2004 Volume 15 Issue 11

Synthesis of 5,10,15,20-Tetra(N-methyl-6-quinolyl)-21,23-dithiaporphyrin Chloride as Cationic Core-modified Porphyrin
Tao , Laurence H. HURLEY
2004, 15(11): 1261-1264
[Abstract](160) [FullText HTML] [PDF 1708KB](1)
First cationic 6-quinolyl substituted dithiaporphyrin was synthesized using Skraup quinoline methodology from thiaporphyrin bearing 4-acetamidophenyl prepared by condensation reaction of aromatic aldehyde with pyrrole.
Solvent-free Mechanochemical and Liquid-phase Reaction of [60]Fullerene with Ethyl 2-Diazopropionate
Yu Jin LI , Ru Fang PENG , You Cheng LIU , Guan Wu WANG
2004, 15(11): 1265-1268
[Abstract](172) [FullText HTML] [PDF 1727KB](0)
The solvent-free mechanochemical reaction and the liquid-phase reaction of C60 with ethyl 2-diazopropionate prepared in situ or preformed from alanine ethyl ester hydrochloride and sodium nitrite have been investigated. Methanofullerene 1 and fulleroids 2 and 3 from these reactions were obtained, meanwhile the pyrazoline intermediate was not observed. Fulleroids 2 and 3 can be converted to methanofullerene 1 in refluxing toluene.
Facile Synthesis of Ureas in Ionic Liquid
Wei Xing QIAN , Feng Yang JU , Yong Min ZHANG , Wei Liang BAO
2004, 15(11): 1269-1272
[Abstract](157) [FullText HTML] [PDF 1433KB](0)
The reaction of isocyanates with aliphatic and aromatic amines in the 1-n-butyl-3- methylimidazolium tetrafluoroborate (bmimBF4) ionic liquid in good to excellent yields is described. Due to its insolubility, the desired urea solids could be recovered by simple filtration from the ionic liquid after reaction.
A Novel Synthesis of (-)-10-epi-α-Cyperone
Li Jing FANG , Jin Chun CHEN , Guo Jun ZHENG , Yu Kun GUAN , Yu Lin LI
2004, 15(11): 1273-1275
[Abstract](155) [FullText HTML] [PDF 980KB](1)
An alternative route for the synthesis of (-)-10-epi-α-cyperone 1 starting from (+)- dihydrocarvone 2 is described by using an asymmetric Michael addition as a key step. The route features more efficiently and can be performed in large scale.
Synthesis and Crystal Structure of 2-Amino-1, 1-diferrocenylethanol
Hai Ying ZHAO , Zhan Xi BIAN , Bao Guo LI
2004, 15(11): 1276-1278
[Abstract](742) [FullText HTML] [PDF 1042KB](0)
2-Amino-1,1-diferrocenylethanol 2 was prepared by reduction of trimethylsilyl cyanohydrin ether of diferrocenyl ketone. The crystal structure of 2 was further defined by X-ray diffraction.
Regioselective Synthesis of Multi-substituted Phenylselenomethyl Isoxazolines
Wei Ming XU , Lu Ling WU , Xian HUANG
2004, 15(11): 1279-1280
[Abstract](166) [FullText HTML] [PDF 566KB](0)
A mild, regioselective 1, 3-dipolar cycloaddition protocol for the preparation of phenylselenomethyl isoxazolines through substituted allyl phenyl selenides and nitrile oxides was reported.
Synthesis of Arylsubstituted Imidazolin-2-one Analogues
Yun Feng CHENG , Yong Zhou HU
2004, 15(11): 1281-1284
[Abstract](164) [FullText HTML] [PDF 1159KB](2)
Herein we reported a one-pot synthesis of arylsubstituted imidazolin-2-ones by the cyclization of α-aminoacetophenone hydrochloride analogues 2 with arylisocyanates 3. Compared with other known synthetic route, this method resulted in higher yield.
Design and Synthesis of Novel Molecular Tweezers Derived from Chenodeoxycholic Acid
Zhi Gang ZHAO , Qi Ming MU , Shu Hua CHEN
2004, 15(11): 1285-1288
[Abstract](164) [FullText HTML] [PDF 1629KB](0)
A novel type of chiral molecular tweezers has been designed and synthesized by using chenodeoxy cholic acid as spacer and the aromatic compounds as arm. Their structures were characterized by 1HNMR, IR, MS spectra and elemental analysis. These chiral molecular tweezers showed good enantioselectivity for D-amino acid methyl esters.
Intermolecular Phosphoryl Transfer Between Serine and Histidine Residues
Yu Qian SU , Ming Yu NIU , Shu Xia CAO , Jian Chen ZHANG , Yu Fen ZHAO
2004, 15(11): 1289-1291
[Abstract](157) [FullText HTML] [PDF 885KB](0)
A novel intermolecular phosphoryl transfer from O-trimethylsilyl-N-(O, O-diisopropyl) phosphoryl serine trimethylsilyl ester to N, N'-bis(trimethylsilyl) histidine trimethylsilyl ester was studied through electrospray ionization mass spectrometry (ESI-MS). It was proposed that the transfer reaction went through penta-coordinated phosphorus intermediate.
The Synthesis of Bis(carboxyalkylmethyl) Diselenides by Selenium Transfer Reaction of Aryl Selenoamides
Hua Rong ZHAO , Xiao Feng LI , Xin Jian ZHAO , Yang Ping NIU
2004, 15(11): 1292-1294
[Abstract](161) [FullText HTML] [PDF 953KB](1)
Aryl selenoamides react smoothly with α-haloacetic acid in various alcohol to give corresponding bis(carboxyalkylmethyl) diselenides in good yields.
Nickel Chloride Promoted Glaser Coupling Reaction in Hot Water
Pin Hua LI , Lei WANG , Min WANG , Jin Can YAN
2004, 15(11): 1295-1298
[Abstract](171) [FullText HTML] [PDF 1380KB](1)
A Glaser coupling reaction of terminal alkynes in the presence of nickel chloride without any organics and bases in hot water has been developed, which produces the corresponding homo-coupling products in good yields.
Effect of Catalase on Biocatalytic Synthesis of Pyruvate by Enzymes from Pseudomonas sp.
Jing Song GU , Yuan Xiu WANG , Qiang JIAO
2004, 15(11): 1299-1302
[Abstract](165) [FullText HTML] [PDF 1233KB](0)
Pyruvate was produced from DL-lactate by a kind of green-chemical biocatalyst-cell-free extract from bacterial strain Pseudomonas sp. SM-6. Catalase in cell-free extract, which could stabilize the pyruvate formed by lactate oxidase, played an important role in pyruvate preparation. The effect of catalase in conversion process was evaluated.
A New Triterpenoid from Doellingeria scaber
Su Ping BAI , Li DONG , Zhi An HE , Li YANG
2004, 15(11): 1303-1305
[Abstract](168) [FullText HTML] [PDF 1069KB](0)
A new oleanane-type triterpene was isolated from the roots of Doellingeria scaber. Its structure was identified as 3-oxo-16α-hydroxy-olean-12-en-28-oic acid based on 1D and 2D NMR spectroscopy and X-ray analysis.
Two New Diarylheptanoids from the Rhizomes of Zingiber officinale
Jian Ping MA , Xiao Ling JIN , Li YANG , Zhong Li LIU
2004, 15(11): 1306-1308
[Abstract](166) [FullText HTML] [PDF 1113KB](0)
Two new diaryheptanoids, (5S)-5-acetoxy-1,7-bis(4-hydroxy-3-methoxyphenyl)-3- heptanone (1) and (3S,5S)-3,5-diacetoxy-1,7-bis(4-hydroxy-3-methoxyphenyl)heptane (2) were isolated from the rhizomes of Zingiber officinale. Their structures were elucidated by spectral methods.
A New Sesquiterpene Lactone from Scorzonera austriaca
Juan LI , Quan Xiang WU , Yan Ping SHI , Ying ZHU
2004, 15(11): 1309-1310
[Abstract](168) [FullText HTML] [PDF 657KB](2)
A new guaianolide was isolated from the roots of Scorzonera austriaca. The structure was elucidated on the basis of spectral methods including 2D NMR.
Purification and Primary Structure Determination of a Novel Polypeptide Isolated from Mistletoe Viscum coloratum
Jing Lin KONG , Xiu Bao DU , Chong Xu FAN , Ying CAO , Hui JIANG , Jian Fu XU , Xiao Jun ZHENG
2004, 15(11): 1311-1314
[Abstract](173) [FullText HTML] [PDF 1545KB](0)
A novel polypeptide was isolated from mistletoe Viscum coloratum. The primary structure of the polypeptide 'named viscotoxin B2' was determined to be KSCCKNTTGRNIYNT CRFAGGSRERCAKLSGCKIISASTCPSDYPK by Edman degradation. Viscotoxin B2 shared high sequence homology with viscotoxins isolated from Viscum album. Pharmacological experiments showed that viscotoxin B2 had distinct cytotoxic activity on tumor cells. Viscotoxin B2 could be used as a leading compound in cancer therapy.
Trace Determination of Zirconium(Ⅳ) by Anodic Adsorptive Voltammetry at a Carbon Paste Electrode
Xun MAO , Huan Xin LAI , Ju Nan LI , Peng GAO , Zhi Hong YAN
2004, 15(11): 1315-1318
[Abstract](165) [FullText HTML] [PDF 1533KB](0)
A new sensitive adsorptive voltammetric method was described for the determination of zirconium at a carbon paste electrode (CPE) in the presence of alizarin complexone (ALC). Optimal analytical conditions are: 1.0×10-6 or 5.0×10-7 mol/L ALC, 0.20 mol/L HAC-NaAc (pH 4.3), accumulation for 60 s at 0V (vs. SCE), and linear scanning from 0V to 1.0V at 250 mV/s. The peak potential of the complex is at 0.81V. By using a model JP-303 polarographic analyzer, 2.0×10-10 mol/L (S/N=3) zirconium can be detected with a 90 s accumulation, when the 2nd-order derivative linear sweep technique is used, and the linear range is 6.0×10-10-2.0×10-8 mol/L (5.0×10-7 mol/L ALC) and 2.0×10-8-2.0×10-7mol/L (1.0×10-6 mol/L ALC), respectively. The developed method was applied to the determination of trace zirconium in the ore samples with satisfactory results.
A Novel Method for the Selective Determination of Silver (Ⅰ) Ion
Jian Gong LIANG , Hai Yan XIE , Xin Ping AI , Zhi Ke HE , Dai Wen PANG
2004, 15(11): 1319-1322
[Abstract](161) [FullText HTML] [PDF 1395KB](0)
Water-soluble CdSe quantum dots (QDs) capped by bovine serum albumin (BSA) is described as selective silver (Ⅰ) ion probe based on their fluorescence (FL) quenched by silver ion at pH 5.7. The detection limit is 3×10-7 mol L-1 for silver ion. The interference was also investigated.
Preparation and Application of an Immunoaffinity Column for Direct Extraction of Morphine and its Analogs from Opium
Xiao Hua QI , Jian Qiu MI , Xin Xiang ZHANG , Wen Bao CHANG
2004, 15(11): 1323-1326
[Abstract](161) [FullText HTML] [PDF 1321KB](0)
A rapid, simple and accurate method using an immunoaffinity column (IAC) and capillary electrophoresis (CE) for the analysis of the major alkaloids in opium is developed. The IAC was synthesized by coupling specific morphine polyclonal antibodies to CNBr-actived Sepharose 4B. The IAC showed high selectivity and obvious enrichment to morphine, codeine, dionin and thebaine. The extraction solution was analyzed by CE with β-cyclodextrin as an additive. Recoveries of the four alkaloids from PBS were between 93%-105% with RSD value less than 5.0%. The result showed that this method was practical for the determination of morphine analogs in opium.
Gas Chromatographic Enantiomer Separation of Cyclopropane Derivatives on Three 2, 6-Di-O-allyl-3-O-acylated-β-cyclodextrins Chiral Stationary Phases
Ming Ming YIN , Xue Yan SHI , Qing Hua BIAN , Nan LI , Min WANG
2004, 15(11): 1327-1330
[Abstract](162) [FullText HTML] [PDF 1177KB](0)
Eight pairs of enantiomers of cyclopropane derivatives were resolved on capillary gas chromatographic columns using three new 2, 6-di-O-allyl-3-O-acylated-β-cyclodextrins as chiral stationary phases. It was found that the three β-CDs can separate some of the racemic cyclopropane derivatives well.
Characterization of the Interaction between Bovine Serum Albumin and Lomefloxacin by Capillary Zone Electrophoresis
Ming GUO , Qing Sen YU , Jian Wei YAN , Fei TAN , Guo Zheng MA
2004, 15(11): 1331-1334
[Abstract](159) [FullText HTML] [PDF 1347KB](0)
Three capillary zone electrophoresis (CZE) methods of the frontal analysis (FA), vacancy peak (VP) and simplified Hummel-Dreyer (SHD) were applied to investigate interaction between bovine serum albumin (BSA) and lomefloxacin, the experimental condition was established after a large number of tests. Based on the site-binding model, the binding parameters were measured according to the site model by Scatchard.
Studies on Chromatography Fingerprint of Hongqi by High-performance Liquid Chromatography
Shi Lan FENG , Fang Di HU , Jian Xiong ZHAO , Jing Wen XU , Li Ren CHEN
2004, 15(11): 1335-1338
[Abstract](166) [FullText HTML] [PDF 1193KB](0)
Chromatography fingerprint (CFP) of 10 samples of hongqi were studied. 23 common peaks were analyzed, their average similarity was 97.29%. CFP were positioned with main index composition such as formononetin, calycosin and then the contents of index composition were determined. The character and exclusive of CFP of 10 samples of hongqi were clear. CFP and content determination of index composition of hongqi could be used to evaluate the quality of hongqi comprehensively.
Chemically Modified Chitosan Beads as Molecularly Imprinted Polymer Matrix for Adsorptive Separation of Proteins
Tian Ying GUO , Yong Qing XIA , Guang Jie HAO , Bang Hua ZHANG
2004, 15(11): 1339-1341
[Abstract](165) [FullText HTML] [PDF 1005KB](0)
In a phosphate buffer, a hemoglobin (Hb)-imprinted polymer complex was prepared using maleic anhydride (MAH) modified chitosan beads as matrix, acrylamide (AM) as functional monomer, N,N-methylenebisacrylamide (MBA) as cross-linker and potassiumpersulfate (KPS)/sodium hydrogen sulfite (NaHSO3) as initiators. Langmuir analysis showed that an equal class of adsorption was formed in the molecular imprinting polymer (MIP), and the MIP has high adsorption capacity and selectivity for the imprinted molecule. The MIP can be reused and the recovery was approximately 100% at low concentration.
Preparation and Characterization of Nano-polymer Porous MgO
Xue Liang ZHAI , Ai Dong ZHAO , Mi Ying JIA
2004, 15(11): 1342-1344
[Abstract](175) [FullText HTML] [PDF 1240KB](0)
Porous carrier MgO which was aggregated by nano-particles has been firstly prepared by using a normal technology route. The MgO was rod-shaped and had large surface area. The factors which affect grain size and microstructure of MgO were explored.
A New Method for the Synthesis of Selenium Nanoparticles and the Application to Construction of H2O2 Biosensor
Juan ZHANG , Sheng Yi ZHANG , Jing Juan XU , Hong Yuan CHEN
2004, 15(11): 1345-1348
[Abstract](1107) [FullText HTML] [PDF 1716KB](13)
The well-distributed, stable selenium nanoparticles (10 nm) with good adhesive ability and biocompatibility were successfully synthesized by using the template of chitosan cross-linked with glutaradehyde. The resulting selenium nanoparticles were used as a new carrier for horseradish peroxidase to construct H2O2 biosensors with good performances.
Synthesis and Photoluminescence of a New Red Phosphorescent Iridium(Ⅲ) Quinoxaline Complex
Guo Lin ZHANG , Ze Hua LIU , Hai Qing GUO
2004, 15(11): 1349-1352
[Abstract](171) [FullText HTML] [PDF 1235KB](0)
A new cyclometalated iridium(Ⅲ) complex with the formula [Ir(DPQ)2(acac)] (DPQ=2,3-diphenylquinoxaline; acac=acetylacetone) was prepared. The structure of the complex was confirmed by Elemental Analysis (EA), 1H NMR, and mass spectroscopy (MS). The UV-vis absorption and photoluminescent properties of the complex were investigated.
Manufacture of Boron-free Magnesia with High Purity from Residual Brine
Fa Qiang LI , Bao Ping LING , Pei Hua MA
2004, 15(11): 1353-1356
[Abstract](143) [FullText HTML] [PDF 1236KB](0)
A novel method for removing boron with ion exchange resin from residual brines to manufacture boron-free magnesia is described. The concentration of boron in the target magnesia manufactured thereby from Qinghai salt lakes is lower than 5μg/g, and the typical D50 size of product is 10.625μm.
Effect of TiO2 Support on the Composition, Morphology and Catalytic Property of the NiB Amorphous Alloy Catalyst
Lai Jun WANG , Ming Hui ZHANG , Wei LI , Ke Yi TAO
2004, 15(11): 1357-1360
[Abstract](150) [FullText HTML] [PDF 1581KB](0)
Both the unsupported and supported NiB amorphous alloy catalysts (NiB and NiB/TiO2) were prepared by the chemical reduction method. Their catalytic activities were tested by the hydrogenation of sulfolene. The interactions between the NiB alloy and TiO2 were discussed for the first time by using XRD, ICP, SEM and TEM.
Immobilization of Glucose Oxidase on Cellulose/Cellulose Acetate Membrane and its Detection by Scanning Electrochemical Microscope (SECM)
Jin Sheng ZHAO , Zhen Yu YANG , Yi He ZHANG , Zheng Yu YANG
2004, 15(11): 1361-1364
[Abstract](207) [FullText HTML] [PDF 1542KB](5)
Cellulose/cellulose acetate membranes were prepared and functionalized by introducing amino group on it, and then immobilized the glucose oxidase (Gox) on the functionalizd membrane. SECM was applied for the detection of enzyme activity immobilized on the membrane. Immobilized biomolecules on such membranes was combined with analysis apparatus and can be used in bioassays.
Formation and Characterization of Europium Bisphthalocyanine Organic Nanowires by Electrochemical Deposition
Han Bo ZHOU , Hong Zheng CHEN , Lei CAO , Yu RONG , Jin Zhi SUN , Mang WANG
2004, 15(11): 1365-1368
[Abstract](157) [FullText HTML] [PDF 1640KB](0)
Europium bisphthalocyanine (EuPc2) nanowires were prepared by electrochemical deposition method. Scanning electron microscopy (SEM) images show the evolution of the morphologies of nanowires obtained under different deposition time (Td). The optical properties of europium bisphthalocyanine films were studied by UV-Vis absorption spectra. The morphology of EuPc2 nanowires could be controlled by changing deposition conditions, which provides a useful method to make organic nanowires.
Low Sheet Resistance Counter Electrode in Dye-sensitized Solar Cell
Gui Qiang WANG , Rui Feng LIN , Miao WANG , Chang Neng ZHANG , Yuan LIN , Xu Rui XIAO , Xue Ping LI
2004, 15(11): 1369-1372
[Abstract](142) [FullText HTML] [PDF 1336KB](1)
In order to search for the high efficiency and low sheet resistance counter electrode in dye-sensitized solar cell, we used Ti plate as the conducting substrate to prepare the counter electrode by thermal decomposition of H2PtCl6. Ti plate counter electrode shows low sheet resistance, good reflecting performance and matching kinetics. The dye-sensitized solar cell with the Ti plate counter electrode shows better photovoltaic performance than that of the cell with the fluorine-doped tin oxide-coated glass counter electrode.
Synthesis of a Novel Organic Soluble and Thermal-stable Fullerene-perylene Dyad
Jian Li HUA , Fang DING , Fan Shun MENG , He TIAN
2004, 15(11): 1373-1376
[Abstract](155) [FullText HTML] [PDF 1568KB](0)
A novel organic soluble and thermal-stable fullerene-perylene dyad, in which a perylene moietyis attached to C60, has been prepared by 1, 3-dipolar cycloaddition of the azomethine ylides generated in situ from the aldehyde and N-methylglycine and characterized by NMR, FT-IR, TGA, absorption and fluorescent spectra etc.
Cyclic Oligomers of Phenolphthalein Polyarylene Ether Sulfone (Ketone): Preparation Through Cyclo-depolymerisation of Corresponding Polymers
Hong Hua WANG , Jin Ying DING , Tian Lu CHEN
2004, 15(11): 1377-1379
[Abstract](151) [FullText HTML] [PDF 882KB](0)
Cyclic oligomers of phenolphthalein polyarylene ether sulfone(ketone) were prepared through cyclo-depolymerisation of corresponding polymers using CsF as the catalyst in dipolar aprotic solvent DMAc and DMF, and a family of macrocycles containing from dimer up to at least heptamer were confirmed by GPC, HPLC and MALDI-TOF-MS. The yields of cyclics get as high as 86.3% and 87.9% respectively.
3D-QSAR Analysis of Agonists of nAChRs: Epibatidine Analogues
Hua Bei ZHANG , Chun Ping LIU
2004, 15(11): 1380-1382
[Abstract](157) [FullText HTML] [PDF 1253KB](0)
A 3 D-QSAR about nAChRs agonists-epibatidine analogues was performed using the CoMFA and CoMSIA. The correlation coefficients were Rcv2=0.546, Rncv2=0.907 in CoMFA and Rcv2=0.655, Rncv2=0.962 in CoMSIA of the final model. The prediction using the final models to the test set was r2=0.675 in CoMFA and r2=0.462 in CoMSIA. This model will be useful in the design of novel compounds with high affinity.
Theoretical Study on Intramolecular Proton Transfer of Perylenequinonoid Derivatives
Liang SHEN , De Zhan CHEN
2004, 15(11): 1383-1386
[Abstract](171) [FullText HTML] [PDF 1364KB](0)
Intramolecular proton transfer of hypomycin A in the ground state S0 and singlet excited state S1 were calculated by high level quantum chemical method in this letter. It was found that the IPT barriers for I→TS1 are 38.56 kJ/mol in S0 and 8.19 kJ/mol in S1, while those for I→TS4 get approximately 17 kJ/mol higher in S0 and 28 kJ/mol higher in S1. The calculation of IPT rate constants suggests that the experiment observed process of PQD is in S1. The height of the IPT barriers correlate not only with the variance of charge for labile hydrogen, the change of H-bond's length, the change of O-H bond's length and the change of O-O distance, but also with the reactant molecular H-bond's length. Moreover, the correlations are the same for S0 and S1.
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