Chemical Research in Chinese Universities

Cover and Content of Chemical Research in Chinese Universities Vol.30 No.2(2014)

2014, 30(2): 0-0.

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Light-harvesting Complex Ⅱ Sensitized Oxide Photoanodes with Organic Acceptor Molecule as Electron Transfer Mediator

DONG Wenjing, ZHANG Tianning, LIU Kun, SUN Ruixue, HUANG Chanyan, SUN Yan, LIU Cheng, CHEN Xin, YANG Guoqiang, YANG Chunhong, DAI Ning

2014, 30(2): 181-184. doi:10.1007/s40242-014-3516-1

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Synthesis, Structures and Properties of Two Complexes Based on Benzimidazole or Benzothiazole Ligand

ZHANG Zhongqiang, DI Di, ZHAI Jingshuo, WU Lili, ZHU Qinlei, XU Yanqing, HUANG Rudan

2014, 30(2): 185-189. doi:10.1007/s40242-014-3434-2

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Two complexes, Co(Hbim)₂(NCS)₂(Hbim=benzimidazole)(1) and [Cu(Hbzt)SCN]_n(Hbzt=benzothiazole) (2) were synthesized by the same synthesis method and characterized by elemental analysis, infrared spectroscopy(IR), thermogravimetric analysis(TGA), X-ray powder diffraction(XRPD) and single-crystal X-ray diffraction. The results from the single-crystal X-ray diffraction indicate that complex 1 is zero-dimensional(0D) framework and complex 2 is 2-dimensional(2D) framework. In complex 2, the 3-dimensional(3D) supermolecular architecture was built up by means of π-π stacking interaction, and two helical chains existed in its structure. The luminescence properties and the magnetic properties of the two complexes were investigated.

Luminescent Properties of Terbium(Ⅲ) and Europium(Ⅲ) Complexes with Six 4-Acetyl-bispyrazolones

GOU Ruhu, WANG Yaling, YANG Rudong, LAN Yan

2014, 30(2): 190-193. doi:10.1007/s40242-014-3380-z

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The lowest triplet energy levels of the six ligands(T) were determined to be 22989 cm^-1[1,3-bis-(1'-phenyl-3'-methyl-5'-pyrazolon-4')-1,3-propanedione, BPMPTD], 23148 cm^-1[1,4-bis-(1'-phenyl-3'-methyl-5'- pyrazolon-4')-1,4-butanedione, BPMPBD], 23419 cm^-1[1,5-bis-(1'-phenyl-3'-methyl-5'-pyrazolon-4')-1,5-pentane-dione, BPMPPD], 23310 cm^-1[1,6-bis-(1'-phenyl-3'-methyl-5'-pyrazolon-4')-1,6-hexanedione, BPMPHD], 21978 cm^-1[1,9-bis-(1'-phenyl-3'-methyl-5'-pyrazolon-4')-1,9-nonanedione, BPMPND] and 21930 cm^-1[1,10-bis-(1'-phenyl-3'-methyl-5'-pyrazolon-4')-1,10-decanedione, BPMPDD], respectively. It was explained satisfactorily that the six ligands are more efficient for sensitizing the luminescence of Tb³⁺ than that of Eu³⁺ at room temperature, and the order of the luminescent intensities for the Tb³⁺ complexes is explained by the relative energy gap between T and ⁵D_J of Tb³⁺ or Eu³⁺. As a conclusion, when 2700 cm^-1<ΔE(T-⁵D₄)<3000 cm^-1, the luminescent intensity of the Tb³⁺ complex is the strongest. This means that the lowest triplet energy level of the ligand is a chief factor to dominate RE³⁺ luminescence.

Structural Characterization and Luminescence Properties of Two 4d-4f Ln-Ag Coordination Compounds Based on Dinuclear Lanthanide Clusters

ZHANG Yu, CHEN Lei, JU Weiwei, XU Yan

2014, 30(2): 194-199. doi:10.1007/s40242-014-3368-8

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Two new compounds,[ErAg(INA)₂(C₂O₄)]·2H₂O(1)(HINA=nicotinic acid) and [Tb_0.8Y_0.2Ag₂(IN)₄·(H₂O)₅]·NO₃·2H₂O(2)(HIN=isonicotinic acid), based on the {Ln₂} building units, have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, infrared spectroscopy, thermal analysis and powder X-ray diffraction(PXRD). Single-crystal X-ray diffraction data reveal that both compounds crystallized in the low-symmetry triclinic space group P1. Compound 1 is a 3D heterometallic coordination framework based on {Er₂} clusters, oxalate ligands and bridging [Ag(INA)] linkers, while compound 2 consists of 0D [Tb_0.8·Y_0.2Ag₂(IN)₄(H₂O)₅]₂ subunits that give a 3D supramolecular structure through hydrogen bond interaction. The photoluminescent properties of both compounds(1 and 2) were studied.

Facile Synthesis of Al-pillared Mesoporous Montmorillonite Assisted with Concentrated Al₁₃ Solution

ZHAO Tianqi, LI Wenjie, WANG Hongyan, MENG Fanyu

2014, 30(2): 200-204. doi:10.1007/s40242-014-3271-3

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Al-pillared mesoporous montmorillonite was facilely synthesized from concentrated Al₁₃ solution obtained by vacuum concentrating-ultrasonic pillaring strategy. Concentrated Al₁₃ solution could reduce the process of pillare and increase pillaring efficiency. The absolute value of layer distance could be increased by 0.96 nm via concentrated Al₁₃ solution pillare. ²⁷Al NMR indicates that Al Keggin ions of concentrated Al₁₃ are arranged in a more regular way by vacuum concentrating method. The Al-pillared mesoporous montmorillonite from concentrated Al₁₃ solution has bigger specific surface area and even pore size distribution which were characterized by X-ray diffraction(XRD) and nitrogen adsorption measurement. Furthermore the catalytic activity of Al-pillared montmorillonite loaded Ni and Mo catalysts was tested by the hydrodesulfurization of thiophene. The thiophene conversion reached 77.5%, which was higher than the corresponding value reported in the literature.

Voltammetric Determination of Epinephrine in the Presence of Uric Acid Based on Aminated Graphene and Ag NPs Hybrid Membrane Modified Electrode

XU Huanhuan, WANG Xueliang, CHEN Rong, YU Zhangyu

2014, 30(2): 205-210. doi:10.1007/s40242-014-3463-x

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A hybrid membrane consisted of aminated graphene and Ag nanoparticles(Ag NPs) was prepared on the surface of glassy carbon electrode(GCE) by cyclic voltammetry(CV) with aminated graphene(GR-NH₂) as matrix for immobilizing Ag NPs. The morphology and electrochemical properties of this hybrid membrane were characterized by scanning electron microscopy(SEM) and CV, respectively, and on this membrane, the voltammetric behaviors of epinephrine(EP) were studied in detail. The membrane exhibited excellent eletro-catalytic activities for the redox of EP, and could resolve the electrochemical response of EP and uric acid(UA) into two oxidation peaks. The peak current of EP was linear with its concentration in the ranges of 0.916―18.3 μmol/L and 18.3―184 μmol/L. The detection limit was 2.0 nmol/L(S/N=3). The proposed modified electrode retained the advantages of easy fabrication, high sensitivity and good repeatability for the determination of EP.

Tumor Cell Detection Device Based on Surface Plasmon Resonance Imaging and Image Processing

YANG Mengchao, JIN Xinyu, YUAN Maokai, LIU Fan, LANG Yicong, WU Zhongyu, XIANG Liancheng, ZHOU Chao, OUYANG Bo, JIN Wei, MU Ying

2014, 30(2): 211-215. doi:10.1007/s40242-014-3415-5

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A laboratory-made tumor cell detection device was fabricated based on both surface plasmon resonance imaging(SPRi) and image processing. In this device, a gravity-induced flow injection chip(gFIC) was exploited to replace a pump. Also two charge coupled devices(CCDs) were used to detect HepG2 cells by SPRi and image processing, respectively. The results of two CCDs are associated. Protein A was used to modify the sensing surface. The inlet angle was carefully adjusted for the device to get an enhanced image. In the test, the contrast among cell solutions at different concentrations can be easily distinguished. The other CCD using image processing can tell false-positive in some degree. This detection is label-free, real time, and precise.

Preparation of a Hybrid Organic-inorganic Monolith for Extraction and Purification of Quercetin and Myricetin from Chamaecyparis obtusa

ZHU Tao, LEE Yuri, ROW Kyungho

2014, 30(2): 216-221. doi:10.1007/s40242-014-3394-6

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A new hybrid organic-inorganic monolithic cartridge was synthesized and used as the selective sorbent for the extraction and purification of quercetin and myricetin from Chamaecyparis obtusa via a solid-phase extraction method. The morphology of the monolithic material was examined by field emission-scanning electron microscopy and a Brunauer-Emmett-Teller(BET) test. The adsorption capacity of the obtained material for quercetin and myricetin was investigated by fitting the adsorption data to four different adsorption equations, of which the Langmuir-Freundlich isotherm was selected as the most suitable model. Under optimized conditions, good calibration curves were observed at nine concentrations ranged from 0.5 μg/mL to 100.0 μg/mL of quercetin and myricetin. The extraction recovery ranged from 74.5% to 84.6% and the inter-and intra-day relative standard deviations were <6%. This type of hybrid monolith has potential for the separation and purification of bioactive compounds from natural plant extracts.

Spectral Studies on the Conformational Transitions of Bovine Insulin During Denaturant-induced Unfolding

JI Xu, MA Xiaojuan, BIAN Liujiao

2014, 30(2): 222-227. doi:10.1007/s40242-014-3372-z

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Transitions among various molecule states and conformational changes of bovine insulin were investigated under different denaturing conditions by means of fluorescence phase diagrams, fluorescence quenching, 1-anilinonaphthalene-8-sulfonate(ANS) binding assay and circular dichroism(CD) spectra. In both guanidine hydrochloride(GuHCl)-and urea-denatured procedures, the spatial structure of insulin molecules changed from ordered states to relative unordered ones with the increasing of denaturant concentration. The GuHCl-denatured process followed a four-state model, for there were two intermediates existed in 2.0 and 6.0 mol/L GuHCl, respectively. Intermediate I₁ is more compact than the normal protein. And intermediate I₂ has lost most of the secondary structures. When GuHCl concentration was above 6.0 mol/L, the fluorophores originally existed in the internal of insulin molecules would expose to the surface. However, the urea-denatured process followed a three-state model, only one intermediate existed in 2.5 mol/L urea. During the urea-denatured procedure, the fluorophores originally existed in the internal of insulin molecules didn't expose to the surface.

Design, Synthesis and Insecticidal Activity of Novel Anthranilic Diamides Containing Oxime Ester and Diacylhydrazine Moieties

LIU Chen, ZHANG Jifeng, ZHOU Yunyun, WANG Baolei, XIONG Lixia, LI Zhengming

2014, 30(2): 228-234. doi:10.1007/s40242-014-3408-4

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Two series of novel anthranilic diamides containing oxime ester and diacylhydrazine moieties were designed and synthesized. Their structures were characterized by melting points, ¹H NMR, ¹³C NMR and high resolution mass spectrometry(HRMS). The single crystal structure of compound 7e was determined by X-ray diffraction and their evaluated insecticidal activity against oriental armyworm(Mythimna separata) indicates that some of the compounds exhibited moderate insecticidal activities. Among the 20 compounds, 6a and 6b show 100% larvicidal activity against Mythimna separate Walker at the test concentration of 100 mg/L.

Lewis Base Organocatalyzed Enantioselective Hydrosilylation of α-Keto Ketimines

LIU Lixin, ZHENG Yongsheng, HU Xiaoyan, LIAN Chunxia, YUAN Weicheng, ZHANG Xiaomei

2014, 30(2): 235-241. doi:10.1007/s40242-014-3396-4

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A chiral Lewis base organocatalyzed enantioselective hydrosilylation of α-keto ketimines was investigated. The reactions afforded various enantioenriched α-amino ketones with good yields(up to 95%) in moderate to good enantioselectivities(up to 98% e.e.). Furthermore, one of the products was reduced to a chiral 1,2-amino alcohol. Following cyclization of it with triphosgene generated a cannabinoid receptor 1(CB1) inhibitor with good diastereoselectivity.

Design, Synthesis and Properties of Novel C₆₀-Crown Dyads by 1,3-Dipolar Cycloaddition

DI Xingdong, YE Jinqi, YANG Fafu, GUO Hongyu, YAN Xiaoyun

2014, 30(2): 242-244. doi:10.1007/s40242-014-3296-7

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Based on the 1,3-dipolar cycloaddition of azomethine ylide generated in situ from aldehyde and sarcosine attached to C₆₀, two novel benzo-15-crown-5/C₆₀ dyads with a different linking chain in each were designed and synthesized in yields of 30% and 38%, respectively. It was found that their UV-Vis absorption spectra could be regulated hypsochromically by metal ions complexed. The long and soft linking chain was favorable for cooperate interaction of crown ether unit and C₆₀ unit.

Synthesis, Crystal Structure and Copper Complex of 1,3-Alternate p-tert-Butylthiacalix[4]arene 2-picolyl Schiff Base

HUANG Kun, LIU Kai, YAN Chaoguo

2014, 30(2): 245-249. doi:10.1007/s40242-014-3277-x

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A p-tert-butylthiacalix[4]arene-based polydentated ligand with four Schiff base units on 1,3-alternate position at lower rim has been prepared in three steps, which coordinated to copper ion to form a novel dicopper complex. The structures of the polydentated thiacalixarene ligand and copper complex were fully characterized by spectroscopy and X-ray single crystal diffraction method.

Facile Synthesis of Enantiomerically Pure1-(5-Bromo-2-chlorophenyl)-1-(4-ethoxyphenyl)ethane

ZHANG Shuo, WANG Wenjin, LI Chuan, LIU Peng, XU Weiren, TANG Lida, WANG Jianwu, ZHAO Guilong

2014, 30(2): 250-256. doi:10.1007/s40242-014-3257-1

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A facile 7-step procedure for the synthesis of enantiomerically pure 1-(5-bromo-2-chlorophenyl)-1-(4-ethoxyphenyl)ethanes[(R)-2 and(S)-2] that started from (5-bromo-2-chlorophenyl)(4-ethoxyphenyl)methanone 3 was developed. The key step was the resolution of 2-(5-bromo-2-chlorophenyl)-2-(4-ethoxyphenyl)acetic acid 6 by crystallizations of its L-and D-menthyl esters 7 and 8 from petroleum ether to give optically pure enantiomers 9 and 10, respectively. The absolute configurations of the products were unambiguously determined by single-crystal X-ray diffractions of four key intermediates, 9, 10, 13 and 14. This procedure is characterized by inexpensiveness, scalabi-lity and ability to produce two individual enantiomers of a diarylethane with unambiguously determined absolute configurations and high enantiomeric purities.

Design, Synthesis and Anticancer Activity of Novel 6-(Aminophenyl)-2,4-bismorpholino-1,3,5-triazine Derivatives Bearing Arylmethylene Hydrazine Moiety

HUANG Qiang, FU Qiangqiang, LIU Yajing, BAI Jinying, WANG Qianying, LIAO Huimin, GONG Ping

2014, 30(2): 257-265. doi:10.1007/s40242-014-3253-5

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In an attempt to develop potent and selective anticancer agents, we designed and synthesized a series of novel bis(morpholino-1,3,5-triazine) derivatives bearing aylmethylene hydrazine moiety and evaluated their cytotoxicity, in vitro, against H460(non-small-cell lung cancer), HT-29(human colorectal cancer) and MDA-MB-231(human breast cancer) cell lines. The pharmacological results indicate that all the compounds exhibit enhanced cytotoxicity than BMCL-200908069-1, and six target compounds(7e, 7h, 7j, 9a, 9b, 9c) were superior to PAC-1 against all the tested cancer cell lines. The most active compound 7j, with IC₅₀(inhibitory concentration 50%) values of 0.75, 0.34 and 0.60 μmol/L against HT-29, H460 and MDA-MB-231 cancer cell lines, was 39-, 28-, and 60-fold more potent than BMCL-200908069-1(29.24, 9.52 and 36.21 μmol/L), respectively.

K₃PO₄-Catalyzed Regiospecific Bromoamidation of β, β-Dicyanostyrene Derivatives with N-Bromoacetamide(NBA)

CHEN Zhanguo, LI Yanan, ZHOU Jimei, WANG Dan, GE Miao

2014, 30(2): 266-271. doi:10.1007/s40242-014-3234-8

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An efficient method for the bromoamidation of β,β-dicyanostyrene derivatives with N-bromoacetamide (NBA) was developed. This protocol provides a convenient process to convert β,β-dicyanostyrene derivatives into the vicinal haloamines in excellent yields(up to 99%) at room temperature in the presence of anhydrous K₃PO₄as a catalyst without the protection of the inert gaseous in CH₂Cl₂. A total of 11 examples were investigated and all the products showed the regionspecific feature. Based on the observation of different activities for the different substrates involving the electron-rich or electron-deficient β,β-dicyanostyrenes, a possible Michael addition mechanism was proposed.

Proteomics Dissection of Cold Responsive Proteins Based on PEG Fractionation in Arabidopsis

LI Shanyu, LIU Xiangguo, WANG Shang, HAO Dongyun, XI Jinghui

2014, 30(2): 272-278. doi:10.1007/s40242-014-3311-z

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Proteome profiling was performed on Arabidopsis plant exposed to cold stress at 4 ℃ for 24 h in an attempt to explore the mechanisms of plant climate adaptation. The polyethylene glycol(PEG) fractionation protocol developed in this lab was used to identify as many differentially expressed low-abundance proteins as possible. In comparison with those of the biological controls, 67 protein spots with at least two-fold difference in expression were identified for the plant exposed to cold temperatures; and from these spots, 50 proteins were successfully identified by matrix-assisted laser desorption/ionization time of flight mass spectrometry(MALDI-TOF MS). Bioinformatics studies on these proteins show that 57.8% of these proteins were localized in the chloroplast. Of these proteins, 8 ones have functions in photosynthesis, including glycine hydroxymethyltransferase, Rubisco large subunit, Rubisco activase, PSBO2, fructose-1,6-bisphosphate aldolase, NADP-dependent malate dehydrogenase, sedoheptulose bisphosphatase and photosystem Ⅱ reaction center PsbP family protein, suggesting that photosynthesis is greatly affected by cold stress. The identified proteins were validated by quantitative real-time polymerase chain reaction(qPCR). Taken together, our results suggest that the chloroplast might also act as a cold stress sensor and that photosynthesis-related proteins may play important roles in cold acclimation for Arabidopsis.

DRIFT Study on Cr₂O₃-SO₄^2-/TiO₂ Catalyst for Low Temperature Selective Catalytic Reduction of NO with NH₃

ZHANG Yiming, ZHANG He, ZHOU Liang, HAN Wei

2014, 30(2): 279-283. doi:10.1007/s40242-014-3446-y

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Chromium oxides supported on TiO₂ showed good activity for the selective catalytic reduction of NO by NH₃. The catalytic activity of Cr₂O₃-SO₄^2-/TiO₂ catalyst was greatly enhanced by the addition of SO₄^2- into TiO₂ support. The catalyst surface properties were characterized with NH₃-TPD(temperature programmed desorption) and H₂-TPR(temperature programmed reduction). The sulphate on the catalyst surface could enhance the acidity and redox of the catalyst obviously. The reaction mechanism on this catalyst was researched in detail by in situ diffuse reflectance Fourier transform infrared(FTIR) spectroscope. Eley-Rideal and Langmuir-Hinshelwood mechanism existed simultaneously for selective catalytic reduction(SCR) reaction of NO over Cr₂O₃-SO₄^2-/TiO₂ catalyst.

Immobilization of Chiral Catalyst on Amorphous Al₂O₃ for the Selective Hydrogenation of Ethyl 1H-Indole-2-carboxylate

GUAN Ruqi, CHAO Guoku, YE Caiping, WANG Yuxiang, LIU Yanmei, LI Haihua, ZHAO Yajuan, TAI Yulei

2014, 30(2): 284-288. doi:10.1007/s40242-014-3421-7

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Ru-B/γ-Al₂O₃catalyst was prepared by reductant impregnation method, which was applied in the selective hydrogenation of ethyl 1H-indole-2-carboxylate for producing ethyl 2,3,3a,7a-tetrahydro-1H-indole-2-carboxylate with hydrogen as reductant. Furthermore, we discussed the influences of substrate concentration, reaction solvent, hydrogenation temperature, initial hydrogen pressure and reaction time on the catalytic performance of the as-prepared catalyst. The obtained Ru-B/γ-Al₂O₃catalyst showed a high-efficiency for the selective hydrogenation of ethyl 1H-indole-2-carboxylate(>99% conversion and selectivity) in i-propanol used as solvent at a concentration of 10%(mass fraction) of ethyl 1H-indole-2-carboxylate, a pressure of hydrogen of 6 MPa and a reaction temperature of 373 K.

Enzymatic Promiscuity：Escherichia coli BioH Esterase-catalysed Aldol Reaction and Knoevenagel Reaction

JIANG Ling, YU Hongwei

2014, 30(2): 289-292. doi:10.1007/s40242-014-3401-y

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Esterase BioH, which is obligatory for biotin synthesis in Escherichia coli, was found to exhibit a promiscuous ability to catalyse Aldol and Knoevenagel reactions with moderate to good yields. The reaction conditions including organic solvent, molar ratio of ketone to aldehyde, enzyme amount, and reaction time were investigated to evaluate the effect of different reaction conditions on yield. Target compounds were afforded in the best yield of 91.2% for Aldol reaction and 54.7% for Knoevenagel reaction. In addition, because the enzyme could be prepared with a low cost, this protocol could provide an economic route to conduct Aldol and Knoevenagel reactions, which expand the field of enzymatic promiscuity.

Electrochemical Reduction of Nitrobenzene in Ionic Liquid BMImAc

ZHANG Yinxu, MAO Xinbiao, REN Shuying, MA Chunan

2014, 30(2): 293-296. doi:10.1007/s40242-014-3398-2

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Ionic liquid, 1-butyl-3-methylimidazolium acetate(BMImAc), was used in the electrochemical reduction of nitrobenzene. The electro-reduction of nitrobenzene on platinum electrode was studied by cyclic voltammetry(CV), in situ Fourier transform infrared(FTIR) spectroscopy and constant-potential electrolysis. The experimental results show that electrochemical reduction process of nitrobenzene was controlled by diffusion, the main reduction product was azobenzen at -1.45 V, and the influences of scan rate and temperature on the electrochemical behaviors were obviously. A reduction mechanism of nitrobenzene in an ionic liquid was a probable ‘nitrobenzene→nitroso-benzene→azobenzene→aniline’ main reductive reaction route.

Pharmacophore and Docking-based 3D-QSAR Studies on HIV-1 Integrase Inhibitors

ZHANG Xiaoyi, DENG Dongjie, TAN Jianjun, HE Yu, LI Chunhua, WANG Cunxin

2014, 30(2): 297-305. doi:10.1007/s40242-014-3395-5

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Integrase(IN) plays an essential role in the process of HIV-1 replication. IN inhibitors of diketo acid derivatives(DKAs) were analysed by the Comparative Molecular Field Analysis(CoMFA) and Comparative Molecular Similarity Induces Analysis(CoMSIA) methods. A set of 42 compounds were randomly selected as the training set(35) and test set(7). Firstly, a good pharmacophore(goodness of hit=0.787) was obtained and used to align ligands. Then, predictive models were constructed with the CoMFA and CoMSIA methods based on the pharmacophore alignment. As a result, the CoMSIA method yielded the best model with an r² of 0.955 and a q² of 0.665, which can predict the activities of the tested DKAs very well(r²=0.559). Finally, DKAs were docked into IN, and the predicit modes were superimposed on the contour maps obtained from the best CoMSIA model. The superimposed maps gave a visualized and meaningful insight into the inhibitory behaviors, providing significantly useful information for the rational drug design of anti-IN agents.

Synthesis of Flower-like Manganese Wad and Its Decolorization Performance for Azo Dye Congo Red

YANG Aili, WEI Bingqing, ZHANG Zhengjun

2014, 30(2): 306-309. doi:10.1007/s40242-014-3384-8

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Flower-like manganese wad(MW) with high activity was synthesized via ultrasonic-assisted redox reaction of sole manganese salt MnO₄^-. MW was characterized by X-ray diffraction(XRD), scanning electron micros-copy(SEM) and X-ray photoelectron spectroscopy(XPS). The experimental results indicate that the maximum decolorization rate of Congo red(CR) reached above 95% within 15 min in a wide pH range from 2.0 to 6.0. Results also show that MW has excellent decolorization performance for azo dye CR which implies potential application for removing dye pollutants from industrial effluents.

Ruthenium Complex Immobilized on Mesoporous Silica as Recyclable Heterogeneous Catalyst for Visible Light Photocatalysis

HE Hongyan, LI Wenliang, XIE Zhigang, JING Xiabin, HUANG Yubin

2014, 30(2): 310-314. doi:10.1007/s40242-014-3367-9

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Aldehyde group-functionalized [Ru(bpy)₂L](PF₆)₂ catalyst was prepared and immobilized onto the mesoporous silica nanoparticles to act as a heterogeneous catalyst for the selective oxidation of thioanisole to methyl phenyl sulfoxide under visible light. The heterogeneous catalyst can be easily recovered by simple centrifugation without chemical treatment, exhibiting comparable catalytic efficiency with homogeneous ones and no decrease in catalytic efficiency after at least 5 cycles.

Simple and Effective Method to Prepare Microfiber Reinforced Nanofiber Film with Significant Improvement of Mechanical Properties

SONG Yan, ZHANG Chaoqun, YANG Qingbiao, LI Yaoxian

2014, 30(2): 315-319. doi:10.1007/s40242-014-3504-5

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Microfiber reinforced nanofiber films were prepared with the help of two nozzles technology. We designed a new device via placing two nozzles on the opposite sides of a rolling cylinder, with a piece of thin insulation board with a certain size of hole in the middle part installed to accommodate the cylinder so as to form two entirely independent electric fields. Playing the role of support, microfiber may be favorable for enhancing the mechanic performance of the nanofiber. Compared with that of single nanofiber, the tensile strength of the composite micro/nanofiber prepared by this method has been increased by a factor of 4.5. After the further improvement of the fiber orientation, the tensile strength is 7.96 times that of non-oriented composite micro/nanofibers film, 30 times that of the single nanofiber film.

Sonochemical Synthesis of Three-dimensional Aggregates of Pd Nanoparticles with High Electrocatalytic Activity Towards Ethanol Oxidation

WANG Yanli, TAN Dexin

2014, 30(2): 320-325. doi:10.1007/s40242-014-3362-1

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Flower-like aggregates composed of (4.0±0.8) nm palladium(Pd) nanoparticles were prepared via ultrasonics in the palladium(Ⅱ) chloride(PdCl₂) H₂O/EtOH(5/1, volume ratio) solution with the addition of a quantity of poly(vinyl pyrrolidone)(PVP) and sodium dodecyl sulfonate(SDS). The morphologies, crystal structures and the optical properties of the flower-like Pd nanostructures were characterized by X-ray diffraction(XRD), X-ray photo-electron spectroscopy(XPS), scanning electron microscopy(SEM), transmission electron microscopy(TEM), selected area electron diffraction(SAED) and UV-visible absorption spectroscopy, respectively. The mechanism of sonoche-mical reduction of Pd(Ⅱ) ions was also investigated. The results show that the molar ratio of PVP to SDS affected the formation of the flower-like aggregates of Pd nanoparticles. Moreover, the electrocatalytic properties of Pd aggregates modified glassy carbon electrode for ethanol oxidation were also investigated by cyclic voltammetry(CV). This material exhibits remarkable electrocatalytic activity for ethanol oxidation in 1 mol/L KOH and appears as a promi-sing candidate to be applied in direct ethanol fuel cells.

Preparation and Investigation of Arsenic Trioxide-loaded Polylactic Acid/Magnetic Hybrid Nanoparticles

SONG Xiaoli, YOU Juan, WANG Juan, ZHU Aiping, JI Lijun, GUO Rong

2014, 30(2): 326-332. doi:10.1007/s40242-014-3306-9

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In order to improve the therapeutic index and reduce the side effects of As₂O₃ so as to expand its clinical utility to solid tumors, As₂O₃-loaded polylactic acid(PLA)/magnetic nanoparticles(PAMNs) were prepared and the preparation conditions were optimized by the improved double emulsion solvent-evaporation method to obtain as a drug delivery system with a high As₂O₃ encapsulation efficiency and homogeneous nanosized particles. Successful loading of magnetic nanoparticles into the nanoparticles was confirmed by Fourier transform infrared(FTIR) spectroscopy. The drug loading, encapsulation efficiency and releasing properties of As₂O₃ in PAMNs were investigated by atomic fluorescence spectrometer analysis. Subsequently, the in vitro antitumor efficacy of free As₂O₃and As₂O₃-PAMNs against SMMC-7721 cell line was investigated. Finally, confocal fluorescence microscopy was conducted to reveal the celluar uptake of As₂O₃-loaded PAMNs by SMMC-7721 cell line.

Synthesis, Characterization and Application of Methyl 3,5-Disulfo-benzoate Dipotassium Dihydrate as Nucleating Agent for Poly(L-lactide)

SUN Zhiqiang, ZHANG Han, PANG Xuan, BIAN Xinchao, CHEN Wenqi, CHEN Xuesi

2014, 30(2): 333-338. doi:10.1007/s40242-013-3275-4

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A newly synthesized aromatic sulfonate compound, complex 2 with formula of K₂[H₃COOC-C₆H₃(SO₃)₂]·2H₂O(methyl 3,5-disulfo-benzoate dipotassium dihydrate) was synthesized and characterized by elemental analysis, infrared(IR) spectrometry, nuclear magnetic resonance(NMR) and crystal structure measurement. Single-crystal X-ray diffraction(XRD) revealed that complex 2 crystallized in the triclinic system with space group P1. Complex 2 was used as nucleating agent for poly(L-lactide)(PLLA). The crystallization of PLLA with powder of complex 2 was investigated by means of differential scanning calorimetry(DSC) and polarized optical microscopy (POM). The results prove that complex 2 was effective as nucleating agent for PLLA. It could accelerate crystallization by reducing the induction time and increasing the density of nuclei in the crystallization process. The half-time of crystallization(t_0.5) for pure PLLA wasabout 8 times longer than that of PLLA sample with 1.0%(mass fraction) of complex 2.

Grafting of Poly(lauryl acrylate) onto Nano-silica by ‘Click Chemistry’

CHEN Kailing, ZHAO Yunhui, YUAN Xiaoyan

2014, 30(2): 339-342. doi:10.1007/s40242-013-3274-5

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Poly(n-alkyl acrylate) with long side groups, namely, poly(lauryl acrylate)(PLA) was synthesized by reversible addition-fragmentation chain transfer(RAFT) polymerization, and the trithioester terminal groups were converted to thiol by reducing reaction. Grafting of the obtained polymer onto nano-silica modified with 3-(methacryloxy)propyl-trimethoxysilane(SiO₂-MPS) was conducted by thiol-ene ‘click chemistry’. PLA was characterized by proton nuclear magnetic resonance(¹H NMR) and gel permeation chromatography(GPC). Fourier transform infrared(FTIR) spectrometry and thermogravimetric analysis(TGA) were used to demonstrate the grafting reaction, and the grafted hairy nano-silica(SiO₂-g-PLA) was viewed under a transmission electron microscope(TEM). According to TGA, grafting ratio and grafting density of SiO₂-g-PLA are 30.27% and 0.013 chain/nm², respectively. The static water contact angle of SiO₂-g-PLA is (80.10±2.97)°, which ensures its hydrophobicity. Dispersion experiment was carried out to confirm its dispersibility in mixed solvents, indicating its potential application in coatings or composites.

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