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Photogeneration of the free radicals and singlet oxygen by chrysophanol from rheum

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Science china chemistry 2004年第5期47卷 381-387页

作者： RAO Jing1,2. XIE Jie1, ZHAO Jingquan1 & ZHU Teng2.1. Key Laboratory of Photochemistry, Center for molecular Science, Institute of chemistry, The Chinese Academy of sciences, Beijing 100080, china 2. University of Science and Technology Beijing, Beijing 10083, china 1. Key Laboratory of Photochemistry Center for Molecular Science Institute of Chemistry The Chinese Academy of Sciences 100080 Beijing China 2. University of Science and Technology Beijing 10083 Beijing China

In the current work, chryosphanol (MHAQ) was isolated and purified from rheum, and the photosensitization activities were studied. In nitrogen-saturated DMSO solution, irradia- tion of chryosphanol (MHAQ) with visible light (>430 nm) produced the semiquinone radical anions (MHAQ??), which was intensified significantly by an electron donor NADH, suggesting electron transfer between the excited and ground state photosensitizer molecules. In an air-saturated DMSO solution, superoxide radical anions (O2.), trapped by DMPO, were detected. ?? It was proved that O2.was not originated from the singlet oxygen (1O2. but dependent on DMPO, ?? chrysophanol, oxygen and the irradiation time. The singlet oxygen and OH could also be pro- ? duced by the photosensitization of the photosensitizer. These suggest that chrysophanol pos- sesses the photosensitization activity via Type I mechanism and Type II mechanism. To evaluate the photosensitization activities of MHAQ, emodin and mixed anthraquinone derivatives ex- tracted from rheum, the relative productivities of O2.were estimated to be 1.8, 1.1 and 1.0 re- ?? spectively and the quantum yields for singlet oxygen to be 0.36, 0.53 and 0.14 respectively. Therefore, these low-cost pigments may be potentially used as phototherapeutic medicine for some kind of vascular diseases or photo-activated pesticides.

关键词： chrysophanol, ESR, semiquinone radical anions, superoxide radical anions, hydroxyl radical, singlet oxygen.

Silylated and acetylated β-cyclodextrins for gas chromatographic stationary phases

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Journal of Central South University of Technology 2001年第4期8卷 239-243页

作者： TANG Ke wen 1,2.,YI Jian ming 2.ZHOU Chun shan 1,ZHONG Shi an 1 (1. college of chemistry and Chemical Engineering, Central South University, Changsha 410083,{2. 2. college of chemistry and Chemical Engineering, Yueyang Normal University 1. college of chemistry and Chemical Engineering Central South University 410083 Changsha China 2. college of chemistry and Chemical Engineering Yueyang Normal University 414000 Yueyang China

Two new chiral stationary phases, 2.3 di O acetyl 6 O trimethylsilyl β cyclodextrin (DATBCD) and 2.6 di O trimethylsilyl 3 O acetyl β cyclodextrin(DTABCD), were synthesized, their structures were identified by means of infrared and NMR spectra. Capillary columns were coated with the two stationary phases by dynamic method. The chromatographic properties, and enantiomers separation, such as ketone, esters, alcohols and olefines, were investigated on the silylated and acetylated β cyclodextrin stationary phases. The experimental results show that the silylated and acetylated β cyclodextrins are suitable to be used as capillary gas chromatographic stationary phases, the relative polarity of DATBCD and DTABCD stationary phases is respectively 4143 and 392., the column efficiencies are respectively 3084 and 4198, and DATBCD is of stronger enantioselectivity than DTABCD, capacity factor of the first eluted enantiomer ( k 1) and separation factor(α)of α phenylethanol on DATBCD stationary phase are respectively 8.2. and 1.019.

关键词： capillary gas chromatography silylated and acetylated β-cyclodextrins enantiomeric separation

Proton Conducting Composite Membranes from Sulfonated Polyether Ether Ketone and SiO_2

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Journal of wuhan University of Technology(Materials Science) 2009年第1期24卷 95-99页

作者：张高文 college of chemistry and Environment Hubei University of Technology

Proton conducting composite membranes from sulfonated polyether ether ketone and SiO2.for direct methanol fuel cell （DMFC） application were prepared with sulfonated polyether ether ketone（SPEEK） and tetracethoxy silane（TEOS） by sol-gel method. The covalent crosslinking structure was formed between —SO3H of SPEEK via SiO2. The SEM images show that the interfacial compatibility of SPEEK and SiO2.is improved obviously and SiO2.disperses uniformly in the polymer matrix and the particle diameter of SiO2.does not exceed 40 nm. The proton conductivity of composite membranes decreases slightly compared with the SPEEK membrane while the methanol permeability and swelling of composite membrane are improved remarkablely owing to covalent cross-linking between —SO3H and SiO2..

关键词： direct methanol fuel cell sulfonated polyether ether ketone sol-gel method proton conductivity methanol permeability

Approach to synthesis of novel chiral 3-chloro-2.5H)- furanone and its application in asymmetric reactions

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Chinese Science Bulletin 2000年第8期45卷 711-716页

作者： HUANG Hui & CHEN Qinghua1. Department of chemistry, Tonghua Teacher’s college, Tonghua 134002.{2. 2. Department of chemistry, Beijing Normal University, Beijing 100875,{2. Department of chemistry Tonghua Teacher’s College Tonghua China Department of chemistry Beijing Normal University Beijing China

The synthetic method of the novel chiral synthon, 5-/-menthyloxy-3-chloro-2.(5H)-furanone 5a and its application in asymmetric reactions were investigated. 5a is easily obtained in highly optical purity, and acts as a stable acceptor of Michael addition with oxygen nucleophiles in tandem double Michael addition / internal nucieophilic substitution to offer the spiro-cyclopropane derivative containing four stereogenic centers 8, which it is difficult to obtain by routine methods. The synthetic methods for 5a and 8 are reported in detail and the new compounds are identified on the basis of their analytical data and spectroscopic data, such as UV, IR, H NMR,13 C NMR, MS and elementary analysis. The absolute configuration of the interesting spiro-cyclopropanes, spiro [1-chloro-4-(/-menthyloxy)-5-oxo-6-oxa-biscyclo[3.1.0]hexane-2.3i(4’-/-menthyloxy-5’-/-menthyloxy- butyrolactone)] 8 was established by X-ray crystallography. This result can provide important synthetic strategy in synthesis of some complex

关键词： new chiral synthon. 5-l-menthyloxy-3-chloro-2.(5H)-furanone absolute configuration spiro-cyclopropane derivative containing multiple chiral centers.

Interfacial behaviors of PMMA-PEO block copolymers at the air/water interface

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Science china chemistry 2005年第6期48卷 567-573页

作者： CHENG Caixia1, JIAO Tifeng2. TANG Rupei1, LIU Minghua2.& XI Fu1 1. State Key Laboratory of Polymer Physics and chemistry, Joint Laboratory of Polymer Science and Materials, Institute of chemistry, Chinese Academy of {2., Beijing 100080, china 2. CAS Key Laboratory of Colloid and Interface Science, Institute of chemistry, Chinese Academy of {2., Beijing 100080, china 1. State Key Laboratory of Polymer Physics and chemistry Joint Laboratory of Polymer Science and Materials Institute of Chemistry Chinese Academy of Sciences 100080 Beijing China 2. CAS Key Laboratory of Colloid and Interface Science Institute of Chemistry Chinese Academy of Sciences 100080 Beijing China

Diblock copolymer of PMMA2.1-b-PEO114 and triblock copolymer of PMMA12.-b- PEO2.7-b-PMMA12. were synthesized and their interfacial properties at the air-water interface were investigated, where both blocks of polyethylene oxide (PEO) and poly(methyl methacrylate) (PMMA) are surface active but the former is soluble in water while the latter is not. Both the block copolymers could form monolayers with two obvious transition regions. The first transition point is around 10 mN/m, which could be assigned to the pancake-brush change of the PEO chains. The other is around 18 mN/m, which could be ascribed to the condensed packing of PMMA. The surface morphological changes during the compression of the Langmuir monolayers are inves-tigated by using the AFM and SEM methods for the films deposited at different surface pressure or molecular areas. At a lower surface pressure, a typical morphology of PEO-con- taining lipopolymers is observed. Upon compression, sphere-dominant morphologies were observed. While the diblock copolymer is easy to folding, the triblock copolymer is in favor of formation of circular domains through vesiculation.

关键词： PMMA-PEO, block copolymers, monolayer, Langmuir-Blodgett films, AFM.

Status of study on biological and toxicological effects of nanoscale materials

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Science china chemistry 2005年第5期48卷 385-394页

作者： WANG Bing1, FENG Weiyue1, ZHAO Yuliang1, XING Gengmei1, CHAI Zhifang1, WANG Haifang2.& JIA Guang3 1. Laboratory for Bio-Environmental Health sciences of Nanoscale Materials (Nanosafety Lab), Institute of High Energy Physics, Chi-nese Academy of sciences, Beijing 100049,{2. 2. college of chemistry and molecular Engineering, Peking University, Beijing 100871,{2. 3. Department of Occupational and Environmental Health sciences, School of Public Health, Peking University, Beijing 100083,{2. 1. Laboratory for Bio-Environmental Health sciences of Nanoscale Materials (Nanosafety Lab) Institute of High Energy Physics Chinese Academy of Sciences 100049 Beijing China 2. college of chemistry and {2. Engineering Peking University 100871 Beijing China 3. Department of Occupational and Environmental Health sciences School of Public Health Peking University 100083 Beijing China

Because the physical and chemical properties of nanosized materials mostly differ from the existing microsized materials, their potential impacts on human health and the envi-ronment will be topics under the serious discussions in press and in a number of international scientific journals. We analyze and summarize the existing data of the experimental study on the biological activities and adverse effects of nanoscale materials/particles including single wall carbon nanotubes, multi wall carbon nanotubes, titanium oxide and iron powders. Though some biological behaviors of nanoscale materials observed cannot be understood on the basis of the current knowledge, as the existing data are mostly preliminary, it is too early to make some ex-clusive conclusions on biological activities (or the toxicity) of any of nanoscale materials. The experimental techniques, the current topics, and the future research directions for this new re-search field are also discussed.

关键词： nanomaterials, single wall carbon nanotubes, multi wall carbon nanotubes, titanium oxide and iron, biological activity and toxicological effect.

Synthesis and Characterization of Two New Photochromic Inorganic-organic Hybrid Materials Based on Keggin-type Polyoxometalates

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Journal of wuhan University of Technology(Materials Science) 2008年第3期23卷 367-371页

作者：库宗军 college of chemistry and Materials {2. Xiaogan University

Two new photochromic inorganic-organic hybrid materials formed from Keggin-type polyoxometalates（POMs） and metronidazole （C6H9N3O3, MNZ）, formulated as H3PMo12.aO-3MNZ·3H2. （1） and H3PW12.40.3MNZ·3H2.（2., were synthesized and characterized by elemental analysis, IR spectra, electronic spectra, electron spin resonance （ESR） spectra and thermogravi-metry-differential thermal analysis （TG-DTA）. Reflectance spectra show the presence of weak intermolecular charge transfer between the organic and inorganic moieties in the solid state. The photochromic properties were studied by solid diffuse reflectance spectra and ESR spectra, and the photochromic reactions were found to exhibit first-order kinetics. TG-DTA showed that two hybrid materials have similar thermal behavior.

关键词： polyoxometalate metronidazole hybrid material photochromism kinetics

A Series Piezoelectric Quartz Crystal Response Kinetics for *** Growth in the Presence of Cu(Ⅱ)

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Journal of Central South University 2000年第1期12卷 15-19页

作者： CHAI Li yuan 1,2.,WEI Wan zhi 2.YAO Shou zhuo 2.1. Department of Metallurgical Science and Engineering, Central South University of Technology, Changsha 410083, china 2. college of {2. and Chemical Engineering, Hunan University, Changsha 1. Department of Metallurgical Science and Engineering Central South University of Technology 410083 Changsha China 2. college of chemistry and Chemical Engineering Hunan University 410082 Changsha China

The kinetics on the growth of *** in the presence of Cu(Ⅱ) was studied using of series piezoelectric quartz crystal (SPQC). Arsenic ion inhibits the growth of *** , which is consistent with the previous results by other measuring methods. This further demonstrates that the SPQC can monitor the chemical activity of *** growth. Cupric ion accelerates the growth of *** . The mechanism was discussed, i. e., copper promotes the protein enzyme of *** , rusticyanin, to form over the range of cupric ion concentration studied. The reaction order of cupric ion in accelerating the bacterial growth is 0.067. The growth of *** is dependent on temperature, the apparent reaction activation energy decreases from 2..56 kJ/mol to 18.32.kJ/mol because of the addition of 10 mg/L Cu(Ⅱ) to the bacterial growth solution of pH 2.0 at initial inoculum of 10%.

关键词： series piezoelectric quartz crystal T.ferrooxidans growth kinetics sigmoid curve cupric ion

Synthesis, Crystal Structures and Catalysis of Dinuclear Cd(Ⅱ) Complexes Bridged by Unusual (N,O,O′)-Coordinated α-Amino Acids

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Chemical Research in Chinese Universities 2012年第1期28卷 73-78页

作者： DENG Dong-sheng1,2. WANG Li1, PEI Ya-mei1, FENG Lu2.and LIU Chang-lin1 1. Key Laboratory of Pesticide & Chemical Biology, Ministry of Education, School of chemistry, Central china Normal University, {2. 430079, P. R. china 2. college of chemistry and Chemical Engineering, Luoyang Normal University, Luoyang 47102., P. R. china School of chemistry Central China Normal University Key Laboratory of Pesticide & Chemical Biology Ministry of Education Wuhan 430079 college of chemistry and Chemical Engineering Luoyang Normal University Luoyang 471022

Four dinuclear amino acid cadmium（II） complexes [Cd2.tren）2.dl-alaninato）]（ClO4）3·H2.（I）, [Cd2.tren）2. （l-alaninato）]（ClO4）3·H2.（II）, [Cd2.tren）2.dl-phenylalaninato）]（ClO4）3（III） and [Cd2.tren）2.l-phenylalaninato）]· （ClO4）3（IV）, constructed from mixed ligands of tris（2.aminoethyl）amine（tren） and racemic or natural amino ac ids（amino acids=dl or l-alanine, and dl or l-phenylalanine）, have been synthesized and characterized by X-ray crys tallography. The structural analysis of complexes I and III reveals that the cadmium centers are coordinated by one tren ligand and one amino acid molecule with the unusual （N,O,O′）-bridged mode, resulting in asymmetric chromo phores of CdN4O and CdN5O in complex I, CdN4O2.and CdN5O in complex III, respectively. The utility of the four complexes as efficient water-compatible Lewis acid catalysts for the direct aldol reaction in water was examined. The reaction proceeded smoothly to afford the corresponding β-hydroxy ketones in up to 99% yield. Moreover, the dias tereoselectivity of the reaction favors the formation of the syn-isomers.

关键词： Dinuclear cadmium(II) complex Amino acid Aldol reaction