• Volume 33,Issue 5,2016 Table of Contents
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    • >Review and monographs
    • Trends and Challenges of Development of Food Flavors

      2016, 33(5).

      Abstract (455) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:Food flavors are one category of food additives, which account for a quarter of the worldwide market for food additives. The development of food flavors has been influenced by many factors in recent years. These factors can be divided into two classes: technological factors and social factors. The former includes techniques of separation and extraction, techniques of equipment analysis and biotechnology, the latter includes psychological requirements of consumers and requirements for sustainable development. Affected by these factors, sulfur-containing flavors have developed to be one impact category of food flavors, which are featured by active chemical reactivity, low contents in food, low threshold values and distinctive characters, and the market of natural flavors is growing steadily. The status of the development of these two classes of flavors has been introduced and analyzed briefly.

    • >Functional materials
    • Preparation and Drug Release Properties of the Self-crosslinked Conjugated Linoleic Acid Ufasomes by Thermal Polymerization

      2016, 33(5).

      Abstract (913) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Polymerizable monomer conjugated linoleic acid (CLA) and its ionized species (soap) were employed as raw materials to construct CLA-Ufasomes through pH-induced self-assembling in aqueous solution. Subsequently, CLA-Ufasomes self-assembled at high concentration were chemically tethered by intra-ufasomal self-crosslinking of conjugated double bonds in the CLA molecules through thermal polymerization to obtain the stable CLA-FAV. The morphologies and size distribution were characterized by transmission electron microscopy (TEM) and dynamic light scattering (DLS). The experimental results indicated that the morphology of the CLA-FAV prepared through thermal polymerization was consistent with that of the CLA-FAV obtained by UV irradiation at pH 8.6. Moreover, the CLA-FAV with diameter of 10-20 nm were always obtained in a wide concentration range of 3-100 mmol?L-1 (500 times of critical vesicular concentration of CLA). Finally, the in vitro release results of 5-fluorouracil (5-FU) showed that the CLA-FAV self-crosslinked through thermal polymerization possessed a good effect on encapsulation and release of 5-FU.

    • Synthesis and Properties of Novel UV-curable Antistatic Materials

      2016, 33(5).

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      Abstract:A series of antistatic quaternary ammonium salts with single or multiple UV-curable functional group were synthesized by DMAEMA .The UV-curable antistatic coating was obtained by combining UV-curable coatings technology with antistatic technology. Curing time, washability and thermal stability of the UV-curable films were studied.The influences of kinds and concentration of the antistatic agent on the antistatic properties were discussed.The results showed that the surface resistivity of coating film decreased to 107Ω and hardly changed after washed 10 times, and the UV-curable coating could be cured quickly to give a film with excellent antistatic properties and washability .The results of the TG test showed that the antistatic UV curing coating has good thermal stability.

    • NIR sensitive hyperthermia antitumor of cysteine modified gold nanorods via Infrared thermal imaging method

      2016, 33(5).

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      Abstract:Cys-AuNRs were prepared via ligands exchange method using zwitterionic cysteine to modify AuNRs for the clinical photothermal therapy. And the photothermal effect, the infrared thermal imaging, hyperthermia effect on tumor cells and fluorescence imaging experiment of Cys-AuNRs were investigated under irradiation by an 808 nm NIR laser at a power density of 200mW∙cm-2. The survival rate of HeLa cells incubated with Cys-AuNRs at the concentration of 57 μg/mL, still remains 90.1%. However, under NIR irradiation for10 min , the survival rate of Hela cells sharply decreases to 60.1%. The results suggest that Cys-AuNRs have good biocompatibility and low cytotoxicity, can also kill tumor cells effectively under the laser radiation. Therefore, the modification of AuNRs with biocompatible cysteine has an important practical significance in the clinical noninvasive hyperthermia treatment.

    • Adsorption Performance of Methylene Blue Dye by LS-g-P AA / AMPS /APT Resin

      2016, 33(5).

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      Abstract:Novel lignosulfonate sodium graft 2-acrylamido-2-methylpropanesulfonicacid and acrylic acid and attapulgite (LS-g-P AA / AMPS /APT) biomass resin adsorption was synthesized by grafting polymerization using microwave irradiation.The chemical micstructure of resin was determined by means of FTIR and XRD .The effects of adsorbent dosage,the solution pH, concentration of the dye and the adsorption time and temperature on adsorption process for methylene blue (MB) were studied. The results shows that under the conditions of adsorbent dosage of 0.1g,the dye concentration of 500mg/L and the volume of 200mL,the adsorption capacity and removal was found to be 968 mg/g and 96%, respectively. The resin has strong pH sensitivity and high adsorption capacity.The equilibrium data were fitted to the Freundlich isotherm. The adsorption process of MB onto resin can be described with the pseudo-second-order kinetic model,indicating that the adsorption process is mainly endothermic chemisorption.

    • >Leather chemicals
    • One-step Synthesis of Carboxyl Epoxy Resin/nano ZrO2 nanocomposites and their applications

      2016, 33(5).

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      Abstract:Abstract: The carboxyl epoxy resin/nano ZrO2 nanocomposites were prepared by free radical copolymerization with the nano ZrO2 nanoparticles modified by Triethoxyvinylsilane(A-151), vinyl methyl ether and methyl acrylic acid. The modified nano ZrO2 nanoparticles and the carboxyl epoxy resin/nano ZrO2 nanocomposites were characterized by fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The results show that the surface of the modified nano ZrO2 Nanoparticles was covered by the carbon-carbon double bonds. TEM results show that the nano ZrO2 nanoparticles were evenly dispersed in the polymer matrix and its surface generate layer by reaction of vinyl methyl ether and methyl acrylic acid. The carboxyl epoxy resin/nano ZrO2 nanocomposites were applied in leather tanning process. The application results show that the shrinkage temperature, thickening and softness of leather tanned by the carboxyl epoxy resin/nano ZrO2 nanocomposites with 3% chromium powder significantly improve compared with these of leather tanned by chrome and the content of Cr2O3 in tanning waste water effectively reduce.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Performance Evaluation of the Copolymer-PAAND Used as Fluid Loss Additive in Drilling Fluid

      2016, 33(5).

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      Abstract:The copolymer, which was used as fluid loss additive for drilling fluid was synthesized by free radical polymerization in aqueous solution, using N-Vinyl-2-pyrrolidon (NVP), Dimethyl- aminoethyl acrylate methylchloride (DAC), 2-Acrylamide-2-methylpropanesulfonic acid (AMPS) and acrylamide (AM) as monomers, ammonium persulfate and sodium sulfite as initiators. The synthetic conditions with optimal property were achieved by the orthogonal experiment, and the structure of copolymer was characterized by FT-IR. The results of performance evaluation showed that the synthesized copolymer had excellent temperature resistance, good heat resistance as well as salt tolerance. When the mass fraction of copolymer was 1.5%, the API filtrate volume (0.7 MPa, 30 min) of fresh water drilling fluid, saline water drilling fluid, saturated-brine drilling fluid and composite-brine drilling fluid were 5.6 mL,9.7 mL,19.0 mL and 16.1 mL. Compared with frequently-used fluid loss additives of SP-8,JT888,MAN104 and HJ-3 in Xijiang oil field, the synthesized copolymer showed the better property in controlling the fluid loss of drilling fluid system. The evaluation of field application demonstrated that the fluid loss additive had good site suitability with potassium calcium based sulphonated polymer drilling and completion fluid system, MMH drilling and completion fluid system, and sulphonated polymer drilling and completion fluid system in Xinjiang oil-field.

    • >Special dyes and pigments
    • Research on Synthesis and Spectral Properties of Water-Soluble Indocyanine Dye and Its Application

      2016, 33(5).

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      Abstract:3 novel water-soluble indocyanine dyes (em. 690 nm) were designed, synthesized and characterized by nuclear magnetic resonance (NMR) for fluorescent labeling of biomolecules. Spectral properties of the prepared dyes in different solvents were tested. In order to investigate the application of fluorescent dyes in the field of biomedical analysis, the absorption and emission spectra of the dyes in the surfactants as CTAB, SDS were measured, the photostability of dyes were measured by cyclic voltammetry (CV). The application of the new dyes in cellular imaging has been demonstrated through direct conjugating of the dyes with living renal carcinoma cells, then imaging was visualized by near-infrared fluorescence microscopy. The molar extinction coefficient and the fluorescence quantum yield of the dyes were calculated.

    • >Surfactants
    • Preparation and Properties of a series of m-3(OH)-m Type Surfactant

      2016, 33(5).

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      Abstract:Under conditions of hydrochloric acid aqueous solution,long-chain alkyl dimethyl tertiary amine, epichlorohydrin as the main raw material,synthesised a series of 1,3-bis (alkyl dimethyl ammonium chloride) isopropanol Gemini quaternary ammonium salt , m-3(OH)-m ,(m= C8、C10、C12、C14、C16、C18)with one-pot method. Melting point as a method for the study to detect the purity of Gemini quaternary ammonium salt m-3(OH)-m. In C12-3(OH)- C12 case, FT-IR and 1HNMR are adopted to structural characterization. Surface tension was measured at various concentrations,foaming ability and emulsifying ability were measured in 0.1% aqueous solution. The results shows:With the change of m, surfactant, foaming power and emulsifying capacity shows a regular change for each compound. The CMC and γcmc of each compound respectively were 0.09、0.075、0.03、0.024、0.026、0.14 mML-1 and 54.01、32.56、25.74、29.41、30.51、30.28 mNm-1 in the order of m=C8、C10、C12、C14、C16、C18. Foaming capacity and foaming stability showed better results at m=C10 and m=C12. Emulsifying capacity revled the better result at m= C14.

    • Synthesis and Surface Activity of Cationic Gemini Surfactant N,N’-bis(octadecyl/ tetradecyl dimethyl) -1,2-dichloro- 1,4-Benzene dimethyl ammonium salt

      2016, 33(5).

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      Abstract:Cationic Gemini surfactant was synthesized directly from 1,4-Bis -(chloromethyl)-benzene, N,N-dimethyldodecylamine and N,N-Dimethyltetradecyl -amine. In order to obtain optimal reaction conditions, orthogonal experiment was conducted. The optimal reaction condition was performed with the molar ratio of amine and XDC 2.2:1 at 75℃ for 3 h. The chemical structure of the purified product was confirmed by FT-IR, 1HNMR and 13CNMR. The aqueous solution surface activity properties were studied and the results showed that the surface tension (γCMC) are 40.71 and 35.37 mN?m-1, critical micellar concentration (CMC) are 1.36?0-5 and 2.56?0-6 mol?L-1 , pC20 are 5.63 and 6.18, excess adsorption amounts(Γmax) are 2.41?0- 6 and 3.09?0- 6 mol?m-2, the saturation adsorption areas permolecule (Amin) are 0.69 and 0.54 nm2. The CMC of the Gemini surfactants are only one percent of the monomer similar as its corresponding monomer.

    • Study on the Synthesis and Application of Bifunctional Epoxy Emulsifier

      2016, 33(5):0-0.

      Abstract (1373) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:A multiblock epoxy emulsifier with bifunctional group (Hydroxyl and Carboxyl) was synthesized by a series of raw materials, including epoxy resin (E-44), trimellitic anhydride (TMA) and polyethylene glycol (PEG4000) in the presence of the catalyst boron trifluoride etherate. Then waterborne epoxy emulsion was prepared by phase inversion method with the above emulsifier. The chemical structure of emulsifier was characterized by FTIR、1HNMR and GPC. The effects of the amount of catalyst, reaction temperature and time on the esterification epoxy conversion rate in the emulsifier synthesis process were studied. Simultaneously, the effects of the amount of emulsifier and emulsifying temperature on Emulsion stability were explored. The optimum conditions of synthesis emulsifier: catalyst dosage was 0.36 % (the total reactant mass), esterification reaction time was 2 h and temperature was 70 ℃, esterification rate reached 96.6 %. Epoxy ring-opening reaction time was 5 h and temperature was 95 ℃, ethylene conversion reached 94.2 %. Moreover, the emulsion with small average particle size (about 312 nm) and good stability was obtained when emulsifiers dosage was 15 % (the mass of E-44) and temperature was 60 ℃.

    • >Building chemicals
    • Dispersity of graphene oxide in cement matrix and its impact on the structure and properties

      2016, 33(5).

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      Abstract:Copolymer (PAAS) of acrylic acid (AA), acryloyloxyethyltrimethyl ammonium chloride (AAC) and sodium allylsulfonate (SAS) was prepared by polymerization in order to solve the problem of uniformly dispersity of graphene oxide (GO) nanosheets in cement matrix. PAAS with GO nanosheets forms the PAAS/GO composites achieve the dispersive effects. The tested results indicated that the PAAS/GO composites consisted of PASS with mass fraction of 2% and GO with mass farction of 0.01%, 0.02% and 0.03%, respectively, can regulate the cement matrix to from regulation and order microstructure gathered by flower-like, polyhedron-like and needle-like crystals, respectively. The flexural strength of corresponding to cement materials have an increase of 63.0%, 90.4% and 87.9% at 28 d, respectively, and the corresponding tensile strength have an increase of 32.6%, 74.2% and 71.3%, respectively. These cement hydration crystals usually easily growed in cracks and holes of cement matrix and had repairing function for the cracks and holes. PASS forming the composites with GO nanosheets achieve uniformly dispersion GO nanosheets in cement matrix and effective control the microstructure and properties.

    • >Fine chemical intermediates
    • Microwave-assisted Iodine Catalyzed Deoximations in Water

      2016, 33(5).

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      Abstract:The deoximation of oximes into their corresponding carbonyl compounds is one of the most important processes in organic synthesis. There has been increasing interest in the development of methods for deoximation. Herein, twelve aldehydes and ketones were synthesized in 68%~92% yields by deoximations of oximes catalyzed with iodine in green solvent water under microwave-assisted condition. The structures of all products were confirmed by the corresponding nuclear magnetic resonance spectrum (1H NMR) and mass spectrum (MS). The effects of solvent, the amount of iodine, microwave power and reaction temperature on the reaction were considered. The optimized reaction conditions: oximes, iodine (50 mol%), and water (1 mol/L), microwave power 300 W, reaction temperature 85 ℃, reaction time 35 min. A possible mechanism was proposed on the results of the experiments.

    • >Biological engineering
    • Preparation of β-glucosidase from bitter almond by three-phase partitioning

      2016, 33(5).

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      Abstract:Three-phase partitioning used salt and an organic solvent to precipitate enzymes or proteins from complex mixtures. Three-phase partitioning was applied to prepare β-glucosidase from bitter almond crude extract. In order to enhance the purification fold degree and activity recovery of β-glucosidase, the study discussed the influence of organic solvents, organic solvent concentration, ammonium sulfate concentration, pH values and temperature on the parameters of β-glucosidase partitioning process. The results were shown below: t-butanol was the best organic solvent, the ratio of crude extract and t-butanol was 1.0:1.5 (v/v), ammonium sulfate saturation was 50% (w/v), the system of pH value was 5.0 and the optimum temperature was 25℃. Under the optimized conditions, the β-glucosidase was purified to 5.97-fold with 85.7% activity recovery. The SDS-PAGE of the enzyme analyzed that comparatively purification and protein molecular weight of the enzyme was found to be about 60.0 kDa. This study showed that three-phase partitioning is a simple, quick and economical method, which was applied to β-glucosidase separation and purification.

    • >Modernization technology of traditional Chinese medicines
    • A New Kind of Amino Acid Descriptor for ACE Inhibition QSAR study

      2016, 33(5).

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      Abstract:A new descriptor of amino acids-SVREW was derived from principal components analysis of the matrix of 47 walk and path counts descriptors, 44 eigenvalue-based indices descriptors and 41 randic molecular profiles descriptors of amino acids. The structure of ACE Inhibition Peptides was characterized with SVREW, using multiple linear regression (MLR) to establish a quantitative structure-activity relationship, at the same time, adopt the method of internal and external double verify the stability of the model. The relevant statistical parameters as follows: the correlation coefficient (Rcum2), leava-one-out(LOO) cross-validation correlation coefficient (Rcv2) and external validation correlation coefficient (Qext2) were 0.907, 0.791, 0.633 for dipeptides model; 0.831, 0.603, 0.723 for tripeptides model; 0.834,0.668,0.718 for tripeptides model 0.964, 0.853, 0.948 for nonapeptides model; Studies show that the MLR models constructed by SVREW descriptor had good fitting and predictive abilities,to become an effective structure characterization methods in peptide drugs QSAR study and provide guidance for new drug discovery and research.

    • >Catalysis,separation and purification technology
    • Synthesis and Catalytic Properities of Molybdenum Acid Peroxide Ionic Liquid

      2016, 33(5).

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      Abstract:3-octyl-1-methyimidazole molybdenum acid peroxide ionic liquid [C8MIM]2[MO2O11] was synthesized with N-methylimidazole, n-octyl chloride, sodium molybdate and hydrogen peroxide as raw materials, and the product was characterized by 1H, 13C, FTIR and elemental analysis. The catalytic oxidation properties of the functionalized ionic liquid for dibenzothiophene were examined. The optimum experiment conditions (the volume of the model gas oil was 5 times of extraction agent, the mole ratio of oxygen to sulfur was 6:1, the dosage of catalyst was 5g per liter of model gas oil, the reaction temperature was 40 oC and reaction time was 30 min) of extraction coupled catalytic oxidation desulfurization were determined through the single factor analysis. The initial sulfur content (500 μg/mL) of the dibenzothiophene/ isooctane model gas oil dropped below 10 μg/mL, and the desulfurization rate was as high as 98.83% at the optimum condition. The system recycling performance was further investigated and the result showed the desulfurization rate was about 98.4% after 16 times repeated uses.

    • Preparation and Catalytic Properties of La2O3/AAO Nanoarrays by Sol-gel Method

      2016, 33(5).

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      Abstract:La2O3/AAO nanoarrays catalysts were controllable prepared with anodic aluminum oxide (AAO) template by sol-gel method, and catalytic activity of the catalyst was tested using aldol condensation of acetone to diacetone alcohol as a probe reaction. The catalysts were characterized by XRD, SEM, TEM, BET and CO2-TPD. The results showed that La2O3 were highly and homogeneously dispersed on the AAO surface. When the calcination temperature was 900 ℃, calcination time was 1 hour and the reaction time was 3 h, La2O3/AAO-900 catalyst showed the highest catalytic activity which the conversion of acetone was 4.01 % and the selectivity to diacetone alcohol was 96.32 %. The activity and selectivity of La2O3/AAO-900 catalyst remain basically unchanged after five runs. The higher catalytic performance of La2O3/AAO-900 catalyst is attributed to its larger specific surface area, weak basic sits and a large basic amounts.

    • Methanol Decomposition on CuZnAl Catalysts with MgO Modified

      2016, 33(5).

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      Abstract:MgO modified CuZnAl catalysts were prepared by coprecipitation method. The structure and physic-chemistry properties were characterized by BET, XRD, SEM, H2-TPR and CO2-TPD. The catalytic performance of MgO modified CuZnAl catalysts for methanol decomposition to hydrogen was evaluated in a fixed-bed reactor. The results showed that the addition of MgO to CuZnAl catalysts increased BET surface area of the catalysts and CuO dispersity, modified the redox property of catalysts and enhanced the catalytic activity and selectivity. The optimization catalyst was achieved as CuZnAlMg2, with mass ration of m(CuO):m(ZnO):m(Al2O3):m(MgO) = 16:13:3:2. The conversion of methanol decomposition was 99.1% and the gas recovery were 97.0% over CuZnAlMg2 under the reaction condition of reaction temperature 280℃, reaction pressure 1.0 MPa and LHSV 0.6h-1. The analysis to liquid products of methanol decomposition showed the adding suitable amount of MgO improved the alkalinity of catalysts, effectively inhibited liquid by-products and increased the gas yield.

    • >Drug and cosmetic materials
    • Functionalized Bronsted-Lewis acidic ionic liquid as an efficient catalyst for synthesis of 1-amidoalkyl-2-naphthols

      2016, 33(5).

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      Abstract:A Brϕnsted-Lewis acidic ionic liquid,[CH2COOHmim]FeCl3Br was synthesized.This ionic liquid exhibited high catalytic performance in the synthesis of 1-amidoalkyl-2-naphthols through one-pot three-component condensation reaction of 2-naphthol, aldehydes and acetamide at 100 ℃ under solvent-free conditions.The product confirmed by IR,1H-NMR and 13C-NMR spectra.The experimental results demonstrate that this method is environmentally friendly,simple,highly-yielding.Furthermore,the catalyst can be recycled and reused several times without obvious significant loss of activity.

    • Synthesis and Antitumor Activity of Amino Acid Derivatives Containing Phosphonate backbones

      2016, 33(5):0-0.

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      Abstract:In search of more effective anticancer agents, according to the combination principle, 9 phosphonate derivatives were designed and synthesized. Their structures were clearly established by elemental analysis, IR, 1HNMR and 13CNMR, and their antiproliferative activities were evaluated against some tumor cell lines by using a methylthiazolyldiphenyl- tetrazolium bromide (MTT) method. Preliminary results in bioactivity tests indicated that they exhibited certain antitumor activities. Among the active compounds, compounds Ⅲf, Ⅲi had better inhibition effect on cells growth, espectively, compounds Ⅲi showed remarkable activities against A-549, SGC-7901 and EC-109 with IC50 values of 7.0±0.8, 6.9±0.8 and 7.3±0.7 μmol/L respectively, similar to cisplatin, which were worth further investigation.