya-li and ZHANG Gui-zhen*

2010, 26(2):  259-262. 

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An improved allele-specific PCR(AS-PCR) approach was applied to investigating –55C/T polymorphism in promoter region of the uncoupling protein 3(UCP3)gene. AS-PCR is a competitive PCR method which is based on positioning the 3′ base of a PCR primer to match one single nucleotide polymorphism(SNP) allele and accurately extend only the correctly matched primer. But it is limited in use because of its poor specificity. In this study, we improved the specificity of AS-PCR by introducing additional mismatch at the penultimate base of 3′ end of AS-PCR primer in combination with decreasing the level of dNTP in the reaction mixture. Sensitivity, specificity and reliabi- lity of this method were assessed for both simple plasmid model and complex human genomic SNP targets. The –55C/T(rs1800849) polymorphism of the UCP3 gene was analyzed via this AS-PCR and restriction fragment length polymorphism(RFLP), the latter was used as a gold standard. The results suggest that the increase in AS-PCR discrimination with this method should facilitate the use of this simple, rapid, and inexpensive technique for SNP genotyping application.

Poly(ethylene glycol)-supported Piperazine——Synthesis and Application in Knoevenagel Condensation

WANG Cui-e, JIN Jie, ZHANG Min, YU Shu-yan, SHANG Yong-jia* and HU Jin-song

2010, 26(2):  263-267. 

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A soluble, poly(ethylene glycol)-supported piperazine catalyst was prepared. This soluble catalyst efficiently catalyzes the Knoevenagel condensation of various aromatic aldehydes with diethyl malonate or ethyl acetoacetate in a homogeneous phase to afford the desired alkenes in good purity and yield with a facile work-up process. It was found that the polymer reagent could be repeatedly used at least four times without the too much loss of activity. The catalyst has shown a good activity, stability, and recycling capability.

Synthesis and Anti-inflammatory Activity of a Novel Series of 9,10-Dihydro-4H,8H-chromeno[8,7-e][1,3]oxazin-4-one Derivatives

LIU Xiao-ping, WANG Ying, LAN Hui-yu, SONG Ai-hua, TSIM Karl Wah-keung, ...

2010, 26(2):  268-271. 

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Flavonoids exhibit a wide range of biological activities including anti-inflammatory activity, while some 1,3-benzoxazine derivatives show anti-inflammatory activity. In order to explore the novel anti-inflammatory agents, based on the principles of bioisosterism and hybridization, ten novel chromeno[8,7-e][1,3]oxazin-4-ones were synthesized and characterized with IR, ¹H NMR, MS and elemental analyses. The anti-inflammatory activities of the target compounds were evaluated via the croton oil-induced ear oedema test in Swiss mice. According to screened results, some target compounds show potent anti-inflammatory activity.

Synthesis and in vitro Anti-hepatitis B Virus Activity of Some Ethyl 5-Hydroxy-4-substituted Aminomethyl-2-sulfinylmethyl-1H-indole-3-carboxylates

ZHAO Yan-fang, FENG Run-liang, LIU Ya-jing, ZHANG Yi-kun and GONG Ping*

2010, 26(2):  272-277. 

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A novel series of ethyl 5-hydroxy-4-substituted aminomethyl-2-sulfinylmethyl-1H-indole-3-carboxylates 8a―8j and 11e―11f was synthesized and evaluated in HepG2.2.15 cells for their anti-hepatitits B virus(HBV) acti- vity and cytotoxicity. Among them, six compounds showed more potent inhibitory activity than lamivudine. Compound 8e exhibited the most significant anti-HBV activity with an IC₅₀ value of 1.62 μmol/L, which was 33-times more potent than the reference drug lamivudine(IC₅₀=54.78 μmol/L).

Synthesis and Characterization of Magnetic TiO₂/SiO₂/NiFe₂O₄ Composite Photocatalysts

YUAN Jin, Lü Yong-kang, LI Yu* and LI Jun-ping

2010, 26(2):  278-282. 

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Magnetic TiO₂/SiO₂/NiFe₂O₄ composite photocatalytic particles with high crystalline TiO₂ shell were synthesized via a mild solution route. The prepared composite particles were characterized with X-ray diffraction(XRD), transmission electron microscopy(TEM), high resolution transmission electron microscopy(HRTEM), scanning electron microscopy(SEM), ultraviolet-visible(UV-Vis) spectroscopy and vibrating sample magnetometer(VSM). The results show that the obtained TiO₂/SiO₂/NiFe₂O₄ composite particles were composed of spherical nanoparticles, about 30 nm in diameter, with several NiFe₂O₄ fine particles about 20 nm in diameter as cores and silica as coatings and barrier layers between the magnetic cores and titania shells. The photocatalytic activity of the composite photocatalytic particles was also investigated for the degradation of Basic Violet 5BN(BV5) under UV irradiation. About 97% of original BV5 decomposed in 360 min in the presence of magnetic composite nanoparticles under UV light. The synthesized magnetic composite nanoparticles exhibited high photocatalytic efficiency that would find potential application to cleaning polluted water with the help of magnetic separation.

Comparative Studies on Structure and Electronic Properties Between Thermal Lithiated Li_0.5MnO₂ and LiMn₂O₄

WANG Deng-pan, CHEN Hong, DU Fei, BIE Xiao-fei, LIU Li-na, WEI Ying-jin, ...

2010, 26(2):  283-286. 

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Monoclinic Li_0.5MnO₂ was synthesized by solid state reaction and the spectral and magnetic properties were studied in comparison with those of spinel LiMn₂O₄. The XRD pattern and Raman spectrum of Li_0.5MnO₂ are different from those of LiMn₂O₄, which indicate the different long-range and short-range crystal structure. XPS result shows the binding energies of 2p_3/2 and 2p_1/2 in Li_0.5MnO₂ are located at 642.3 and 653.6 eV, respectively. Through fitting the XPS spectra, the valence state of Mn ion in Li_0.5MnO₂ coincides with that in LiMn₂O₄. The high-temperature susceptibility of Li_0.5MnO₂ can be fitted by Curie-Weiss law whose Curie and Weiss constants are 33 A·m²·K/(mol·T) and –277(6) K, respectively. Although Li_0.5MnO₂ shows spin glass ground state, the transition temperature of Li_0.5MnO₂ is about 9 K lower than that of LiMn₂O₄.

Electro-oxidation of Ascorbic Acid on PVP-stabilized Graphene Electrode

HAN Dong-fang, SHAN Chang-sheng, GUO Li-ping, NIU Li and HAN Dong-xue*

2010, 26(2):  287-290. 

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Polyvinylpyrrolidone-stabilized graphene(PVP-graphene) was synthesized and investigated as a modifier for the determination of ascorbic acid(AA). With PVP acting as stabilizer and dispersant, the resulting PVP-graphene material could disperse well into water. And the PVP-graphene modified glassy carbon electrode(PVP-graphene- GCE) showed an obvious electrocatalytical activity toward the oxidation of AA in a phosphate buffer solution(PBS, pH=7.0) with an oxidation potential of AA at 0.052 V vs. Ag|AgCl(sat. KCl). The calibration curve for AA was linear in a concentration range from 1.0×10^–5 to 5.0×10^–4 mol/L with a correlation coefficient of 0.9998. And the detection limit was found to be 1 μmol/L. During the oxidation of AA, the π-π interaction of graphene plane with conjugated hexenoic acid-lactone in AA molecules might play a key role. As a result, an obvious decrease of overpotential was achieved at such a PVP-graphene electrode through a possible adsorption/enrichment process, which will probably trigger potential applications for the electroanalysis of some aromatic and heterocyclic compounds.

Physical and Electrochemical Characterization of Hydrothermal Prepared α′-NaV₂O₅ Crystals

HU Fang, WEI Ying-jin, JIANG Tao, MING Xing, CHEN Gang and WANG Chun-zhong*

2010, 26(2):  291-293. 

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α′-NaV₂O₅ was prepared by a simple hydrothermal process. X-ray diffraction confirmed the orthorhombic structure of α′-NaV₂O₅, with preferential growth along the (001) direction. Scanning electron microscopy showed α′-NaV₂O₅ was composed of flake-shaped crystals. X-ray photoelectron spectroscopy confirmed the co-existence of V⁴⁺ and V⁵⁺ in α′-NaV₂O₅, which results in an average V^4.5+ oxidation state of α′-NaV₂O₅. The observed Raman bands are ascribed to different V―O vibrations. α′-NaV₂O₅ shows a reversible specific capacity of about 100 mA·h·g^–1 between 3.5 and 1.0 V, with a good capacity retention. The good electrochemical stability of the material is attributed to its structural stability during Li⁺ intercalation.

Fragmentation Behavior and Ionization Potentials of Aluminum Clusters Al_n(n≤40)

ZHANG Wei, LI Zhuo, ZHANG Gang and Lü Wen-cai*

2010, 26(2):  294-299. 

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Al₂－Al₄₀ clusters were studied by means of the all-electron DFT method. The properties of the aluminum clusters including binding energy, the second difference in energy, HOMO-LUMO gap, especially fragmentation energies and ionization potentials, were analyzed. The main products from the dissociations of aluminum cluster ions are shown to be Al + Al⁺_n–1 for the larger clusters, and Al⁺+Al_n–1 for the smaller ones. And, the calculated ionization potentials are consistent with the experiment data.

Non-isothermal Decomposition Mechanism and Kinetics of LiClO₄ in Nitrogen

HONG Jian-he, SONG Li, ZHOU Xin-wen, DIAKITE Kahirou and ZHANG Ke-li*

2010, 26(2):  300-303. 

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The non-isothermal decomposition kinetics of LiClO₄ in flow N₂ atmosphere was studied. TG-DTA curves show that the decomposition proceeded through two well-defined steps below 900 °C, and the mass loss was in agreement with the theoretica1 value. XRD profile demonstrates that the product of the thermal decomposition at 500 °C is LiCl. For the decomposition kinetics study, the activation energies calculated with the Friedman method were considered as the initial values for non-linear regression and were used for verifying the correctness of the fitted models. The decomposition process was fitted by a two-step consecutive reaction: extended Prout-Tompkins equation[Bna, f(α) is (1-α)_nα^α] followed by a 1th order reaction(F1). The activation energies were (215.6±0.2) and (251.6±3.6) kJ/mol, respectively. The exponentials n and α for Bna reaction were (0.25±0.05) and (0.795±0.005), respectively. The reaction types and activation energies were in agreement with those obtained from the isothermal method, but the exponentials were optimized for better fitting and prediction.

Crystal Structure and Thermodynamic Study of Ephedrine Hydrochloride C₁₀H₁₆NOCl(s)

YANG Wei-wei, DI You-ying*, LI Jing and KONG Yu-xia

2010, 26(2):  304-308. 

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The crystal structure of ephedrine hydrochloride was determined by means of X-ray crystallography. The crystal system of the compound is monoclinic, and the space group is P2₁. Unit cell parameters are a=0.7308(6) nm, b=0.6124(5) nm, and c=1.2618(11) nm; α=90°, β=102°, and γ=90°; Z=2. Low-temperature heat capacities of the title compound were measured with an improved precision automated adiabatic calorimeter over a temperature range from 77 K to 396 K. A polynomial equation of the heat capacities as a function of temperature in the temperature region was fitted by the least-squares. Based on the fitted polynomial equation, the smoothed heat capacities and thermodynamic functions of the compound relative to the standard reference temperature 298.15 K were calculated and tabulated at the intervals of 5 K.

Apparent Molar Volumes and Solvation Coefficients in Ternary-pseudo-binary Mixtures [(Styrene+Ethyl Acetate or Benzene)+(N-Methyl-2-pyrrolidone+Ethyl Acetate or Benzene)]

HOU Hai-yun*, PENG San-jun, WANG Sheng-ze and GENG Xing-peng

2010, 26(2):  309-317. 

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Over the full range of compositions, in the ternary-pseudo-binary mixtures of x[(1-y)C₆H₅CH=CH₂+yCH₃COOC₂H₅(or C₆H₆)]+(1-x)[(1-y)NMP+yCH₃COOC₂H₅(or C₆H₆)], the apparent molar volumes of each pseudo-pure component at different y values were calculated from the density data at 298.15 K and atmospheric pressure. The results show that the four parameters cubic polynomial can correlate the apparent molar volume with the molar fraction well over the full molar fraction range. The limiting partial molar volumes and the molar volumes of each pseudo-pure component were evaluated with different methods. Based on the limiting partial molar volume and molar volume at a certain y value, a new universal coefficient termed as solvation coefficient γ was defined to describe quantitatively the solvation degree of pseudo-pure solute and the interactions of solute-solvent molecules from the macroscopical thermodynamics viewpoint. The results demonstrate the solvation coefficients decrease with the amount of the third component increasing for each pseudo-pure solute, irrespective of the pseudo-pure solvent. Then the solvation degrees of each pseudo-pure component, the specific interactions between the solute molecule and the solvent one were discussed in terms of the solvation coefficient.

Preparation of Ultrafine Water-soluble Polymers Nanofiber Mats via Electrospinning

SUN Guo-en, TENG Hong, ZHANG Chun-ling, DOU Yan-li and LI Yi*

2010, 26(2):  318-322. 

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A series of water-soluble polymers such as poly(ethylene oxide)(PEO), polyacrylamide(PAM) and poly(vinyl pyrrilidone)(PVP) was successfully prepared via the electrospinning of their aqueous solutions without the use of a surfactant. The effects of solution properties on the electrospinning of PEO, PAM and PVP solutions were investigated. The viscosity of the solution, charge density carried by the jet, and the surface tension of the solution are the key factors that influence the morphology and diameter size of the fibers. The viscosity of the solution was  measured on a modular compact rheometer. The morphology and the diameter size distribution of the fibers were  observed under an environmental scanning electron microscope(ESEM). The results show that the diameters of the nanofibers electrospun from the solutions of these water soluble polymers were uniform and less than 300 nm.

Affinity Adsorption of Bilirubin on Cibacron Blue F3GA-modified Microporous Polytetrafluoroethylene Capillary

JIN Gu* and YAO Jian-xia

2010, 26(2):  323-330. 

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Bilirubin removal from human plasma was obtained via an affinity microporous polytetrafluoroethylene(MPTFE) capillary. The new adsorbent comprised grafted glycidyl methacrylate(GMA) via radiation-induced polymerization as hydrophilic coating and reactive sites; ethylenediamine(EDA) as a spacer arm; Cibacron Blue F3GA(CB F3GA) as an affinity ligand; MPTFE capillary as the supporting matrix. The average density of CB F3GA attachment to MPTFE capillaries was found to be 136.5 μmol/g. The capacity of bilirubin adsorbed on affinity MPTFE capillaries is 76.1 mg bilirubin/g polymer(at 25 °C). This new adsorbent has advantages over both membrane and traditional micro-column, and this system is stable and easy to operate. The results of blood tests suggest the CB F3GA affinity capillary has good blood compatibility.

Research Note

4-Amino-1,2,4-triazole Resin-supported Palladium Complex as Phosphine-free Catalyst for Suzuki Reaction in Aqueous Phase

WU Xiang-mei*, WANG Yan and GUO Sheng-rong

2010, 26(2):  331-334. 

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A palladium catalyst immobilized on 4-amino-1,2,4-triazole resin was readily prepared and effectively catalyzed the Suzuki reaction of aryl or heteroaryl halides and phenylboronic acid with low palladium amount under aqueous conditions in the absence of phosphine ligand. This catalyst showed reusability in the Suzuki reaction of aryl iodide at least three times.