Formation of the Inclusion Complex of Orange II with β-Cyclodextrin and Its Photostability

Inclusion complex of Orange II with β-Cyclodextrin (β-CD) and the anti-photolysis effect under UV-light were investigated. The molar ratio of inclusion complex of β-Cyclodextrin and Orange Ⅱ is 1∶1. The formation constant K=1.236×103 L/mol was determined by the UV and Fluorescence spectra respectively, which was quite in accordance with the calculation with a modified Benesi-Hildbrand equation. The inclusion complex was characterized by the IR spectra and the molar ratio of inclusion complex is 1∶1 too. The formation constant K=1.266×103 L/mol was determined by 1 H NMR analysis and was nearly the same by UV and fluorescence spectra. The photocatalytic decolorization rate of Orange Ⅱ solutions containing β-CD and TiO2 was smaller by 51.9% than that of the Orange Ⅱ solutions only containing TiO2, while in the case of direct photolysis of Orange Ⅱ solutions, β-CD can lower the photolysis rate by 48.1% under UV-light. This result indicates β-CD can inhibit the photolysis and photocatalytic decolorization of Orange Ⅱ under UV-light. The β-CD inclusion complex was found to be persistent to UV-light photolysis.     

Preparation,Characterization and Antioxidant Activity of Inclusion Complex of Bakuchiol with Hydroxypropyl-β-cyclodextrin

Bakuchiol isolated from Psoralea corylifolia is a naturally occurring prenylated phenolic monoterpene with a variety of bioactivities. The aim of this study was to improve the water solubility and thermal stability of bakuchiol through complexing it with hydroxypropyl-β-cyclodextrin(HP-β-CD). The bakuchiol/HP-β-CD inclusion complex's behavior and characterization were investigated by ultraviolet-visible(UV-vis) spectroscopy, Fourier transform infrared spectroscopy(FT-IR), thermogravimetric analysis(TGA),X-ray diffraction(XRD),~1H nuclear magnetic resonance(NMR), and two-dimensional(2 D) NMR. The obtained results indicated the formation of 1∶1 inclusion complex for bakuchiol with HP-β-CD. Water solubility of bakuchiol was significantly improved by complexation with HP-β-CD as demonstrated by phase solubility studies. The encapsulation of bakuchiol was confirmed by UV-vis, FT-IR, and XRD. The thermal stability was effectively enhanced by TGA and derivative thermogravimetry(DTG) analysis. In vitro antioxidant activity showed that bakuchiol/HP-β-CD inclusion complex had a little higher antioxidant ability than free bakuchiol. Moreover, we got the possible inclusion mode for the bakuchiol/HP-β-CD inclusion complex through NMR analysis. These results suggest that the inclusion complex can be a potentially useful approach in the design of novel formulations of bakuchiol for medical applications.     

In Vitro Cytotoxicity and Protein Drug Release Properties of Chitosan/Heparin Microspheres

Chitosan/heparin microspheres were prepared using the water-in-oil emulsification solvent evapo- ration technique. The microsphere diameters were controlled by selecting the fabrication process parame- ters. Scanning electron micrographs showed that the chitosan/heparin microspheres were regular and the surface morphology was smooth. Fourier transform infrared showed that the chitosan amino groups reacted with heparin carboxylic groups to form acylamides in the microspheres. Analysis of the microsphere cytotox- icity showed that they had no cytotoxic effect and behaved very similar to the negative control (polystyrene). To analyze the protein drug release profiles of the microspheres, bovine serum albumin was loaded as a model drug into the microspheres and released in vitro. Marked retardation was observed in the BSA re- lease profiles. The results show that chitosan/heparin microspheres may provide a useful controlled release protein drug system for used in pharmaceutics.     

Preparation and chiral recognition of new chiral stationary phases derived from cellulose microspheres

A new way to prepare cellulose-type chiral stationary phases (CSPs) has been established in the present work.Cellulose microspheres with a volume-average diameter of 11.5 m were prepared by an emulsion-solidification method.Three new CSPs were obtained by crosslinking the cellulose microspheres with terephthaloyl chloride (TPC),and then modifying the crosslinked microspheres with 4-methylbenzoyl chloride,3,5-dimethylbenzoyl chloride and 3,5-dichlorobenzoyl chloride,respectively.The microspheres and the CSPs were characterized by FT-IR,element analysis and scanning electronic microscopy (SEM).The chiral recognition ability of the CSPs was evaluated with high-performance liquid chromatography (HPLC).The chromatographic results demonstrate that the CSP prepared from 3,5-dichlorobenzoyl chloride possesses better chiral recognition ability compared with two other CSPs.     

In Vitro Cytotoxicity and Protein Drug Release Properties of Chitosan/Heparin Mlcrospheres

Chitosan/heparin microspheres were prepared using the water-in-oil emulsification solvent evaporation technique. The microsphere diameters were controlled by selecting the fabrication process parameters. Scanning electron micrographs showed that the chitosan/heparin microspheres were regular and the surface morphology was smooth. Fourier transform infrared showed that the chitosan amino groups reacted with heparin carboxylic groups to form acylamides in the microspheres. Analysis of the microsphere cytotoxicity showed that they had no cytotoxic effect and behaved very similar to the negative control （polystyrene）. To analyze the protein drug release profiles of the microspheres, bovine serum albumin was loaded as a model drug into the microspheres and released in vitro. Marked retardation was observed in the BSA release profiles. The results show that chitosan/heparin microspheres may provide a useful controlled release protein drug system for used in pharmaceutics.     

Effects of heat treatment on magnetic properties of Co–Fe-plated hollow ceramic microspheres

Functional hollow ceramic microspheres plated with Co-Fe were obtained through electroless plating technique for the application of lightweight microwave absorbers.They were treated at different temperatures by vacuum annealing method.The surface-coated hollow microspheres were characterized by scanning electron microscopy(SEM) and X-ray diffraction analysis (XRD).The microwave electromagnetic loss and absorbing properties of hollow microspheres plated with Co-Fe were tested by network vector analysis.Th...     

Research of Inclusion Complexation of 4,4'-Thiodiphenol Effected by β-Cyclodextrin in Aqueous Solutions and the Effect on Photodegradation

The inclusion behavior of 4,4′ -Thiodiphenol (TDP),a typical bisphenol and endocrine disruptor,reacts with β-cyclodextrin (β-CD) in aqueous solutions has been investigated by means of UV absorption spectrum and quantum-chemical calculation with Gaussian 98 software. The results show that the inclusion behavior of TDP is quite different in acidic solutions (pH 5.9) from that in alkaline solutions (pH 10.0). This behavior difference is attributed to the different formula structures in aqueous solutions at acidic and alkaline pH values that are demonstrated by quantumchemical modeling and calculation. TDP forms a 1∶1 β-CD inclusion complex in aqueous solutions. The equilibrium constant K was calculated to be 553.49 L/mol at pH 5.9 and 1 318.20 L/mol at pH 10.0 respectively for the inclusion complex reaction by using the modified Benesi-Heldbrand equation. After inclusion TDP's structure is changed especially at the inclusion part with the bond order becoming larger,which results in inhibitive photodegradation during direct photooxidation and H2O2 assisted photooxidation.     

Fiber-Based Chitosan Tubular Scaffolds for Soft Tissue Engineering： Fabrication and in Vitro Evaluation

Porous, two-ply tubular chitosan conduits for guided tissue regeneration were fabricated by combining the textile technique （inner layer） with the thermally induced phase separation process （outer layer）. A hollow chitosan tube was prepared using an industrial warp knitting process with chitosan yarns. Then, an appropriate diameter mandrel was inserted into the pre-fabricated tube. The tube and the mandrel were dipped into the chitosan solution together, taken out, and freeze-dried. After being neutralized in alkaline solution and dried at room temperature, the mandrel was removed to create the chitosan tubular scaffold. Scanning electron micrographs show that the resulting tubes have a biphasic wall structure, with a fibrous inner layer and a semipermeable outer layer. The swelling properties and the mechanical strength before and after in vitro degradation were investigated. The biocompatibility of the scaffolds was also investigated by co-culturing neuroblastoma cells （N2A, mouse） with the scaffolds. The results suggest that these chitosan tubular scaffolds are useful for the regeneration of tissues requiring a tubular scaffold.     

Investigation on preparing boron nitride by nitriding pure boron at 1200–1550 1C

Boron nitride (BN) was prepared by nitriding pure boron (B) deposited on carbon substrates by chemical vapor deposition (CVD). Thermodynamic analysis of preparing BN by nitriding CVD B at 1200–1550 1C was firstly performed. And then, the effects of nitridation conditions, including temperature, nitridation atmosphere and CVD B microstructure, on the conversion of B to BN were analyzed by scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Results show that the conversion degree of B to BN firstly increased and then slightly decreased with rising temperature. The nitridation degree was controlled by mutual actions between the nitridation of B and consumption of the effective nitrogen source (NH3). The morphology of products and the reaction mechanism between B and N were influenced by nitridation temperature. At high temperatures (1400–1500 1C), BN with highly ordered microstructure was produced. On using N2–H2 as nitridation atmosphere instead of NH3–H2– N2, no BN was obtained in the studied temperature range. The microstructure and component of BN obtained in nitridation process were little affected by the microstructure of CVD B.     

CuS-poly （N-isopropylacryl-amide-co-acrylic acid） composite microspheres with patterned surface structures： preparation and characterization

N-isopropylacrylamide (NIPAM) and acrylic acid (AA) copolymer microspheres with various compositions were prepared by reverse suspension polymerization technique. The microspheres thus prepared were employed as micro-reactors for the deposition of CuS. In this way, several CuS-P(NIPAM-co-AA) composite microspheres with different surface morphologies were prepared. It was demonstrated that the surface structures of the composite microspheres can be tailored to a certain extent by varying the ratio of the two monomer units in the template (microgels) and/or the amount of CuS deposited. It is in prospect that the inherent advantages of microgel templates (the size, composition, charge nature and density, and crosslinking density could be easily controlled) would make the microgel template method extremely useful in the preparation of composite microspheres with different patterned surface structures.     

FENG Guo-dong, et al

Aim To investigate a new method for synthesis of an Immobilized-Metal Affinity Chromatography(IMAC) adsorbent with superparamagnetism(Fe3O4/SiO2-GPTMS-Asp-Co).Method The magnetic microspheres were synthesized in situ modification and the transmission electron microscope,field emission scanning electron microscopy,X-ray diffractometer,energy spectrometer and vibrating sample magnetometer were used to characterize the appearance,particle size distribution,phase composition,chemical constituents and magnetic properties of silica magnetic microspheres(MMS).Results The silica MMS prepared by reverse microemulsions exhibit a superior core-shell structure.The size distribution of the microspheres varies from between 100 nm to 200 nm and the main phase of microspheres is amorphous SiO2 and spinel Fe3O4.The microspheres retain superparamagnetism and can be used as biomaterials.Conclusion The result indicates that the IMAC adsorbent we prepared has outstanding advantages in the separation of the natural products proteins from the crude bacterial lysate,such as simple operation,high selectivity and capacity.     

Preparation of poly （methyl methacrylate）／nanometer calcium carbonate composite by in-situ emulsion polymerization

Methyl methacrylate (MMA) emulsion polymerization in the presence of nanometer calcium carbonate(nano-CaCO3) surface modified with γ-methacryloxypropyltrimethoxysilane (MPTMS) was carried out to prepare poly (methyl methacrylate) (PMMA)/nano-CaCO3 composite. The reaction between nano-CaCO3 and MPTMS, and the grafting of PMMA onto nano-CaCO3 were confirmed by infrared spectrum. The grafting ratio and grafting efficiency of PMMA on nano-CaCO3 modified with MPTMS were much higher than that on nano-CaCO3 modified with stearic acid. The grafting ratio of PMMA increased as the weight ratio between MMA and nano-CaCO3 increased, while the grafting efficiency of PMMA decreased. Transmission electron micrograph showed that nano-CaCO3 covered with PMMA was formed by in-situ emulsion polymerization.     

Preparation and Characterization of Chitosan Nanofibers Containing Silver Nanoparticles

Chitosan(CS)nanofibers containing silver nanoparticles(AgNPs)were prepared by in-situ reducing method.A water soluble carboxymethyl chitosan(CMCT)was applied for the preparation of AgNPs.The impact factor such as the concentration of CMCT,silver nitrate(AgNO_3)content,temperature and the heating time during the preparation of AgNPs were studied.The result showed that the proper value of the concentration of CMCT,AgNO_3content,temperature and the heating time were set as0.1%,20μL AgNO_3(1.7 mol/L),90°and 3 h,separately and the maximum concentration of AgNPs could be acquired.To solve the spinnability of chitosan nanofiber,a super high molecular weight polyethylene oxide(PEO)was introduced to the system,and a new mixed solvent system was prepared by adding acetic acid,dimethyl sulfoxide(DMSO)and several drops of Triton X-100TMto distilled water.CS/PEO(80/20)with the concentration of 3%was dissolved in the mixed solvent to prepare electrospinning solution for CS/PEO(80/20)nanofiber fabrication.The CS containing AgNPs electrospun solution could be prepared by replacing the distilled water to silver nanoparticle solution during the preparation of mixed solvent.Ultraviolet visible(UV-Vis)spectra and transmission electron microscope(TEM)results showed that silver nanoparticles were prepared successfully.CS membranes with and without AgNPs were acquired via a traditional electrospinning equipment.These two nanofiber membranes were characterized by scanning electron microscope(SEM)images and mechanical testing.It could be noticed from the SEM images that there was a good morphology and random distribution for the nanofibers with an average fiber diameter of 180 nm.The mechanical property results showed that the addition of AgNPs decreased the mechanical strength significantly but the mechanical strength could still support wound dressing application.     

Glycyrrhetinic acid-modified nanoparticles for drug delivery: Preparation and characterization

In this work, glycyrrhetinic acid-modified chitosan （mGA-suc-CTS） used as liver targeted carrier for drug delivery, was prepared via hemisuccinate as a bridged group. The structure of the product was confirmed by IR and NMR methods and the degree of substitution （DS） of glycyrrhetinic acid groups was estimated via elemental analysis. Nanoparticles were formed by ionic gelation methold. The drug-loading and release behavior of the nanoparticles were investigated using BSA as the model drug. The results indicated that the carrier with a highest DS of 5.19% could be got and the DS was controlled by changing reaction temperature or feed ratio. BSA could be entrapped into the nanoparticles with the drug-loading ratio of 26.3% and the encapsulation efficiency of 81.5%. A sustained release over an 11-day period was observed in pH 7.4 in vitro.     

Electrochemically functionalized graphene as an anti-corrosion reinforcement in Cu matrix composite thin films

Cu–graphene(Gr) composite thin films were prepared by electrodeposition route using in-house synthesized Gr sheets. The Gr sheets were synthesized by the electrochemical exfoliation route using 1 M HClO_4 acid as electrolyte. The Gr sheets were confirmed by X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FTIR), field-emission scanning electron microscopy(FESEM), and transmission electron microscopy(TEM). The(002) plane of Gr sheets was observed at 2θ of 25.66°. The(002) plane confirmed the crystal structure of carbon peaks. The stretching vibration of C=C bond at a wavelength of 1577 cm~(-1) and other functional groups of carboxyl and epoxide groups were observed from FTIR. TEM confirmed the transparent structure of Gr sheets. The prepared Gr sheets were used as reinforcement at concentrations of 0.1 and 0.3 g/L with a copper matrix to synthesize the Cu–Gr composite. The prepared composite thin films were characterized by XRD, SEM, and energy-dispersion spectrometry(EDS) for morphological and analytical studies. The presence of Gr sheets in Cu–Gr composite was confirmed by EDS analysis. The prepared Cu–Gr nanocomposite thin film showed higher corrosion resistance compared with pure copper thin films in 3.5 wt% NaCl, as confirmed by Tafel plots. Electrochemical impedance spectroscopy complimented the above results and showed that 0.3 g/L composite film achieved the highest film resistance.     

Preparation of molecularly imprinted microspheres by photo-grafting on supports modified with iniferter

Molecularly imprinted microspheres (MIMs) of D-mandelic acid were synthesized in this study. Chloromethylated polystyrene beads modified with iniferter were used as supports for photo-grafting of a molecularly imprinted polymer (MIP) layer. The polymers were characterized by FT-IR, elemental analysis and thermo-gravimetric analysis to testify the polymer formation and its thermal stability. Scan- ning electron micrographs (SEM) show that the MIP particles are mono-dispersed and well-spherical, with the average diameter of 4.38 μm and size distribution coefficient of 1.02. Furthermore, the MIMs were packed in a stainless steel column and evaluated as stationary phases in high performance liquid chro- matography (HPLC). The prepared MIP exhibited a considerable capability of chiral separation between template and its enantiomer. Accordingly, this kind of MIP is likely to have wide applications in chemical sensing, chromatographic analysis and solid phase extraction.     

Effect of annealing temperature on CrN microspheres synthesized by CAP technology

CrN microspheres were synthesized by using a cathodic arc plasma source system. The obtained samples were annealed in air at temperatures of 300-800 ℃ for 60 min. The influence of annealing temperature on the microstructure and surface morphology of the CrN microspheres was investigated. The CrN microspheres were characterized by means of scanning electron microscopy, transmission electron microscopy and X-ray diffraction analysis. The results show that the CrN nanoparticles arranged into leaf-like structures before annealing. With the rising of the annealing temperature, the size of CrN crystal nanoparticals became larger. When the annealing temperature exceeded the oxidation point(500 ℃), the CrN was oxidized and the leaf-like structure was broken. With further increase of the annealing temperature(700 ℃), the arrangement of CrN nanoparticles was changed from leaf-like structure to be discrete.     

Hydrothermal synthesis and photoluminescence behavior of CeO_2 nanowires with the aid of surfactant PVP

<正>Well-crystalline CeO_2 nanowires were prepared via a surfactant-assisted hydrothermal process.Reaction temperature and reaction time were changed for the determination of optimal synthesis parameters.The as-obtained products were characterized by X-ray diffraction (XRD),high-resolution transmission electron microscopy(HRTEM),and field emission scanning electron microscopy(FESEM).The results show that single crystal CeO_2 nanowires with high yield and good uniformity can be obtained hydrothermally at 180℃for 12 h with the aid of 2.0 g surfactant(polyvinyl pyrrolidone,PVP).The role of PVP was then discussed and a possible growth mechanism was proposed. Moreover,room temperature photoluminescence(PL) spectra were obtained for these CeO_2 nanowires,which are believed to be related to the abundant defects in these nanostructures.     

Structural and optical properties of Zn1−xNixTe thin films prepared by electron beam evaporation technique

Zn1-xNixTe thin films with different composition(x=0.0, 0.05, 0.10, 0.15 and 0.20) were deposited on glass substrate by electron beam evaporation technique followed by its characterization using advanced structural and optical analysis techniques. Structural properties of the prepared thin films were studied by X-ray diffraction(XRD). The XRD patterns revealed that the binary compounds transformed into a ternary compound with cubic structure having preferred orientation along the c-direction with(111) planes. Composition analysis of the films was determined by energy dispersive analysis of X-rays(EDAX) and found to be in agreement with the precursor composition. Optical properties such as extinction coefficient(k) and band gap energy of these films were examined by using a spectroscopic ellipsometer. It was found that the extinction coefficient(k) increased with the addition of Ni content in the alloy. In comparison, the band gap energy was also determined by using transmission spectra and found to be agreed with that of the ellipsometric results. These analyses confirm that the band gap energy decreases with the increase of Ni content in the alloy.