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Sample records for prepared robust cross-linked

  1. A novel strategy for preparing mechanically robust ionically cross-linked alginate hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Jejurikar, Aparna; Lawrie, Gwen; Groendahl, Lisbeth [School of Chemistry and Molecular Biosciences, University of Queensland, Brisbane, Queensland 4072 (Australia); Martin, Darren, E-mail: l.grondahl@uq.edu.au [Australian Institute for Bioengineering and Nanotechnology, University of Queensland, Brisbane, Queensland 4072 (Australia)

    2011-04-15

    The properties of alginate films modified using two cross-linker ions (Ca{sup 2+} and Ba{sup 2+}), comparing two separate cross-linking techniques (the traditional immersion (IM) method and a new strategy in a pressure-assisted diffusion (PD) method), are evaluated. This was achieved through measuring metal ion content, water uptake and film stability in an ionic solution ([Ca{sup 2+}] = 2 mM). Characterization of the internal structure and mechanical properties of hydrated films were established by cryogenic scanning electron microscopy and tensile testing, respectively. It was found that gels formed by the PD technique possessed greater stability and did not exhibit any delamination after 21 day immersion as compared to gels formed by the IM technique. The Ba{sup 2+} cross-linked gels possessed significantly higher cross-linking density as reflected in lower water content, a more dense internal structure and higher Young's modulus compared to Ca{sup 2+} cross-linked gels. For the Ca{sup 2+} cross-linked gels, a large improvement in the mechanical properties was observed in gels produced by the PD technique and this was attributed to thicker pore walls observed within the hydrogel structure. In contrast, for the Ba{sup 2+} cross-linked gels, the PD technique resulted in gels that had lower tensile strength and strain energy density and this was attributed to phase separation and larger macropores in this gel.

  2. A Robust Cross-Linking Strategy for Block Copolymer Worms Prepared via Polymerization-Induced Self-Assembly

    Science.gov (United States)

    2016-01-01

    A poly(glycerol monomethacrylate) (PGMA) chain transfer agent is chain-extended by reversible addition–fragmentation chain transfer (RAFT) statistical copolymerization of 2-hydroxypropyl methacrylate (HPMA) with glycidyl methacrylate (GlyMA) in concentrated aqueous solution via polymerization-induced self-assembly (PISA). A series of five free-standing worm gels is prepared by fixing the overall degree of polymerization of the core-forming block at 144 while varying its GlyMA content from 0 to 20 mol %. 1H NMR kinetics indicated that GlyMA is consumed much faster than HPMA, producing a GlyMA-rich sequence close to the PGMA stabilizer block. Temperature-dependent oscillatory rheological studies indicate that increasing the GlyMA content leads to progressively less thermoresponsive worm gels, with no degelation on cooling being observed for worms containing 20 mol % GlyMA. The epoxy groups in the GlyMA residues can be ring-opened using 3-aminopropyltriethoxysilane (APTES) in order to prepare core cross-linked worms via hydrolysis-condensation with the siloxane groups and/or hydroxyl groups on the HPMA residues. Perhaps surprisingly, 1H NMR analysis indicates that the epoxy–amine reaction and the intermolecular cross-linking occur on similar time scales. Cross-linking leads to stiffer worm gels that do not undergo degelation upon cooling. Dynamic light scattering studies and TEM analyses conducted on linear worms exposed to either methanol (a good solvent for both blocks) or anionic surfactant result in immediate worm dissociation. In contrast, cross-linked worms remain intact under such conditions, provided that the worm cores comprise at least 10 mol % GlyMA. PMID:27134311

  3. Method of preparing cross-linked enzyme particles

    NARCIS (Netherlands)

    Mateo, C.; Van Langen, L.M.; Van Rantwijk, F.

    2004-01-01

    The invention relates to a method of preparing cross-linked enzyme particles using a cross-linking agent. According to the invention, the enzyme particles are formed and subsequently cross-linked using a cross-linking agent having at least n reactive groups where N>=3 and a molecular weight of

  4. Method of preparing cross-linked enzyme particles

    NARCIS (Netherlands)

    Mateo, C.; Van Langen, L.M.; Van Rantwijk, F.

    2004-01-01

    The invention relates to a method of preparing cross-linked enzyme particles using a cross-linking agent. According to the invention, the enzyme particles are formed and subsequently cross-linked using a cross-linking agent having at least n reactive groups where N>=3 and a molecular weight of >2,00

  5. Evaluation of ultrasonic atomization as a new approach to prepare ionically cross-linked chitosan microparticles.

    Science.gov (United States)

    Albertini, Beatrice; Passerini, Nadia; Rodriguez, Lorenzo

    2005-07-01

    Ultrasonic atomization was evaluated as a new approach for the preparation of ionically cross-linked controlled-release chitosan microparticles loaded with theophylline as the model drug, using tripolyphosphate (TPP) as counter-ion. It was possible to nebulize both 2% and 3% (w/v) chitosan solutions as a function of their viscosity, usually not processed by employing the conventional nebulizer. The results of the chitosan molecular characterization using the SEC-MALS analysis revealed that ultrasonic atomization caused a certain depolymerization, probably due to the main chain scission of the 1,4-glycosidic bond; however, Fourier transform-infrared spectroscopy revealed the absence of other chemical modifications. The ultrasonic atomization allowed preparation of TPP cross-linked chitosan microparticles mostly ranging between 50 and 200 mum. As regards manufacturing parameters, the linking time and washing medium were found to affect the properties of the microparticles, while the stirring rate of the TPP solution did not show any influence. The evaluation of the formulation variables revealed that chitosan concentration strongly affected both the feasibility of the ultrasonic atomization and the drug release. All the microparticles showed an encapsulation efficiency of > 50 % and, after an initial burst effect, a controlled release of drug for 48 h. In conclusion, the ultrasonic atomization could be proposed as a robust and innovative single-step procedure with scale-up potential to successfully prepare ionically cross-linked chitosan microparticles.

  6. Disulfide cross-linked Fab-aggregates: preparation and biodistribution.

    Science.gov (United States)

    Dalkara, S; Petrov, A; Trubetskoy, V S; Khaw, B A; Torchilin, V P

    1998-01-01

    The high-molecular-weight soluble aggregates of Fab fragments of murine antibodies against cardiac myosin were prepared as a potential long-circulating and low immunogenic pharmaceutical carriers by conjugation of thiolated Fab and Fab modified with succinimidyl 3-(2-pyridyldithio)propionate. The clearance time and biodistribution of 111In-radiolabeled aggregates were studied in normal and nude-mice bearing human breast tumor implant and in rabbits with experimental myocardial infarction. The aggregates had a prolonged circulation time (half clearance time ca. 3-5 h) and ability to concentrate in the tumor and in the necrotic area of infarcted myocardium. Similar tumor-to-normal and infarct-to-normal accumulation ratios (ca. 3 h in both cases) suggest that combination of long circulation with impaired filtration in necrotic tissues is responsible for this accumulation rather than a specific interaction. The aggregates prepared may serve as long-circulating drug carriers able to deliver pharmaceuticals into areas with affected and leaky vasculature.

  7. Preparation of cross-linked hen-egg white lysozyme crystals free of cracks

    Science.gov (United States)

    Yan, Er-Kai; Lu, Qin-Qin; Zhang, Chen-Yan; Liu, Ya-Li; He, Jin; Chen, Da; Wang, Bo; Zhou, Ren-Bin; Wu, Ping; Yin, Da-Chuan

    2016-01-01

    Cross-linked protein crystals (CLPCs) are very useful materials in applications such as biosensors, catalysis, and X-ray crystallography. Hence, preparation of CLPCs is an important research direction. During the preparation of CLPCs, an often encountered problem is that cracks may appear in the crystals, which may finally lead to shattering of the crystals into small pieces and cause problem in practical applications. To avoid cross-link induced cracking, it is necessary to study the cracking phenomenon in the preparation process. In this paper, we present an investigation on how to avoid cracking during preparation of CLPCs. An orthogonal experiment was designed to study the phenomenon of cross-link induced cracking of hen-egg white lysozyme (HEWL) crystals against five parameters (temperature, solution pH, crystal growth time, glutaraldehyde concentration, and cross-linking time). The experimental results showed that, the solution pH and crystal growth time can significantly affect cross-link induced cracking. The possible mechanism was studied, and optimized conditions for obtaining crack-free CLPCs were obtained and experimentally verified. PMID:27703210

  8. Pickering emulsions stabilized by whey protein nanoparticles prepared by thermal cross-linking

    NARCIS (Netherlands)

    Wu, Jiande; Shi, Mengxuan; Li, Wei; Zhao, Luhai; Wang, Ze; Yan, Xinzhong; Norde, Willem; Li, Yuan

    2015-01-01

    A Pickering (o/w) emulsion was formed and stabilized by whey protein isolate nanoparticles (WPI NPs). Those WPI NPs were prepared by thermal cross-linking of denatured WPI proteins within w/o emulsion droplets at 80. °C for 15. min. During heating of w/o emulsions containing 10% (w/v) WPI protein

  9. Preparation and in vitro evaluation of chitosan matrices cross-linked by formaldehyde vapors.

    Science.gov (United States)

    Rao, B S; Murthy, K V

    2000-10-01

    Rifampicin-chitosan matrices were prepared by a chemical cross-linking method to develop a sustained-release form. The effects of cross-linking agent (formaldehyde) on the drug release rate and release kinetics were investigated in this study. Moreover, the kinetics of rifampicin released from chitosan matrices exposed to formaldehyde vapors for predetermined time intervals were analyzed using Ritger and Peppas exponential equation. The in vitro release kinetics exhibited a non-Fickian transport model. Increasing the exposure time to formaldehyde vapors decreased the release rate of rifampicin from chitosan matrices as a result of formation of greater structural strength and tighter texture.

  10. Preparation of Nanocellulose Reinforced Chitosan Films, Cross-Linked by Adipic Acid.

    Science.gov (United States)

    Falamarzpour, Pouria; Behzad, Tayebeh; Zamani, Akram

    2017-02-13

    Adipic acid, an abundant and nontoxic compound, was used to dissolve and cross-link chitosan. After the preparation of chitosan films through casting technique, the in situ amidation reaction was performed at 80-100 °C as verified by Fourier transform infrared (FT-IR). The reaction was accompanied by the release of water which was employed to investigate the reaction kinetics. Accordingly, the reaction rate followed the first-order model and Arrhenius equation, and the activation energy was calculated to be 18 kJ/mol. Furthermore, the mechanical properties of the chitosan films were comprehensively studied. First, optimal curing conditions (84 °C, 93 min) were introduced through a central composite design. In order to evaluate the effects of adipic acid, the mechanical properties of physically cross-linked (uncured), chemically cross-linked (cured), and uncross-linked (prepared by acetic acid) films were compared. The use of adipic acid improved the tensile strength of uncured and chemically cross-linked films more than 60% and 113%, respectively. Finally, the effect of cellulose nanofibrils (CNFs) on the mechanical performance of cured films, in the presence of glycerol as a plasticizer, was investigated. The plasticized chitosan films reinforced by 5 wt % CNFs showed superior properties as a promising material for the development of chitosan-based biomaterials.

  11. Preparation of Nanocellulose Reinforced Chitosan Films, Cross-Linked by Adipic Acid

    Directory of Open Access Journals (Sweden)

    Pouria Falamarzpour

    2017-02-01

    Full Text Available Adipic acid, an abundant and nontoxic compound, was used to dissolve and cross-link chitosan. After the preparation of chitosan films through casting technique, the in situ amidation reaction was performed at 80–100 °C as verified by Fourier transform infrared (FT-IR. The reaction was accompanied by the release of water which was employed to investigate the reaction kinetics. Accordingly, the reaction rate followed the first-order model and Arrhenius equation, and the activation energy was calculated to be 18 kJ/mol. Furthermore, the mechanical properties of the chitosan films were comprehensively studied. First, optimal curing conditions (84 °C, 93 min were introduced through a central composite design. In order to evaluate the effects of adipic acid, the mechanical properties of physically cross-linked (uncured, chemically cross-linked (cured, and uncross-linked (prepared by acetic acid films were compared. The use of adipic acid improved the tensile strength of uncured and chemically cross-linked films more than 60% and 113%, respectively. Finally, the effect of cellulose nanofibrils (CNFs on the mechanical performance of cured films, in the presence of glycerol as a plasticizer, was investigated. The plasticized chitosan films reinforced by 5 wt % CNFs showed superior properties as a promising material for the development of chitosan-based biomaterials.

  12. Design and Preparation of Cross-Linked Polystyrene Nanoparticles for Elastomer Reinforcement

    Directory of Open Access Journals (Sweden)

    Ming Lu

    2010-01-01

    Full Text Available Cross-linked polystyrene (PS particles in a latex form were synthesized by free radical emulsion polymerization. The nano-PS-filled elastomer composites were prepared by the energy-saving latex compounding method. Results showed that the PS particles took a spherical shape in the size of 40–60 nm with a narrow size distribution, and the glass-transition temperature of the PS nanoparticles increased with the cross-linking density. The outcomes from the mechanical properties demonstrated that when filled into styrene-butadiene rubber (SBR, nitrile-butadiene rubber (NBR, and natural rubber (NR, the cross-linked PS nano-particles exhibited excellent reinforcing capabilities in all the three matrices, and the best in the SBR matrix. In comparison with that of the carbon black filled composites, another distinguished advantage of the cross-linked PS particles filled elastomer composites was found to be light weight in density, which could help to save tremendous amount of energy when put into end products.

  13. Preparation of bioimprinting cross-linked enzyme aggregates of phenylalanine ammonia lyase and it's partial properties

    Directory of Open Access Journals (Sweden)

    Jiandong CUI

    2015-12-01

    Full Text Available Phenylalanine ammonia lyase (PAL is a key enzyme for production of L-phenylalanine. Currently, PAL is mainly obtained from Rhodotorula PAL However, Rhodotorula PAL exhibits poor stability, which limits its industrial application. In this study, bioimprinting cross-linked enzyme aggregates of PAL (PAL-iCLEAs is developed by combining cross-linked enzyme aggregates technology and imprinted enzyme method. The most optimal imprinting molecule substrate is screened. Moreover, some characteristics of the PAL-iCLEAs are examined. The results show that the most suitable substrates for preparing PAL-iCLEAs is tran-cinnamic acid. The optimal temperature and pH was 50 ℃ and 10.5, respectively. In addition, PAL-iCLEAs shows good reusability, the recovery of PAL activity still remained 32% after reusing 9 times.

  14. Preparation and Characterization of a pH-Responsive Core Cross-linked Polymer Micelle

    Energy Technology Data Exchange (ETDEWEB)

    Kousaka, Shouta; Sugahara, Makoto; Endo, Tatsuya; Yusa, Shin-ichi, E-mail: yusa@eng.u-hyogo.ac.jp [Department of Materials Science and Chemistry, Graduate School of Engineering, University of Hyogo, 2167 Shosha, Himeji, Hyogo 671-2280 (Japan)

    2011-01-01

    Poly(ethylene glycol)-b-poly(2-(diethylamino) ethyl methacrylate-co-2-cinnamoyl-oxyethyl acrylate) (PEG-b-P(DEA/CEA)) was prepared by reversible addition-fragmentation chain transfer (RAFT) controlled radical polymerization. pH-responsive association behaviour of PEG-b-P(DEA/CEA) in 0.1 M NaCl was characterized by dynamic light scattering (DLS). As solution pH is increased from an acidic pH, the hydrodynamic radius (R{sub h}) increases, indicative of the polymer micelle formation. The formation of a micelle was also supported by static light scattering (SLS) data. The cinnamoyl groups in the core of the polymer micelle undergo photodimerization, yielding cross-links between polymer chains. The core of the polymer micelle was fixed, which was confirmed by DLS, SLS, and small angle X-ray scattering (SAXS) techniques. When pH is decreased to 3, R{sub h} of the core cross-linked (CCL) polymer micelle slightly increases due to the protonation of the DEA unit in the cross-linked core. The reversible pH-induced swelling and shrinking behaviour can be observed.

  15. Mono-dispersed cross-linked polystyrene micro-spheres prepared by seed swelling polymerization method

    Institute of Scientific and Technical Information of China (English)

    Dongsha WANG; Yanjun LIU

    2008-01-01

    A two-step swelling procedure was adopted to synthesize mono-dispersed and highly cross-linked poly (St-divinylbenzene) particles with PSt micro-spheres (1.80 μmin diameter). The PSt micro-spheres were prepared by a dispersion polymerization method and used as seeds. The effects of monomer concentration, ratio of ethanol to water, swelling reagents, crosslinking reagents, swelling temper-ature and agitation speed on particle size were investigated in detail. The morphologies and size distributions of these micro-spheres were examined by SEM and particle size analysis (PSA). The Tg of the micro-spheres was measured by DSC. The results indicate that the particles (6.20 μm in diameter) exhibit excellent mono dispersed property and high crosslinking degree when the concentration of the swelling reagent was 25%, the concentration of the cross-linking reagents was 23%, the swelling temperature was 30℃ and the stirring speed was 150 r/min.

  16. Pickering emulsions stabilized by whey protein nanoparticles prepared by thermal cross-linking.

    Science.gov (United States)

    Wu, Jiande; Shi, Mengxuan; Li, Wei; Zhao, Luhai; Wang, Ze; Yan, Xinzhong; Norde, Willem; Li, Yuan

    2015-03-01

    A Pickering (o/w) emulsion was formed and stabilized by whey protein isolate nanoparticles (WPI NPs). Those WPI NPs were prepared by thermal cross-linking of denatured WPI proteins within w/o emulsion droplets at 80°C for 15 min. During heating of w/o emulsions containing 10% (w/v) WPI proteins in the water phase, the emulsions displayed turbid-transparent-turbid phase transitions, which is ascribed to the change in the size of the protein-containing water droplets caused by thermal cross-linking between denatured protein molecules. The transparent stage indicated the formation of WPI NPs. WPI NPs of different sizes were obtained by varying the mixing speed. WPI NPs of 200-500 nm were selected to prepare o/w Pickering emulsions because of their good stability against coalescence. By Confocal Laser Scanning Microscopy, it was observed that WPI NPs were closely packed and distributed at the surface of the emulsion droplets. By measuring water contact angles of WPI NPs films, it was found that under most conditions WPI NPs present good partial wetting properties, but that at the isoelectric point (pI) and high ionic strength the particles become more hydrophobic, resulting in less stable Pickering emulsion. Thus, at pH above and below the pI of WPI NPs and low to moderate ionic strengths (1-10 mM), and with a WPI NPs concentration of 2% (w/v), a stable Pickering emulsion can be obtained. The results may provide useful information for applications of WPI NPs in environmentally friendly and food grade applications, notably in food, pharmaceutical and cosmetic products.

  17. Preparation, Properties and Mechanism of Inhomogeneous Calcium Alginate Ion Cross-linking Gel Microspheres

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Inhomogeneous calcium alginate ion cross-linking gel microspheres, a novel ion absorbent, were prepared by dropping a sodium alginate solution to a calcium chloride solution via an electronic droplet generator. Calcium alginate microspheres have uniform particle sizes, a smooth surface and a microporous structure. The electrode probe reveals the inhomogeneous distribution of calcium ions with the highest concentration on the surface, and the lowest concentration in the cores of the spheres. As a novel ion adsorbent, calcium alginate gel microspheres have a lower limiting adsorption mass concentration, a higher enrichment capacity and a higher adsorption capacity for Pb2+ than usual ion exchange resins. The highest percentage of the adsorption is 99.79%. The limiting adsorption mass concentration is 0.0426 mg/L. The adsorption capacity for Pb2+ is 644 mg/g. Calcium alginate gel microspheres have a much faster ion exchange velocity than D418 chelating resin and D113 polyacrylate resin. The moving boundary model was employed to interpret the ion exchange kinetics process, which indicates that the ion exchange process is controlled by intraparticle diffusion of adsorbable ions. So the formation of inhomogeneous gel microspheres reduces the diffusion distance of adsorbable ions within the spheres and enhances the ion exchange velocity. Alginate has a higher selectivity for Pb2+ than for Ca2+ and the selectivity coefficient KPbCa is 316. As an ion cross-linking gel, calcium alginate inhomogeneous microspheres can effectively adsorb heavy metal Pb2+ at a higher selectivity and a higher adsorption velocity. It is a novel and good ion adsorbent.

  18. Preparation and characterization of resistant starch type IV nanoparticles through ultrasonication and miniemulsion cross-linking.

    Science.gov (United States)

    Ding, Yongbo; Zheng, Jiong; Xia, Xuejuan; Ren, Tingyuan; Kan, Jianquan

    2016-05-05

    This study aimed to assess the properties of resistant starch type IV (chemically modified starch, RS4) prepared from a new and convenient synthesis route by using ultrasonication combined with water-in-oil miniemulsion cross-linking technique. A three-factor Box-Behnken design and optimization was used to minimize particle size through the developed RS4 nanoparticles. The predicted minimized Z-Avel (576.1nm) under the optimum conditions of the process variables (ultrasonic power, 214.57W; sonication time, 114.73min; and oil/water ratio, 10.54:1) was very close to the experimental value (651.0nm) determined in a batch experiment. After preparing the RS4 nanoparticles, morphological, physical, chemical, and functional properties were assessed. Results revealed that RS4 nanoparticle size reached about 600nm. Scanning electron microscopy images showed that ultrasonication induced notches and grooves on the surface. Under polarized light, the polarized cross was impaired. X-ray diffraction results revealed that the crystalline structure was disrupted. Smaller or no endotherms were exhibited in DSC analysis. In the FTIR graph, new peaks at 1532.91 and 1451.50cm(-1) were observed, and pasting properties were reduced. Amylose content, solubility, and SP increased, but RS content decreased. Anti-digestibility remained after ultrasonication. The prepared RS4 nanoparticles could be extensively used in biomedical applications and in the development of new medical materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. PREPARATION OF NOVEL METALLIC AND BIMETALLIC CROSS-LINKED POLY (VINYL ALCOHOL) NANOCOMPOSITES UNDER MICROWAVE IRRADIATION

    Science.gov (United States)

    A facile method utilizing microwave irradiation is described that accomplishes the cross-linking reaction of PVA with metallic and bimetallic systems. Nanocomposites of PVA-cross-linked metallic systems such as Pt, Cu, and In and bimetallic systems such as Pt-In, Ag-Pt, Pt-Fe, Cu...

  20. NOVEL METALLIC AND BIMETALLIC CROSS-LINKED POLY (VINYL ALCOHOL) NANOCOMPOSITES PREPARED UNDER MICROWAVE IRRADIATION

    Science.gov (United States)

    A facile microwave irradiation approach that results in a cross-linking reaction of poly (vinyl alcohol) (PVA) with metallic and bimetallic systems is described. Nanocomposites of PVA cross-linked metallic systems such as Pt, Cu, and In and bimetallic systems such as Pt-In, Ag-P...

  1. Preparation of cross-linked carboxymethyl jackfruit starch and evaluation as a tablet disintegrant.

    Science.gov (United States)

    Kittipongpatana, Nisit; Suwakon, Janta; Kittipongpatana, Ornanong

    2011-10-01

    The main purposes of this study are to prepare cross-linked carboxymethyl jackfruit starch (CL-CMJF) and to evaluate its pharmaceutical property as a tablet disintegrant. CL-CMJF was prepared by a dual carboxymethyl-crosslinking reaction in a flask containing jackfruit seed starch (JFS), chloroacetic acid (CAA), sodium hydroxide (NaOH) and sodium trimetaphosphate (STMP). The reaction was carried out using methanol as a solvent for 60 min at 70°C and at JFS:CAA:NaOH:STMP ratio of 1.0:0.29:0.28:0.07. The obtained CL-CMJF, with degree of substitution and degree of crosslinking calculated to be 0.34 and 0.06, respectively, was insoluble but swellable in water. Rheological study revealed a decreased in solution viscosity compared to the non-crosslinked CMJF. The water uptake of CL-CMJF was 23 times higher than that of native starch and was comparable to that of a commercial superdisintegrant, sodium starch glycolate (SSG). The swelling ability of CL-CMRS was similar to that of crosscarmellose sodium (CCS), another commercial superdisintegrant. Disintegration test of aspirin tablets containing 2%w/w of JFS, CL-CMJF, SSG and CCS showed disintegration times in the order of SSG < CCS ~ CL-CMJF < JFS. The results suggested that CL-CMJF could be developed as a tablet disintegrant.

  2. Preparation of Thermo-Responsive Poly(ionic liquids-Based Nanogels via One-Step Cross-Linking Copolymerization

    Directory of Open Access Journals (Sweden)

    Jing Zhang

    2015-09-01

    Full Text Available In this study, thermo-responsive polymeric nanogels were facilely prepared via one-step cross-linking copolymerization of ethylene glycol dimethacrylate/divinylbenzene and ionic liquid (IL-based monomers, 1,n-dialkyl-3,3′-bis-1-vinyl imidazolium bromides ([CnVIm]Br; n = 6, 8, 12 in selective solvents. The results revealed that stable and blue opalescent biimidazolium (BIm-based nanogel solutions could be obtained without any precipitation when the copolymerizations were conducted in methanol. Most importantly, these novel nanogels were thermo-response, and could reversibly transform to precipitation in methanol with temperature changes. Turbidity analysis and dynamic light scatting (DLS measurement illustrated that PIL-based nanogel solutions presented the phase transform with upper critical solution temperature (UCST in the range of 5–25 °C. The nanogels were characterized using Fourier transform infrared (FTIR, thermogravimetric analyses (TGA, and scanning electron microscopy (SEM. In addition, BIm-based nanogels could also be used as highly active catalysts in the cycloaddition reaction of CO2 and epoxides. As a result, our attributes build a robust platform suitable for the preparation of polymeric nanomaterials, as well as CO2 conversion.

  3. Silica cross-linked micelles loading with silicon nanoparticles: preparation and characterization.

    Science.gov (United States)

    Pan, Guo-Hui; Barras, Alexandre; Boussekey, Luc; Boukherroub, Rabah

    2013-08-14

    A new family of luminescent and stable silicon-based nanoparticles (NPs), silica cross-linked pluronic F127 (PF127) micelles loaded with decyl capped silicon nanoparticles (decyl-SiNPs), were synthesized in aqueous media. The decyl-SiNPs were prepared by first liberating hydride terminated SiNPs (H-SiNPs) from a porous silicon matrix followed by their functionalization via hydrosilylation with 1-decene under photochemical activation. The silicon-based NPs exhibit bright photoluminescence (PL) with a quantum yield of ∼3.8% and peaking at ∼2.0 eV, which lies within the transmission window that is useful for biological imaging. They display a hydrodynamic size of ∼25 nm with exterior polyethylene oxide (PEO) blocks stretching out in aqueous media. Chloroform was found to quench the excitation at energy above 4.9 eV by shielding the incident light or relaxing the charge carriers, which highlights that caution against solvent interference should be taken when performing the studies on PL origin and luminescence efficiency of SiNPs. For PF127, the blocks of hydrophilic PEO participate in the PL quenching, while poly(propylene oxide) (PPO) does not. The colloidal solution displays excellent PL stability against salt (NaCl) and temperature but is susceptible to basic solution at pH above 9.

  4. Borate cross-linked graphene oxide-chitosan as robust and high gas barrier films

    Science.gov (United States)

    Yan, Ning; Capezzuto, Filomena; Lavorgna, Marino; Buonocore, Giovanna G.; Tescione, Fabiana; Xia, Hesheng; Ambrosio, Luigi

    2016-05-01

    Chitosan (CS) is one of the most promising polymers due to its biocompatibility, biodegradability, and natural abundance. However, its poor mechanical and barrier properties make it difficult to satisfy a wide range of applications. Herein, borate ions, originating from the hydrolysis of sodium tetraborate decahydrate (borax), have been used to crosslink chitosan and graphene oxide (GO) nanocomposites. Chitosan films consisting of 1.0 wt% boron and 1.0 wt% GO exhibit a significant improvement in both the toughness and oxygen barrier properties compared to pristine chitosan. In particular the tensile strength of the samples after thermal treatment increases by ~160% compared to pristine chitosan, whereas their oxygen permeability reduces by ~90%. This is ascribed to the chemical crosslinking between chitosan and GO nanoplatelets through borate ions, as well as the formation of a layered morphology with graphene nanoplatelets oriented parallel to the sample surface. The exceptional robust and high gas barrier film has promising application in the packaging industry. The borate-crosslinking chemistry represents the potential strategy for improving properties of other polymer nanocomposites.Chitosan (CS) is one of the most promising polymers due to its biocompatibility, biodegradability, and natural abundance. However, its poor mechanical and barrier properties make it difficult to satisfy a wide range of applications. Herein, borate ions, originating from the hydrolysis of sodium tetraborate decahydrate (borax), have been used to crosslink chitosan and graphene oxide (GO) nanocomposites. Chitosan films consisting of 1.0 wt% boron and 1.0 wt% GO exhibit a significant improvement in both the toughness and oxygen barrier properties compared to pristine chitosan. In particular the tensile strength of the samples after thermal treatment increases by ~160% compared to pristine chitosan, whereas their oxygen permeability reduces by ~90%. This is ascribed to the chemical

  5. Substrate-Independent Robust and Heparin-Mimetic Hydrogel Thin Film Coating via Combined LbL Self-Assembly and Mussel-Inspired Post-Cross-linking.

    Science.gov (United States)

    Ma, Lang; Cheng, Chong; He, Chao; Nie, Chuanxiong; Deng, Jie; Sun, Shudong; Zhao, Changsheng

    2015-12-01

    In this work, we designed a robust and heparin-mimetic hydrogel thin film coating via combined layer-by-layer (LbL) self-assembly and mussel-inspired post-cross-linking. Dopamine-grafted heparin-like/-mimetic polymers (DA-g-HepLP) with abundant carboxylic and sulfonic groups were synthesized by the conjugation of adhesive molecule, DA, which exhibited substrate-independent adhesive affinity to various solid surfaces because of the formation of irreversible covalent bonds. The hydrogel thin film coated substrates were prepared by a three-step reaction: First, the substrates were coated with DA-g-HepLP to generate negatively charged surfaces. Then, multilayers were obtained via LbL coating of chitosan and the DA-g-HepLP. Finally, the noncovalent multilayers were oxidatively cross-linked by NaIO4. Surface ATR-FTIR and XPS spectra confirmed the successful fabrication of the hydrogel thin film coatings onto membrane substrates; SEM images revealed that the substrate-independent coatings owned 3D porous morphology. The soaking tests in highly alkaline, acid, and concentrated salt solutions indicated that the cross-linked hydrogel thin film coatings owned high chemical resistance. In comparison, the soaking tests in physiological solution indicated that the cross-linked hydrogel coatings owned excellent long-term stability. The live/dead cell staining and morphology observations of the adhered cells revealed that the heparin-mimetic hydrogel thin film coated substrates had low cell toxicity and high promotion ability for cell proliferation. Furthermore, systematic in vitro investigations of protein adsorption, platelet adhesion, blood clotting, and blood-related complement activation confirmed that the hydrogel film coated substrates showed excellent hemocompatibility. Both the results of inhibition zone and bactericidal activity indicated that the gentamycin sulfate loaded hydrogel thin films had significant inhibition capability toward both Escherichia coli and

  6. Preparation and characterization of genipin-cross-linked silk fibroin/chitosan sustained-release microspheres.

    Science.gov (United States)

    Zeng, Shuguang; Ye, Manwen; Qiu, Junqi; Fang, Wei; Rong, Mingdeng; Guo, Zehong; Gao, Wenfen

    2015-01-01

    We report the effects of distinct concentrations of genipin and silk fibroin (SF):chitosan (CS) ratios on the formation of SF-CS composite microspheres. We selected microspheres featuring an SF:CS ratio of 1:1, encapsulated various concentrations of bovine serum albumin (BSA), and then compared their encapsulation efficiency and sustained-release rate with those of pure CS microspheres. We determined that the following five groups of microspheres were highly spherical and featured particle sizes ranging from 70 μm to 147 μm: mass ratio of CS:SF =1:0.5, 0.1 g or 0.5 g genipin; CS:SF =1:1, 0.05 g or 1 g genipin; and CS:SF =1:2, 0.5 g genipin. The microspheres prepared using 1:1 CS:SF ratio and 0.05 g genipin in the presence of 10 mg, 20 mg, and 50 mg of BSA exhibited encapsulation efficiencies of 50.16%±4.32%, 56.58%±3.58%, and 42.19%±7.47%, respectively. Fourier-transform infrared spectroscopy (FTIR) results showed that SF and CS were cross-linked and that the α-helices and random coils of SF were converted into β-sheets. BSA did not chemically react with CS or SF. Moreover, thermal gravimetric analysis (TGA) results showed that the melting point of BSA did not change, which confirmed the FTIR results, and X-ray diffraction results showed that BSA was entrapped in microspheres in a noncrystalline form, which further verified the TGA and FTIR data. The sustained-release microspheres prepared in the presence of 10 mg, 20 mg, and 50 mg of BSA burst release 30.79%±3.43%, 34.41%±4.46%, and 41.75%±0.96% of the entrapped BSA on the 1st day and cumulatively released 75.20%±2.52%, 79.16%±4.31%, and 89.04%±4.68% in 21 days, respectively. The pure CS microspheres prepared in the presence of 10 mg of BSA burst release 39.53%±1.76% of BSA on the 1st day and cumulatively released 83.57%±2.33% of the total encapsulated BSA in 21 days. The SF-CS composite microspheres exhibited higher sustained release than did the pure CS microspheres, and thus these composite

  7. Preparation of molecularly imprinted cross-linked chitosan/glutaraldehyde resin for enantioselective separation of L-glutamic acid.

    Science.gov (United States)

    Monier, M; El-Sokkary, A M A

    2010-08-01

    In the present study, separation of L-glutamic acid from dilute aqueous solution by solid-phase extraction based on molecular imprinting technique using cross-linked chitosan/glutaraldehyde resin was investigated. L-Glutamic acid imprinted cross-linked chitosan (LGIC) was prepared by cross-linking of chitosan by glutaraldehyde cross-linker, in the presence of L-glutamic acid. Non-imprinted cross-linked chitosan (NIC) as control was also prepared by the same procedure in the absence of template molecules. The morphological structures of both LGIC and NIC were examined by scanning electron microscope (SEM). LGIC particles were applied to determine the optimum operational condition for l-glutamic acid separation from dilute aqueous solution. In adsorption step, optimum pH and retention time were 5.5 and 100 min, while corresponding values in extraction step were 2.5 and 60 min, respectively. The adsorption isotherms indicated that the maximum adsorption capacities of L- and D-glutamic acid on LGIC were 42+/-0.8 and 26+/-1.2mg/g, respectively, while in case of NIC, both L- and D-glutamic acid present the same maximum adsorption capacity 7+/-0.6 mg/g, which confirm that the molecular imprinting technique creates an enantioselectivity of LGIC toward L-glutamic acid. In addition, chiral resolution of l-, d-glutamic acid racemic mixture was carried out using column of LGIC. Copyright 2010 Elsevier B.V. All rights reserved.

  8. Preparation of Thermo-Responsive and Cross-Linked Fluorinated Nanoparticles via RAFT-Mediated Aqueous Polymerization in Nanoreactors.

    Science.gov (United States)

    Ma, Jiachen; Zhang, Luqing; Geng, Bing; Azhar, Umair; Xu, Anhou; Zhang, Shuxiang

    2017-01-25

    In this work, a thermo-responsive and cross-linked fluoropolymer poly(2,2,2-Trifluoroethyl) methacrylate (PTFEMA) was successfully prepared by reversible addition-fragmentation chain transfer (RAFT) mediated aqueous polymerization with a thermo-responsive diblock poly(dimethylacrylamide-b-N-isopropylacrylamide) (PDMA-b-PNIPAM) that performed a dual function as both a nanoreactor and macro-RAFT agent. The cross-linked polymer particles proved to be in a spherical-like structure of about 50 nm in diameter and with a relatively narrow particle size distribution. ¹H-NMR and (19)F-NMR spectra showed that thermo-responsive diblock P(DMA-b-NIPAM) and cross-linked PTFEMA particles were successfully synthesized. Influence of the amount of ammonium persulfate (APS), the molar ratio of monomers to RAFT agent, influence of the amount of cross-linker on aqueous polymerization and thermo-responsive characterization of the particles are investigated. Monomer conversion increased from 44% to 94% with increasing the molar ratio of APS and P(DMA-b-NIPAM) from 1:9 to1:3. As the reaction proceeded, the particle size increased from 29 to 49 nm due to the consumption of TFEMA monomer. The size of cross-linked nanoparticles sharply decreased from 50.3 to 40.5 nm over the temperature range 14-44 °C, suggesting good temperature sensitivity for these nanoparticles.

  9. Preparation of Cross-Linked Glucoamylase Aggregates Immobilization by Using Dextrin and Xanthan Gum as Protecting Agents

    Directory of Open Access Journals (Sweden)

    Xiao-Dong Li

    2016-05-01

    Full Text Available In this paper glucoamylase from Aspergillus niger was immobilized by using a modified version of cross-linked enzyme aggregates (CLEA. The co-aggregates were cross-linked with glutaraldehyde; meanwhile dextrin and xanthan gum as protecting agents were added, which provides high affinity with the enzyme molecules. The immobilized glucoamylase was stable over a broad range of pH (3.0–8.0 and temperature (55–75 °C; dependence shows more catalytic activity than a free enzyme. The thermostability, kinetic behavior, and first-order inactivation rate constant (ki were investigated. The two types of protector made the immobilized glucoamylase more robust than the free form. Both of the immobilized enzymes have excellent recyclability, retaining over 45% of the relative activity after 24 runs. In addition, immobilized enzymes reduced only 40% of the initial activity after three months by the storability measure, indicating high activity.

  10. Preparation of new hyper cross-linked chelating resin for adsorption of Cu2+ and Ni2+ from water

    Institute of Scientific and Technical Information of China (English)

    Cheng Cheng; Jin Nan Wang; Li Xu; Ai Min Li

    2012-01-01

    The new hyper cross-linked chelating resin NDWJN2 modified with carboxyl groups was prepared for removal of Cu2+ and Ni2+ from water.NDWJN2 was characterized using BET,SEM and FT-IR spectroscopy.Comparing with commercial resins D113 and IRC84,NDWJN2 could remove Cu2+ and Ni2+ from water more effectively.Langmuir model could fit adsorption isotherms well.

  11. Preparation of novel ferrocene-based shell cross-linked thermoresponsive hybrid micelles with antitumor efficacy.

    Science.gov (United States)

    Wei, Hua; Quan, Chang-Yun; Chang, Cong; Zhang, Xian-Zheng; Zhuo, Ren-Xi

    2010-04-29

    The shell cross-linked (SCL) thermoresponsive hybrid poly(N-isopropylacrylamide-co-aminoethyl methacrylate)-b-polymethyl methacrylate (P(NIPAAm-co-AMA)-b-PMMA) micelle consisting of a cross-linked thermoresponsive hybrid shell and a hydrophobic core domain was fabricated via a two-step process: micellization of P(NIPAAm-co-AMA)-b-PMMA in aqueous solution followed by cross-linking of the hydrophilic shell layer via the amidation reaction between the amine groups of AMA units and the carboxylic acid functions of 1,1'-ferrocenedicarboxylic acid. The SCL micelle showed reversible dispersion/aggregation in response to the temperature cycles through the lower critical solution temperature (LCST) of the thermoresponsive hybrid shell at around 36 degrees C, observed by turbidity measurements and dynamic light scattering (DLS). Besides the usage as an inorganic difunctional cross-linker, the inorganic ferrocene segment further endowed the SCL hybrid micelle with the antitumor efficacy, namely, the resulting SCL micelle exhibited a remarkable cytotoxic effect for HeLa cells with a very low IC50. The results showed that the SCL hybrid micelle developed in this study could be potentially used as an antitumor agent, which is unique compared to the conventional tumor therapy by using the antitumor drug loaded in the micellar core.

  12. Preparation and adsorption property of aminated cross linking microbeads of GMA/EGDMA for bilirubin

    Indian Academy of Sciences (India)

    Zhiping Chen; Baojiao Gao; Xiaofeng Yang

    2009-11-01

    Cross linking microbeads with a controllable diameter were synthesized by suspension copolymerization of the monomer glycidyl methacrylate (GMA) and the cross linking agent ethylene glycol dimethylacrylate (EGDMA). By the ring-opening reaction of the epoxy groups, the microbeads GMA/EGDMA were modified with different aminating agents and resulting in the aminated microbeads. The morphology of the microbeads was characterized by SEM. The adsorption property of aminated microbeads for bilirubin was investigated, and the effects of various factors, such as the chemical structures of the aminating agents, pH values of the medium and the presence of bovine serum albumin in the adsorption medium, on the adsorption property were examined. The experimental results show that the aminated microbeads have strong adsorption ability for bilirubin, and the isotherm adsorption behaviour is fitted to Freundlich equation satisfactorily. The adsorption ability of the aminated microbeads modified with hexanediamine is stronger than that of others, and the longer the molecule of multi-ethylene multiamine, the weaker the adsorption ability for bilirubin. The pH value of the medium affects the adsorption ability greatly, as pH = 6, the adsorption ability is strongest. In the presence of BSA, the microbeads still have a higher adsorption capacity towards bilirubin.

  13. 交联瓜尔胶制备工艺%Preparation of Cross-linked Guar Gum

    Institute of Scientific and Technical Information of China (English)

    唐洪波; 王习光; 李艳平

    2012-01-01

    以瓜尔胶为原料、环氧氯丙烷为交联剂、氢氧化钠为催化剂、乙醇为溶剂,对交联瓜尔胶的制备工艺进行研究。考察环氧氯丙烷用量、pH值、反应时间、反应温度和乙醇质量分数对交联瓜尔胶沉降积的影响。结果表明,环氧氯丙烷用量、pH值、反应时间、反应温度和乙醇质量分数对瓜尔胶交联反应均有影响。制备交联瓜尔胶的最佳工艺条件为交联剂环氧氯丙烷用量8%、pH值、反应时间3.5h、反应温度40℃、乙醇质量分数95%。瓜尔胶交联反应的影响主次顺序依次为环氧氯丙烷用量〉反应温度〉pH值〉反应时间〉乙醇质量分数。热分析表明,随着交联瓜尔胶交联度的增加,交联瓜尔胶的热稳定性、焓变、吸收峰起始温度、峰值温度和结束温度增加。%The preparation of cross-linked guar gum was investigated by using epichlorohydrin as the cross-linking agent, sodium hydroxide as the catalyst and ethanol as the solvent in this study. The effects of epichlorohydrin amount, pH, reaction time, reaction temperature and alcohol concentration on the sediment volume of cross-linked guar gum was explored. The results showed that epichlorohydrin amount, pH, reaction time, reaction temperature and alcohol concentration had obvious impact on cross-linked reaction of guar gum. The optimal conditions for preparing cross-linked guar gum were epichlorohydlin amount of 8%, reaction time of 3.5 h, reaction temperature of 40 ℃ and ethanol concentration of 95%. Five reaction conditions were ranked in decreasing order of their effect on the sediment volume of cross-linked guar gum as follows: epichlorohydrin amount, reaction temperature, pH, reaction time and alcohol concentration. The thermal stability, enthalpy change, endothermic onset temperature, peak temperature and final temperature of cross-linked guar gum increased with increasing degree of cross-linking.

  14. Preparation and characterization of poly(maleic acid)-grafted cross-linked chitosan microspheres for Cd(II) adsorption.

    Science.gov (United States)

    Yu, Zhenzhen; Dang, Qifeng; Liu, Chengsheng; Cha, Dongsu; Zhang, Haifeng; Zhu, Wenjing; Zhang, Qianqian; Fan, Bing

    2017-09-15

    A novel adsorbent, composed of poly(maleic acid)-grafted cross-linked chitosan microspheres (PMACCMs), was prepared via cross-linking with glutaraldehyde and modification by grafting maleic acid. FTIR, zeta potential, elemental analysis, (13)C NMR, DTG, laser particle size analysis, SEM, and BET methods were applied to characterize PMACCMs, exhibiting a successful fabrication, good thermostability, and well-defined surface microstructure beneficial to Cd(II) adsorption. The effects of pH, contact time, and initial concentration on Cd(II) adsorption were also investigated, and the maximum adsorption capacity was 39.2mgg(-1), indicating a great improvement as compared with that (14.5mgg(-1)) of cross-linked chitosan microspheres. The experimental data were well fitted with pseudo-second-order kinetic and Langmuir isotherm models. Five-cycle reusability tests demonstrated PMACCMs could be repeatedly used with a small adsorption capacity loss (<15%). Additionally, the adsorption mechanism was proposed. All the results confirmed that PMACCMs, which presented outstanding adsorption capability and reusability, could be a good candidate for wastewater purification. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Preparation of shell cross-linked nano-objects from hybrid-peptide block copolymers.

    Science.gov (United States)

    Rodríguez-Hernández, Juan; Babin, Jérôme; Zappone, Bruno; Lecommandoux, Sébastien

    2005-01-01

    Supramolecular structures formed by self-assembly of diblock copolymers in solution are stable over restricted environmental conditions: concentration, temperature, pH, or ion strength among others. To enlarge their domain of application, it appears necessary to develop stabilization strategies. We report here different strategies to stabilize the shell of micelles formed by self-assembly of amphiphilic polydiene-b-polypeptide diblock copolymers. For this purpose, covalent bonds can be formed between either amine or carboxylic acid groups distributed along the soluble peptide block and a cross-linking agent that contains respectively aldehyde or amine functions. Shell stabilization affords systems with unique properties that combine three main advantages: shape persistence, control of the porosity, and stimuli-responsive behavior. The covalent capture of such macromolecular objects has been studied by light scattering, AFM, and conductimetry measurements.

  16. Preparation and Characterization of Ionotropic Cross-Linked Chitosan Microparticles for Controlled Release of Aceclofenac

    Directory of Open Access Journals (Sweden)

    N. G. Raghavendra Rao

    2010-04-01

    Full Text Available Aceclofenac, (2-[2-[2-(2, 6-dichlorophenyl aminophenyl] acety] oxyacetic acid a non-steroidal anti-inflammatory drug (NSAID, has been indicated for various conditions like post-traumatic pain, rheumatoid arthritis, ankylosing spondylitis. Multiple-unit systems have been reported to avoid the variations in gastric emptying and different transit rates through gastro-intestinal and spread over a large area preventing exposure of the absorbing site to high drug concentration on chronic dosing. The purpose of this study was therefore to develop aceclofenac loaded chitosan microparticles by ionotropic gelation method. Drug loading efficiency (DLE of microparticles was found between 62.20 to 92.93 % and depended on the formulation variables. Increase in the Tripolyphosphate (TPP concentration, pH of the TPP solution and cross-linking time decreased the drug release. The particle size decreased with increase in cross-linking time and found between the ranges of 1194.1 to 1568.9 µm. Drug release showed slight burst effect in phosphate buffer pH 7.4 in first hour followed by prolonged release for 8 hrs. FTIR and DSC revealed that there was no interaction between drug and polymer. The release data was fitted into first order, zero order and Higuchi model to find release kinetics. The values of regression coefficient r2 were found to be greater (£ 0.9541 for first order than for zero order (£ 0.8740 and the r2 value for Higuchi was £ 0.9805 suggesting diffusion controlled process. The result concluded that TPP-chitosan microparticles developed by ionotropic gelation method might become potential delivery system to prolonging the release of aceclofenac.

  17. Multifunctional Hydrogels Prepared by Dual Ion Cross-Linking for Chronic Wound Healing.

    Science.gov (United States)

    Li, Yonghui; Han, Yan; Wang, Xiaoya; Peng, Jinliang; Xu, Yuhong; Chang, Jiang

    2017-05-17

    The creation of a moist environment and promotion of blood vessel formation are critical for wound healing. Sodium alginate (SA) hydrogel, which has good biocompatibility and is able to provide a moist environment, has been widely used as a wound dressing. However, it lacks antibacterial ability and bioactivities, which would facilitate chronic wound healing. On the basis of the gelation characteristics of SA and the bioactive hardystonite (HS) bioceramic, we designed a unique, bioactive, injectable composite hydrogel through double ion cross-linking, in which divalent ions, such as Ca(2+) and Zn(2+) function as cross-linkers; Zn(2+) also functions as an antibacterial component and as nutrition for wound healing, and Si ions play a key role in determining the bioactivity of the hydrogel. With the controlled release of divalent ions, such as Ca(2+) and Zn(2+) from HS, the gelation process of the composite hydrogel could be efficiently controlled. In addition, in vitro results reveal that the composite hydrogel stimulated proliferation and migration of both human dermal fibroblasts and human umbilical vein endothelial cells, and the in vivo results show that the wound-healing process is obviously enhanced, and the formation of epithelium and blood vessels are evidently advanced. This study indicates the potential of the SA/HS hydrogel as a multifunctional injectable wound dressing with the ability to inhibit bacterial growth and stimulate angiogenesis and wound healing.

  18. Preparation and characterization of a microencapsulated polyethylene glycol cross-linked polyhemoglobin.

    Science.gov (United States)

    Knirsch, Marcos C; Dell'Anno, Filippo; Chicoma, Dennis; Stephano, Marco Antonio; Bou-Chacra, Nádia A; Palombo, Domenico; Converti, Attilio; Polakiewicz, Bronislaw

    2015-11-01

    Many complications are associated to the therapeutic use of blood, among which are not only transfusion adverse events but also other issues such as lack of donors and high costs for collecting, testing, preserving, and distributing blood packages. Therefore, a clinically viable "blood substitute" is considered the holy grail of traumatology and may greatly benefit medicine. One of the most successful approaches to date is conjugating hemoglobin with polyethylene glycol (PEG). This conjugation aims mainly at overcoming free cell hemoglobin toxicity, which makes its use as oxygen carrier in pure form unfeasible. To improve PEG-hemoglobin conjugates feasibility, we propose applying dual functional PEG cross-linking hemoglobin molecules encapsulated by a protein carrier. The new oxygen carrier showed mean values of the hydrodynamic diameter, dispersity, and zeta potential of 1370 nm, 0.029 and -36 mV, respectively, evidencing the successful synthesis of PEG bis(N-succinimidyl succinate) and polyhemoglobin as well as the structuring of protein carrier.

  19. Preparation, stability and antimicrobial activity of cationic cross-linked starch-iodine complexes.

    Science.gov (United States)

    Klimaviciute, Rima; Bendoraitiene, Joana; Rutkaite, Ramune; Siugzdaite, Jurate; Zemaitaitis, Algirdas

    2012-12-01

    Cationic cross-linked starch (CCS)-iodine complexes containing different amounts of quaternary ammonium groups (different degrees of substitution (DS)) and iodine have been obtained by iodine adsorption on CCS from aqueous iodine potassium iodide solution. Equilibrium adsorption studies showed that with an increase of DS the amount of iodine adsorbed on CCS and the affinity of iodine to CCS increased linearly. The influences of the DS of CCS and the amount of adsorbed iodine on the stability of CCS-iodine complexes in a solution of 0.02M sodium acetate and reactivity toward l-tyrosine have been investigated. At the same DS, the stability of CCS-iodine complexes decreased with an increase of the amount of adsorbed iodine. With increasing the DS, the stability of CCS-iodine complexes increased. The iodine consumption in the reaction with l-tyrosine increased significantly with an increase of the amount of adsorbed iodine. The influence of DS on iodine consumption was lower and depended on the amount of adsorbed iodine. The antibacterial activity of CCS-iodine complexes against Bacillus cereus, Staphylococcus aureus, Pseudomonas aeruginosa and Escherichia coli was determined by the broth-dilution and spread-plate methods. The obtained results have demonstrated that an appropriate selection of the CCS-iodine complex composition (the DS of CCS and the amount of adsorbed iodine) could ensure good antimicrobial properties by keeping a low concentration of free iodine in the system. The main advantage of using CCS-iodine complexes as antimicrobial agents is the biodegradability of the polymeric matrix.

  20. IN SITU PREPARED TiO2 NANOPARTICLES CROSS-LINKED SULFONATED PVA MEMBRANES WITH HIGH PROTON CONDUCTIVITY FOR DMFC

    Directory of Open Access Journals (Sweden)

    Jignasa N. Solanki

    2016-07-01

    Full Text Available Organic/inorganic membranes based on sulfonated poly(vinyl alcohol (SPVA and in situ prepared TiO2 nanoparticles nanocomposite membranes with various compositions were prepared to use as proton exchange membranes in direct membrane fuel cells. Poly(vinyl alcohol (PVA was sulfonated and cross-linked separately by 4-formylbenzene-1,3-disulfonic acid disodium salt hydrate and glutaraldehyde. The ion exchange capacity and proton conductivity of the membranes increased with increasing amount of TiO2 nanoparticles. The composite membranes with 15 wt% TiO2 exhibited excellent proton conductivity of 0.0822 S cm-1, as well as remarkably low methanol permeability of 1.11×10-9 cm2 s-1. The thermal stability and durability were also superior and performance in methanol fuel cell was also reasonably good

  1. A Novel Membrane Prepared from Sodium Alginate Cross-linked with Sodium Tartrate for CO2 Capture

    Institute of Scientific and Technical Information of China (English)

    朱娅群; 王志; 张晨昕; 王纪孝; 王世昌

    2013-01-01

    The membrane-based CO2 separation process has an advantage compared to traditional CO2 separation technologies. The membrane is the key of the membrane separation process. In this paper, preparation, characteriza-tion and laboratory testing of the membrane, which was prepared from sodium alginate, hydrogen bond cross-linked with sodium tartrate and used for CO2/N2 separation, were reported. The resistance to SO2 of the membrane was also investigated. The experimental results demonstrate that the membrane possesses a high resistance to SO2. Finally, based on experimental results, the economic feasibility of the membrane used for CO2/N2 separation was evaluated, indicating the two-stage membrane process can compete with the traditional chemical absorption method.

  2. Preparation of porous, chemically cross-linked, PVdF-based gel polymer electrolytes for rechargeable lithium batteries

    Science.gov (United States)

    Cheng, C. L.; Wan, C. C.; Wang, Y. Y.

    This study reports the development of a new system of porous, chemically cross-linked, gel polymer electrolytes based on poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF-HFP) copolymer as a polymer matrix, polyethylene glycol (PEG) as a plasticizer, and polyethylene glycol dimethacrylate (PEGDMA) as a chemical cross-linking oligomer. The electrolytes are prepared by a combination of controlled evaporation and thermal polymerization of PEGDMA. PVdF-HFP/PEG/PEGDMA gel polymer electrolytes with a composition of 5/3/2 exhibit both high ambient ionic conductivity, viz., >1 mS cm -1, and a high tensile modulus of 52 MPa, because of their porous and network structures. All the blends of electrolytes are electrochemically stable up to 5 V versus Li/Li + in the presence of 1 M LiPF 6/ethylene carbonate-diethyl carbonate (EC-DEC). With these polymer electrolytes, rechargeable lithium batteries composed of carbon anode and LiCoO 2 cathode have acceptable cycleability and a good rate capability.

  3. Redox-responsive core cross-linked prodrug micelles prepared by click chemistry for pH-triggered doxorubicin delivery

    Directory of Open Access Journals (Sweden)

    X. T. Cao

    2017-10-01

    Full Text Available A pH-triggered drug delivery system of degradable core cross-linked (CCL prodrug micelles was prepared by click chemistry. Doxorubicin conjugated block copolymers of azido functional poly(ethylene oxide-b-poly(glycidyl methacrylate were synthesized by the combination of RAFT polymerization, epoxide ring-opening reaction, and acid-cleavable hydrazone linkages. The CCL prodrug micelles were produced by the reaction of dipropargyl 3,3′-dithiodipropionate and dipropargyl adipate cross-linking agents with the azido groups of the micellar core via alkyne-azide click reaction, which were denoted as CCL/SS and CCL/noSS, respectively. The TEM images of CCL/SS prodrug micelles showed a spherical shape with the average diameter of 61.0 nm from water, and the shape was maintained with an increased diameter upon dilution with 5-fold DMF. The high DOX conjugation efficiency was 88.4%. In contrast to a very slow DOX release from CCL/SS prodrug micelles under the physiological condition (pH 7.4, the drug release is much faster (90% at pH 5.0 and 10 mM of GSH after 96 h. The cytotoxicity test and confocal laser scanning microscopy analysis revealed that CCL/SS prodrug micelles had much enhanced intracellular drug release capability in HepG2 cells than CCL/noSS prodrug micelles.

  4. Preparation and application of cross-linked core-shell PBA/PS and PBA/PMMA nanoparticles

    Institute of Scientific and Technical Information of China (English)

    Zeng Zhong; Yu Jian; Guo Zhaoxia; Li Ying

    2006-01-01

    This paper reports the preparation of crosslinked core-shell poly(butyl acrylate )/polystyrene (PBA/PS)and poly(butyl acrylate)/poly(methyl methacrylate) (PBA/PMMA) nanoparticles via seeded emulsion polymerization and their application in nylon-based composites.A highly cross-linked structure was formed in both the cores and the shells by using a cross-linking agent,which could prevent the migration of hydrophobic PS shells tO the inside of particles.There were covalent bonds on the interfaces between the cores and the shells of both particles.The average particle sizes were 40-50 nm,and the size distributions were narrow.The kinetics of polymerization was investigated.Well-defined core-shell structure and narrow particle size distribution could be achieved under starved conditions of monomer feeding.Furthermore,PBA/PMMA particles were used to fill nylon 6,good dispersion was obtained because of the strong interfacial interaction between the nanoparticles and the nylon 6 matrix and the good deformation ability of nanoparticles,and the toughness and rigidity of the composites were improved evidently.

  5. Biological Effects of Drug-Free Alginate Beads Cross-Linked by Copper Ions Prepared Using External Ionotropic Gelation.

    Science.gov (United States)

    Pavelková, M; Kubová, K; Vysloužil, J; Kejdušová, M; Vetchý, D; Celer, V; Molinková, D; Lobová, D; Pechová, A; Vysloužil, J; Kulich, P

    2016-08-08

    External ionotropic gelation offers a unique possibility to entrap multivalent ions in a polymer structure. The aim of this experimental study was to prepare new drug-free sodium alginate (ALG) particles cross-linked by Cu(2+) ions and to investigate their technological parameters (particle size, sphericity, surface topology, swelling capacity, copper content, release of Cu(2+) ions, mucoadhesivity) and biological activity (cytotoxicity and efficiency against the most common vaginal pathogens-Herpes simplex, Escherichia coli, Candida albicans) with respect to potential vaginal administration. Beads prepared from NaALG dispersions (3 or 4%) were cross-linked by Cu(2+) ions (0.5 or 1.0 M CuCl2) using external ionotropic gelation. Prepared mucoadhesive beads with particle size over 1000 μm exhibited sufficient sphericity (all ˃0.89) and copper content (214.8-249.07 g/kg), which increased with concentration of polymer and hardening solution. Dissolution behaviour was characterized by extended burst effect, followed by 2 h of copper release. The efficiency of all samples against the most common vaginal pathogens was observed at cytotoxic Cu(2+) concentrations. Anti-HSV activity was demonstrated at a Cu(2+) concentration of 546 mg/L. Antibacterial activity of beads (expressed as minimum inhibition concentration, MIC) was influenced mainly by the rate of Cu(2+) release which was controlled by the extent of swelling capacity. Lower MIC values were found for E. coli in comparison with C. albicans. Sample ALG-3_1.0 exhibited the fastest copper release and was proved to be the most effective against both bacteria. This could be a result of its lower polymer concentration in combination with smaller particle size and thus larger surface area.

  6. Oligo(ethylene glycol)-sidechain microgels prepared in absence of cross-linking agent: Polymerization, characterization and variation of particle deformability.

    Science.gov (United States)

    Welsch, Nicole; Lyon, L Andrew

    2017-01-01

    We present a systematic study of self-cross-linked microgels formed by precipitation polymerization of oligo ethylene glycol methacrylates. The cross-linking density of these microgels and, thus, the network flexibility can be easily tuned through the modulation of the reaction temperature during polymerization. Microgels prepared in absence of any difunctional monomer, i.e. cross-linker, show enhanced deformability and particle spreading on solid surfaces as compared to microgels cross-linked with varying amounts of poly(ethylene glycol diacrylate) (PEG-DA) in addition to self-crosslinking. Particles prepared at low reaction temperatures exhibit the highest degree of spreading due to the lightly cross-linked and flexible polymer network. Moreover, AFM force spectroscopy studies suggest that cross-linker-free microgels constitute of a more homogeneous polymer network than PEG-DA cross-linked particles and have elastic moduli at the particle apex that are ~5 times smaller than the moduli of 5 mol-% PEG-DA cross-linked microgels. Resistive pulse sensing experiments demonstrate that microgels prepared at 75 and 80°C without PEG-DA are able to deform significantly to pass through nanopores that are smaller than the microgel size. Additionally, we found that polymer network flexibility of microgels is a useful tool to control the formation of particle dewetting patterns. This offers a promising new avenue for build-up of 2D self-assembled particle structures with patterned chemical and mechanical properties.

  7. Preparation and characterization of oxidized alginate covalently cross-linked galactosylated chitosan scaffold for liver tissue engineering

    Energy Technology Data Exchange (ETDEWEB)

    Chen Feng [College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065 (China); Suzhou Institute of Sichuan University, Suzhou 215123 (China); Tian Meng; Zhang Dongming; Wang Jianyun; Wang Qiguang [College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065 (China); Yu Xixun [College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065 (China); Suzhou Institute of Sichuan University, Suzhou 215123 (China); Zhang Xiaohua [College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065 (China); Wan Changxiu, E-mail: wanchangxiu@163.com [College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065 (China)

    2012-02-01

    Liver tissue engineering (LTE) requires a perfect extracellular matrix (ECM) for hepatocytes culture to maintain high level of liver-specific functions. Here, we reported a LTE scaffold derived from oxidized alginate covalently cross-linked galactosylated chitosan via Schiff base reaction, without employing any extraneous chemical cross-linking agent. The structure of galactosylated chitosan (GC) and oxidized alginate was confirmed by Fourier transformed infrared (FTIR) spectra, proton nuclear magnetic resonance ({sup 1}H-NMR) spectroscopy, X-ray diffraction (XRD) or thermogravimetric (TG) analysis. The structure and properties of a series of the scaffolds were characterized by FTIR, XRD, scanning electron microscopy (SEM), porosity, equilibrium swelling, mechanical properties, thermal stability and in vitro degradation. FTIR spectra confirmed the characteristic peak of Schiff base groups in the scaffolds and XRD indicated the scaffolds could be amorphous. SEM analysis showed that the scaffolds displayed highly porous surfaces with average pore size of 50-150 {mu}m and interconnected pore structure in the internal structure with average pore size of 100-250 {mu}m. Porosity measurement suggested the scaffolds had a porosity of about 70%. The compressive modulus of the scaffolds (hydrated) was in the range of 4.2-6.3 kPa. Further studies showed that, with the increase of the oxidized alginate content, the equilibrium swelling and in vitro degradation rate of the scaffolds decreased and the thermal stability slightly increased, which might mainly attribute to the difference of the degree of cross-linking and the nature properties of the raw materials. Additionally, the biocompatibility of the scaffolds was evaluated in vitro. The results showed that the hepatocytes cultured on the scaffolds had a typical spheroidal morphology, formed multi-cellular aggregates and presented perfect integration with the scaffolds, which suggested that the scaffolds may be potential

  8. Preparation of a Cyclomaltoheptaose (β-cyclodextrin) Cross-linked Chitosan Derivative via Glyoxal or Glutaraldehyde

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A cyclomaltoheptaose-β-cyclodextrin (β-CD) crosslinked chitosan derivative via glyoxal or glutaraldehyde was prepared. The structures of β-CD crosslined chitosan with glyoxal or glutaraldehyde were characterized by IR spectra. The surface morphology of the β-CD crosslinked chitosan particles was examined using a scanning electron microscope. The immobilization capacity of β-CD on chitosan was affected on the weight ratio of β-CD/chitosan, the utilization amount of crosslinking agent, the acidity of the reaction system and the temperature. The adsorption for nicotine indicated that the chitosan-β-CD was a good adsorbent.

  9. Preparation and water absorption of cross-linked chitosan/silk fibroin blend films

    Energy Technology Data Exchange (ETDEWEB)

    Suesat, Jantip; Rujiravanit, Ratana [Chulalongkorn University, The Petroleum and Petrochemical College, Bangkok (Thailand); Jamieson, Alexander M. [Case Western Reserve Univ., Department of Macromolecular Science, Cleveland (United States); Tokura, Seiichi [Kansai Univ., Faculty of Engineering, Osaka (Japan)

    2001-03-01

    Natural polymer blend films composed of chitosan and silk fibroin were prepared by varying the ratio of chitosan to silk fibroin, with and without glutaraldehyde as a crosslinking agent. The effects of the ratio of chitosan to silk fibroin and crosslinking agent on swelling behavior of the blend films were studied. For the swelling behavior, the blend films exhibited a dramatic change in the degree of swelling when immersed in acidic solutions. The degree of swelling of the films increased as the chitosan content increased; the blend film with 80% chitosan content had the maximum degree of swelling. It appeared that crosslinking had occurred in the blend films which helped the films to retain their three dimensional structure. In addition, FTIR spectra of the films showed evidence of hydrogen bonding interaction between chitosan and silk fibroin. For the effect of salt type, the films were immersed in various types of aqueous salt solutions, viz NaCl, LiCl, CaCl{sub 2}, AlCl{sub 3}, and FeCl{sub 3}. The films immersed in AlCl{sub 3} and FeCl{sub 3} aqueous solutions gave the maximum degree of swelling. The effects of AlCl{sub 3} and FeCl{sub 3} concentrations on swelling behavior were also investigated. It was found that the maximum degree of swelling of the films occurred at 1.0 x 10{sup -2} M of AlCl{sub 3} and FeCl{sub 3} aqueous solutions. (author)

  10. Preparation and characterization of cross-linked β-cyclodextrin polymer/Fe3O4 composite nanoparticles with core-shell structures

    Institute of Scientific and Technical Information of China (English)

    Rui Xue Li; Shu Mei Liu; Jian Qing Zhao; Hideyuki Otsuka; Atsushi Takahara

    2011-01-01

    Cross-linked β-cyclodextrin polymer/Fe3O4 composite nanoparticles with core-shell structures were prepared via cross linking reaction on the surface of carboxymethyl β-cyclodextrin (CM-β-CD) modified Fe3O4 nanoparticles in β-cyclodextrin alkaline solution by using epichlorohydrin as crosslinking agent. The morphology, structure and magnetic properties of the prepared composite nanoparticles were investigated by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectrometry, X-ray diffraction (XRD) measurement, thermogravimetric analysis (TGA) and Vibrating sample magnetometry (VSM), respectively.

  11. Cocoa pod husk, a new source of hydrolase enzymes for preparation of cross-linked enzyme aggregate.

    Science.gov (United States)

    Yusof, Faridah; Khanahmadi, Soofia; Amid, Azura; Mahmod, Safa Senan

    2016-01-01

    Cocoa pod husk (CPH) is a by-product of cocoa production obtained after removing the beans from the fruit. The analysis of CPH has shown that it contains high amounts of protein. This study is aimed to utilize this protein source in hydrolase enzyme production. In this study, seven hydrolase enzymes (amylase, fructosyltransferase, mannanase, glucosidase, glucanase, lipase and protease) were screened from CPH for the first time for feasible industrial production. Among these hydrolases, lipase was chosen for the next steps of experiments as it has a lot of applications in different industries. The extraction of high active lipase from CPH has been done under optimum conditions. The condition that was optimum for the three major factors was achieved using Face centered central composite design (FCCCD) with response surface methodology (RSM) to obtain the highest enzyme activity of crude lipase from CPH. The optimum condition of extraction is used for preparation of cross-linked enzyme aggregate (CLEA). For the production of immobilized biocatalyst, the technique of CLEA is considered as an effective technique for its industrially attractive advantages. Referring to the results of OFAT, CLEA-lipase was prepared in the best condition at the presence of 30 mM ammonium sulphate, 70 mM glutaraldehyde with 0.23 mM Bovine serum albumin as an additive. Immobilization effectively improved the stability of lipase against various organic solvents.

  12. Preparation and characterization of stable cross-linked enzyme aggregates of novel laccase enzyme from Shewanella putrefaciens and using malachite green decolorization.

    Science.gov (United States)

    Sinirlioglu, Zeynep Aydin; Sinirlioglu, Deniz; Akbas, Fahri

    2013-10-01

    A novel type laccase from Shewanella putrefaciens was identified, expressed in Escherichia coli, characterized, prepared in cross-linked enzyme aggregates (CLEA) for industrial applications and investigated of decolorization activity on malchite green dye. Enzyme characterization was investigated by enzyme assay, SDS-PAGE and other biochemical reactions. Moreover, cross-linked enzyme aggregates were prepared and characterized. Saturated ammonium sulphate solution was used as the precipitating agent and cross linked with glutaraldehyde. These CLEA-laccase aggregates showed more catalytic efficiency and more stabilities compared to free laccase against harsh conditions of thermal and chemical agents as well as high reusability. Also it showed more decolorization ability. These results suggest that this CLEA is potentially usable in industrial applications. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Preparation of Thermo-Responsive Poly(ionic liquid)s-Based Nanogels via One-Step Cross-Linking Copolymerization.

    Science.gov (United States)

    Zhang, Jing; Liu, Jingjiang; Zuo, Yong; Wang, Rongmin; Xiong, Yubing

    2015-09-18

    In this study, thermo-responsive polymeric nanogels were facilely prepared via one-step cross-linking copolymerization of ethylene glycol dimethacrylate/divinylbenzene and ionic liquid (IL)-based monomers, 1,n-dialkyl-3,3'-bis-1-vinyl imidazolium bromides ([CnVIm]Br; n = 6, 8, 12) in selective solvents. The results revealed that stable and blue opalescent biimidazolium (BIm)-based nanogel solutions could be obtained without any precipitation when the copolymerizations were conducted in methanol. Most importantly, these novel nanogels were thermo-response, and could reversibly transform to precipitation in methanol with temperature changes. Turbidity analysis and dynamic light scatting (DLS) measurement illustrated that PIL-based nanogel solutions presented the phase transform with upper critical solution temperature (UCST) in the range of 5-25 °C. The nanogels were characterized using Fourier transform infrared (FTIR), thermogravimetric analyses (TGA), and scanning electron microscopy (SEM). In addition, BIm-based nanogels could also be used as highly active catalysts in the cycloaddition reaction of CO₂ and epoxides. As a result, our attributes build a robust platform suitable for the preparation of polymeric nanomaterials, as well as CO₂ conversion.

  14. Preparation and Characterization of Epoxy Resin Cross-Linked with High Wood Pyrolysis Bio-Oil Substitution by Acetone Pretreatment

    Directory of Open Access Journals (Sweden)

    Yi Liu

    2017-03-01

    Full Text Available The use of cost effective solvents may be necessary to store wood pyrolysis bio-oil in order to stabilize and control its viscosity, but this part of the production system has not been explored. Conversely, any rise in viscosity during storage, that would occur without a solvent, will add variance to the production system and render it cost ineffective. The purpose of this study was to modify bio-oil with a common solvent and then react the bio-oil with an epoxy for bonding of wood without any loss in properties. The acetone pretreatment of the bio-oil/epoxy mixture was found to improve the cross-linking potential and substitution rate based on its mechanical, chemical, and thermal properties. Specifically, the bio-oil was blended with epoxy resin at weight ratios ranging from 2:1 to 1:5 and were then cured. A higher bio-oil substitution rate was found to lower the shear bond strength of the bio-oil/epoxy resins. However, when an acetone pretreatment was used, it was possible to replace the bio-oil by as much as 50% while satisfying usage requirements. Extraction of the bio-oil/epoxy mixture with four different solvents demonstrated an improvement in cross-linking after acetone pretreatment. ATR-FTIR analysis confirmed that the polymer achieved a higher cross-linked structure. DSC and TGA curves showed improved thermal stability with the addition of the acetone pretreatment. UV-Vis characterization showed that some functional groups of the bio-oil to epoxy system were unreacted. Finally, when the resin mixture was utilized to bond wood, the acetone pretreatment coupled with precise tuning of the bio-oil:epoxy ratio was an effective method to control cross-linking while ensuring acceptable bond strength.

  15. Preparation and characterization of a micro-porous polymer electrolyte with cross-linking network structure for dye-sensitized solar cell

    Energy Technology Data Exchange (ETDEWEB)

    Wei, T.C.; Wan, C.C.; Wang, Y.Y. [Department of Chemical Engineering, National Tsing-Hua University, 101, Section 2, Kuang Fu Road, Hsin-Chu 300 (China)

    2007-12-14

    A PVdF-HFP/PEG/PEGDMA cross-linking film has been prepared as the electrolyte for dye-sensitized solar cell (DSSC). The film can be made porous by controlling the evaporation behavior of solvents. Room temperature ionic conductivity of the micro-porous film exceeds 1 mS/cm. In addition, we also evaluated the significance of cell gap in DSSC by analyzing the impedance spectroscopy of the cell with polymer electrolyte. Finally, by decreasing the film thickness, the DSSC equipped with 11 {mu}m, micro-porous and cross-linked film showed a conversion efficiency over 4% and 5% under 1 and 0.16 Sun, respectively. (author)

  16. Preparation and properties of gel membrane containing porous PVDF-HFP matrix and cross-linked PEG for lithium ion conduction

    Institute of Scientific and Technical Information of China (English)

    Mei ZHANG; Aiqing ZHANG; Zhenyu CUI; Baoku ZHU; Gaigc HAN; Youyi XU

    2008-01-01

    Lithium ion conducting membranes are the key materials for lithium batteries. The lithium ion conducting gel polymer electrolyte membrane (Li-GPEM) based on porous poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) matrix and cross-linked PEG network is pre-pared by a typical phase inversion process. By immersing the porous PVDF-HFP membrane in liquid electrolyte con-taining poly(ethylene glycol) diacrylate (PEGDA) and an initiator to absorb the liquid electrolyte at 25℃, and then thermally cross-linking at 60℃, the Li-GPEM is fabricated successfully. The measurements on its weight loss, mech-anical and electrochemical properties reveal that the obtained Li-GPEM has better overall performance than the liquid and blend gel systems used as conductive media in lithium batteries. The ionic conductivity of the fabricated Li-GPEM can reach as high as 2.25 × 10-3S/cm at 25℃.

  17. Preparation of cross-linked lipase-coated micro-crystals for biodiesel production from waste cooking oil.

    Science.gov (United States)

    Yan, Jinyong; Yan, Yunjun; Liu, Sanxiong; Hu, Jiang; Wang, Guilong

    2011-04-01

    A dual modification procedure composed of cross-linking and protein coating with K(2)SO(4) was employed to modify Geotrichum sp. lipase for catalyzing biodiesel production from waste cooking oil. Compared to single modification of protein coating with K(2)SO(4), the dual modification of cross-linking and lipase coating improved catalytic properties in terms of thermostable stability, organic solvent tolerance, pH stability and operational stability in biodiesel production process, although biodiesel yield and initial reaction rate for CLPCMCs were not improved. After five successive batch reactions, CLPCMCs could still maintain 80% of relative biodiesel yield. CLPCMCs retained 64% of relative biodiesel yield after incubation in a pH range of 4-6 for 4 h, and 85% of relative biodiesel yield after incubation in a range of 45-50 °C for 4 h. CLPCMCs still maintained 83% of relative biodiesel yield after both treated in polar organic solvent and non-polar organic solvent for 4 h.

  18. Effect of Cross-Linking on the Structure and Growth of Polymer Films Prepared by Interfacial Polymerization.

    Science.gov (United States)

    Berezkin, Anatoly V; Kudryavtsev, Yaroslav V

    2015-11-10

    Interfacial polymerization of tri- and bifunctional monomers (A3B2 polymerization) is investigated by dissipative particle dynamics to reveal an effect of cross-linking on the reaction kinetics and structure of the growing polymer film. Regardless of the comonomer reactivity and miscibility, the kinetics in an initially bilayer melt passes from the reaction to diffusion control. Within the crossover period, branched macromolecules undergo gelation, which drastically changes the scenario of the polymerization process. Comparison with the previously studied linear interfacial polymerization (Berezkin, A. V.; Kudryavtsev, Y. V. Linear Interfacial Polymerization: Theory and Simulations with Dissipative Particle Dynamics J. Chem. Phys. 2014, 141, 194906) shows similar conversion rates but very different product characteristics. Cross-linked polymer films are markedly heterogeneous in density, their average polymerization degree grows with the comonomer miscibility, and end groups are mostly trapped deeply in the film core. Products of linear interfacial polymerization demonstrate opposite trends as they are spontaneously homogenized by a convective flow of macromolecules expelled from the reactive zone to the film periphery, which we call the reactive extrusion effect and which is hampered in branched polymerization. Influence of the comonomer architecture on the polymer film characteristics could be used in various practical applications of interfacial polymerization, such as fabrication of membranes, micro- and nanocapsules and 3D printing.

  19. Preparation of guar gum scaffold film grafted with ethylenediamine and fish scale collagen, cross-linked with ceftazidime for wound healing application.

    Science.gov (United States)

    Jana, Piyali; Mitra, Tapas; Selvaraj, Thirupathi Kumara Raja; Gnanamani, A; Kundu, P P

    2016-11-20

    Present study describes the synthesis of carboxymethyl guar gum (CMGG) from the native guar gum (GG) and the prepared CMGG is grafted with ethylenediamine (EDA) to form aminated CMGG. Then, fish scale collagen and aminated CMGG are cross-linked by ceftazidime drug through non- covalent ionic interaction. The resultant cross-linked film is subjected to the analysis of (1)HNMR, ATR-FTIR, TGA, SEM and XRD. The TNBS results revealed that 45% of interaction between EDA and CMGG and 90-95% of Ceftazidime is released from aminated CMGG-Ceftazidime-Collagen (ACCC) film after 96h of incubation at physiological pH. In vitro cell line studies reveal the biocompatibility of the cross-linked film and the antimicrobial studies display the growth inhibition against Staphylococcus aureus and Pseudomonas aeruginosa organisms. Overall, the study indicates that the incorporation of Ceftazidime into collagen and aminated CMGG can improve the functional property of aminated CMGG as well as collagen, leading to its biomedical applications.

  20. Preparation and Characterization of Polyurethanes with Cross-Linked Siloxane in the Side Chain by Sol-Gel Reactions

    Science.gov (United States)

    Zhao, Hui; Hao, Tong-Hui; Hu, Guo-Hua; Shi, Dean; Huang, Da; Jiang, Tao; Zhang, Qun-Chao

    2017-01-01

    A series of novel polyurethanes containing cross-linked siloxane in the side chain (SPU) were successfully synthesized through a sol-gel process. The SPU was composed of 0%–20% N-(n-butyl)-3-aminopropyltriethoxysilane (HDI-T) modified hexamethylene diisocynate homopolymer. The effects of HDI-T content on both the structure and properties of SPU were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), mechanical properties tests, gel content test, water contact angle measurement and water absorption test. FT-IR, XPS and XRD results confirmed the successful incorporation of HDI-T onto polyurethanes and the formation of Si–O–Si. The surface roughness and the Si content of SPU enhanced with the increase of HDI-T content. Both crystallization and melting temperature shifted to a lower point after the incorporation of HDI-T. The hydrophobicity, tensile strength, Young’s modulus and pencil hardness overall increased with the increasing of HDI-T content, whereas the thermal stability and the elongation at break of SPU slightly decreased. PMID:28772607

  1. Investigation of Genipin Cross-Linked Microcapsule for Oral Delivery of Live Bacterial Cells and Other Biotherapeutics: Preparation and In Vitro Analysis in Simulated Human Gastrointestinal Model

    Directory of Open Access Journals (Sweden)

    Hongmei Chen

    2010-01-01

    Full Text Available Oral therapy utilizing engineered microorganisms has shown promise in the treatment of many diseases. By microencapsulation, viable cells can overcome the harsh gastrointestinal (GI environment and secrete needed therapeutics into the gut. These engineered cells should be encased without escaping into the GI tract for safety concerns, thus robust microcapsule membrane is requisite. This paper examined the GI performance of a novel microcapsule membrane using a dynamic simulated human GI model. Results showed that the genipin cross-linked alginate-chitosan (GCAC microcapsules possessed strong resistance to structural disintegration in the simulated GI environment. Leakage of encapsulated high molecular weight dextran, a model material to be protected during the simulated GI transit, was negligible over 72 h of exposure, in contrast to considerable leakage of dextran from the non-cross-linked counterparts. These microcapsules did not alter the microflora and enzymatic activities in the simulated human colonic media. This study suggested the potential of the GCAC microcapsules for oral delivery of live microorganisms and other biotherapeutics.

  2. Preparation of cross-linked magnetic chitosan-phenylthiourea resin for adsorption of Hg(II), Cd(II) and Zn(II) ions from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Monier, M., E-mail: monierchem@yahoo.com [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt); Abdel-Latif, D.A. [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt)

    2012-03-30

    Highlights: Black-Right-Pointing-Pointer Chitosan was chemically modified through the reaction with phenylisothiocyanate. Black-Right-Pointing-Pointer The modified chitosan-phenylthiourea cross-linked with formaldehyde in presence of magnetite to produce modified magnetic resin. Black-Right-Pointing-Pointer The resulted resin characterized by various instrumental methods. Black-Right-Pointing-Pointer The resin was applied to remove Hg{sup 2+}, Cd{sup 2+} and Zn{sup 2+} from aqueous solutions. - Abstract: In this study, cross-linked magnetic chitosan-phenylthiourea (CSTU) resin were prepared and characterized by means of FTIR, {sup 1}H NMR, SEM high-angle X-ray diffraction (XRD), magnetic properties and thermogravimetric analysis (TGA). The prepared resin were used to investigate the adsorption properties of Hg(II), Cd(II) and Zn(II) metal ions in an aqueous solution. The extent of adsorption was investigated as a function of pH and the metal ion removal reached maximum at pH 5.0. Also, the kinetic and thermodynamic parameters of the adsorption process were estimated. These data indicated that the adsorption process is exothermic and followed the pseudo-second-order kinetics. Equilibrium studies showed that the data of Hg(II), Cd(II) and Zn(II) adsorption followed the Langmuir model. The maximum adsorption capacities for Hg(II), Cd(II) and Zn(II) were estimated to be 135 {+-} 3, 120 {+-} 1 and 52 {+-} 1 mg/g, which demonstrated the high adsorption efficiency of CSTU toward the studied metal ions.

  3. Preparation of γ-aminopropyltriethoxysilane cross-linked poly(aspartic acid) superabsorbent hydrogels without organic solvent.

    Science.gov (United States)

    Meng, Hongyu; Zhang, Xin; Sun, Shenyu; Tan, Tianwei; Cao, Hui

    2016-01-01

    Poly(aspartic acid) (PASP) hydrogel is a type of biodegradable and biocompatible polymer with high water absorbing ability. Traditionally, the production of PASP hydrogel is expensive, complex, environmentally unfriendly, and consumes a large amount of organic solvents, e.g. dimethylformamide or dimethylsulfoxide. This study introduces a one-step synthesis of PASP resin, in which the organic phase was replaced by distilled water and γ-aminopropyltriethoxysilane was used as the cross-linker. Absorbent ability and characteristics were determined by swelling ratio, FTIR, (13)C SSNMR, and SEM. In vitro cytotoxicity evaluation and animal skin irritation tests showed the hydrogel has body-friendly properties. Preparing PASP hydrogel in aqueous solution is promising and finds its use in many applications.

  4. Preparation of Rigid Cross-Linking PVC Foam Plastics%硬质交联PVC泡沫塑料的制备

    Institute of Scientific and Technical Information of China (English)

    王雁国; 汪艳; 张慧

    2014-01-01

    Based on polyvinyl chloride(PVC) resin,rigid cross-linking PVC foam plastics with special performance were prepared by isocyanate and melamine which were used as the cross-linking agent and maleic anhydride which was used as the grafting agent. It is confirmed that the cross-linking reaction happen in the boiling process phase by infrared spectrum analysis, thermal gravimetric analysis,thermal mechanical analysis and gel content measurement. It also shows that the glass transition temperature of the foam plastics is at about 180℃. Dosage of maleic anhydride was studied on the influence of the gel content of the foam plastics,the amount of maleic anhydride has less effect on the degree of cross-linking in plasticization and molding phase and the gel content of the foam plastics is increased with the increase of dosage of maleic anhydride. Bubble pore diameter were measured by optical microscope. It shows that the distribution of bubble pore diameter are homogeneous,the bubble pore diameter of the foam plastics for the density of 60 kg/m3 are mainly distributed in 100~130 μm and the density of 90 kg/m3 are mainly distributed in 70~80 μm. By the determination of the mechanical properties of the foam plastics,it shows that the foam plastics has the same mechanical properties as the Swiss Airex C70 products.%以聚氯乙烯(PVC)为基体,马来酸酐为接枝剂,异氰酸酯、三聚氰胺为交联剂,制备出性能优异的硬质交联PVC泡沫塑料;通过红外光谱、热失重和热机械分析及凝胶含量测定对硬质交联PVC泡沫塑料进行分析,证实交联反应发生在水煮工艺阶段,玻璃化转变温度在180℃左右;研究了马来酸酐用量对硬质交联PVC泡沫塑料凝胶含量的影响,马来酸酐的用量在塑化成型阶段对交联度的影响较小,硬质交联PVC泡沫塑料的凝胶含量随着马来酸酐用量的增加而增大;用光学显微镜对硬质交联PVC泡沫塑料的泡孔直径进行了

  5. Preparation of chitosan from the shrimp shells and its application for pre-concentration of uranium after cross-linking with epichlorohydrin

    Directory of Open Access Journals (Sweden)

    Ahmed M. Motawie

    2014-06-01

    Full Text Available Chitosan (CTS was first prepared by proper treatment of shrimp shells and the cross-linked chitosan (CCTS was then synthesized by its reaction with epichlorohydrin (ECH under alkaline conditions. Adsorption of uranium from aqueous nitrate solution onto CCTS was investigated batch wise. The adsorption isotherm and the adsorption kinetic as well as thermodynamic studies of this adsorption are carried out. The influence factors on uranium (VI adsorption were optimized and were found to include an initial pH of 3 and a contact time of 120 min. The Langmuir adsorption model was then applied for the mathematical description of the obtained adsorption equilibrium and where its data greatly agree with that model and where the maximum adsorption capacity was estimated to be 903 mg/g. Adsorption kinetics data were also tested using pseudo-first-order and pseudo-second-order models and where the studied adsorption followed the latter. In addition, determination of the thermodynamic parameters (ΔG°, ΔH° and ΔS° using van’t Hoff equation has indicated that the prepared CCTS can conveniently be used for uranium adsorption from its aqueous solution.

  6. Preparation of cross-linked magnetic chitosan-phenylthiourea resin for adsorption of Hg(II), Cd(II) and Zn(II) ions from aqueous solutions.

    Science.gov (United States)

    Monier, M; Abdel-Latif, D A

    2012-03-30

    In this study, cross-linked magnetic chitosan-phenylthiourea (CSTU) resin were prepared and characterized by means of FTIR, (1)H NMR, SEM high-angle X-ray diffraction (XRD), magnetic properties and thermogravimetric analysis (TGA). The prepared resin were used to investigate the adsorption properties of Hg(II), Cd(II) and Zn(II) metal ions in an aqueous solution. The extent of adsorption was investigated as a function of pH and the metal ion removal reached maximum at pH 5.0. Also, the kinetic and thermodynamic parameters of the adsorption process were estimated. These data indicated that the adsorption process is exothermic and followed the pseudo-second-order kinetics. Equilibrium studies showed that the data of Hg(II), Cd(II) and Zn(II) adsorption followed the Langmuir model. The maximum adsorption capacities for Hg(II), Cd(II) and Zn(II) were estimated to be 135 ± 3, 120 ± 1 and 52 ± 1 mg/g, which demonstrated the high adsorption efficiency of CSTU toward the studied metal ions.

  7. Study on preparation of cross-linked carboxymethyl guar gum%交联羧甲基瓜尔胶的制备

    Institute of Scientific and Technical Information of China (English)

    陈娜丽; 冯辉霞; 赵霞; 张娟

    2011-01-01

    以植物瓜尔胶为原料、环氧氯丙烷为交联剂、氨乙酸为羧甲基化试剂,制备了交联羧甲基瓜尔胶。研究了环氧氯丙烷的用量、氯乙酸的用量、氢氧化钠的用量及反应温度对产品取代度的影响;考查了产品糊的耐温性能,并用FT—IR对产品的结构进行了表征。实验结果表明:配料质量比瓜尔胶:环氧氯丙烷:氢氧化钠:氯乙酸为1.00:0.015:0.45:0.40,反应温度50℃时,产品的取代度达最高0.340。FT-IR分析结果表明,瓜尔胶分子中引入了羧甲基基团,交联羧甲基瓜尔胶成功制备。与原瓜尔胶糊相比,产品糊的耐温性能得到改善。%With natural guar gum as material,epichlorohydrin as cross-linking agent,chloroacetic acid as carboxymethylating agent,cross-linked carboxymethyl guar gum was prepared. The effects of epichlorohydrin dosage,chloroacetic acid dosage,sodium hydroxide dosage,and reaction temperature on the degree of substitution of product were studied. The temperature resistance of product paste was also investigated. The maximum degree of substitution of product of 0.340 was obtained under the following conditions: the mass ratio of guar gum :epichlorohydrin :sodium hydroxide :chloroacetic acid 1.00:0.015:0.45:0.40,reaction temperature 50℃. The FT-IR results showed that the group of carboxymethyl had introduced to the product,and crosslinked carboxymethyl guar gum was successfully prepared. Product paste had improved temperature resistance in contrast to native guar gum paste.

  8. Cross-link guided molecular modeling with ROSETTA.

    Directory of Open Access Journals (Sweden)

    Abdullah Kahraman

    Full Text Available Chemical cross-links identified by mass spectrometry generate distance restraints that reveal low-resolution structural information on proteins and protein complexes. The technology to reliably generate such data has become mature and robust enough to shift the focus to the question of how these distance restraints can be best integrated into molecular modeling calculations. Here, we introduce three workflows for incorporating distance restraints generated by chemical cross-linking and mass spectrometry into ROSETTA protocols for comparative and de novo modeling and protein-protein docking. We demonstrate that the cross-link validation and visualization software Xwalk facilitates successful cross-link data integration. Besides the protocols we introduce XLdb, a database of chemical cross-links from 14 different publications with 506 intra-protein and 62 inter-protein cross-links, where each cross-link can be mapped on an experimental structure from the Protein Data Bank. Finally, we demonstrate on a protein-protein docking reference data set the impact of virtual cross-links on protein docking calculations and show that an inter-protein cross-link can reduce on average the RMSD of a docking prediction by 5.0 Å. The methods and results presented here provide guidelines for the effective integration of chemical cross-link data in molecular modeling calculations and should advance the structural analysis of particularly large and transient protein complexes via hybrid structural biology methods.

  9. Preparation and characterization of a magneto-polymeric nanocomposite: Fe{sub 3}O{sub 4} nanoparticles in a grafted, cross-linked and plasticized poly(vinyl chloride) matrix

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez-Fernandez, Oliverio S. [Centro de Investigacion en Quimica Aplicada, Boulevard Enrique Reyna Hermosillo No. 140, Saltillo, Coahuila Mexico, C.P. 25253 (Mexico)], E-mail: oliverio@ciqa.mx; Rodriguez-Calzadiaz, C.A.; Yanez-Flores, Isaura G.; Montemayor, Sagrario M. [Centro de Investigacion en Quimica Aplicada, Boulevard Enrique Reyna Hermosillo No. 140, Saltillo, Coahuila Mexico, C.P. 25253 (Mexico)

    2008-07-15

    In this work two kind of materials: (1) grafted, cross-linked and plasticized poly(vinyl chloride) (PVC) 'plastic films' and (2) magnetic plastic films 'magneto-polymeric nanocomposites' were prepared. Precursor solutions or 'plastisols' used to obtain the plastic films were obtained by mixing PVC (emulsion grade) as polymeric matrix, di(2-ethylhexyl)phthalate (DOP) as plasticizer, a thermal stabilizer based in Ca/Zn salts, and a cross-linking agent, 3-mercaptopropyltrimethoxysilane (MTMS) or 3-aminopropyltriethoxysilane (ATES), at several concentrations. Flexible films were obtained from the plastisols using static casting. The stress-strain behavior and the gel content (determined by Soxhlet extraction with boiling THF) of the flexible films were measured in order to evaluate the effect of the cross-linking agent and their content on the degree of cross-linking. The magneto-polymeric nanocomposites were obtained by mixing the optimum composition of the plastisols (analyzed previously) with magnetite (Fe{sub 3}O{sub 4})-based ferrofluid and DOP. Later, flexible films were obtained by static casting of the plastisol/ferrofluid systems. The magnetic films were characterized by the above-mentioned techniques and X-ray diffraction, vibrating sample magnetometry and thermogravimetrical analy0009s.

  10. Study on Preparation and Properties of Cross-Linking and Esterifying Starch of Mechanical Activated Cassava Starch%机械活化木薯交联酯化淀粉的制备及其性能研究

    Institute of Scientific and Technical Information of China (English)

    陈渊; 杨家添; 谢祖芳; 谭义秋; 黄祖强; 周琴

    2012-01-01

    Cross - linking and esterifying starch of mechanical activated cassava starch was prepared by using mechanical activated cassava starch as raw material, and using sodium trimetaphosophate for cross - linking agent and acetic anhydride for acetification, which its synthesis route prepared by continual reactions in one - step synthesis way. The effects of reaction temerature, cross - linking agent and esterifying agent dosage, pH value of cross — linking and esterifying and cross - linking time on the cold viscosity of cross - linking and esterifying starch paste were investigated respectively, and the physical and chemical Parameters and structure of the cross - linking and esterifying starch with mechanical activated cassava starch and cross - linking and esterifying starch with raw cassava starch were studied. The results indicated that the above reaction conditions were all found to affect the preparation of cross - linking and esterifying mechanical activated cassava starch. Under the reaction temperature 40℃ ,1.0% amounts of sodium trimetaphosphate,crosslinking pH value 10.0,crosslinking time 2. 0 h,acetic anhydride amount 0. 5 mL,esterifying pH value 9.0, esterifying time 60 min, the cold viscosity of cross - linking and esterifying starch paste of mechanical activated cassava was enhanced from 847 mPa. S of cassava starch to 3 225 mPa. S, and the stability, acidity - resistance, staling resistance of the viscosity of starch paste were significantly improved. Cross - linking and esterifying composite modified was propitious to formation of V type crystal starch.%以机械活化木薯淀粉为原料,三偏磷酸钠为交联剂,醋酸酐为酯化剂,采用一步连续法制备机械活化木薯交联酯化淀粉,考察反应温度、交联剂用量、交联pH、交联时间、酯化剂用量、酯化pH、酯化时间等因素对交联酯化淀粉糊冷黏度的影响,并与原木薯淀粉合成的交联酯化淀粉进行比较,研究了产物的理化特性

  11. Preparation of Hydroxypropyl-β-cyclodextrin Cross-linked Multi-walled Carbon Nanotubes and Their Application in Enantioseparation of Clenbuterol

    Institute of Scientific and Technical Information of China (English)

    Yu Jingang; Huang Dushu; Huang Kelong; Hong Yong

    2011-01-01

    A method of cross-linking multi-walled carbon nanotubes by a nucleophilic substitution of brominated multi-walled carbon nanotubes using hydroxypropyl-β-cyclodextrin anions was studied. The modified multi-walled carbon nanotube samples were characterized using thermogravimetric analysis, energy-dispersive X-ray spectros-copy, transmission electron microscopy, scanning electron microscopy, Raman spectroscopy and Fourier transform infrared spectroscopy. The hydroxypropyi-β-cyclodextrin modified multi-walled carbon nanotubes were used as a chiral stationary phase additive for thin-layer chromatography to separate clenbuterol enantiomers, and the chiral separation factor was increased.

  12. 交联青霉素G酰化酶聚集体制备及其催化特性研究%Preparation of Cross-linked Penicillin G Acylase Aggregates and Its Catalytic Property

    Institute of Scientific and Technical Information of China (English)

    程仕伟; 王玉芳; 步长平; 张桂春

    2012-01-01

    目的 考察交联青霉素G酰化酶聚集体催化特性,探讨其应用潜力.方法 以硫酸铵为沉淀剂获得青霉素G酰化酶蛋白沉淀,戊二醛交联沉淀的蛋白质制备交联酶聚集体,在此基础上研究交联酶聚集体的催化特性.结果 交联粪产碱杆菌来源青霉素G酰化酶聚集体的最适反应温度55℃,最适pH 9.0,其酸碱和热稳定性均优于游离酶,重复使用13批次几乎无酶活性丢失,反应20批次后仍有50.9%的活性.结论 交联酶聚集体的稳定性较游离酶好,具有一定的工业应用前景.%Objective Cross-linked enzyme aggregates (CLEA) have more advantages than carrier-bound immobilized enzymes. And this paper explored the potential application of cross-linked aggregates of penicillin G acylase by investigating its catalytic property. Methods The preparation of cross-linked aggregates about penicillin G acylase from Alcaligenes faecalis was as follows: the enzyme was precipitated by ammonium sulfate and then was cross-linked with glutaraldehyde. Furthermore, its catalytic property was studied. Results The optimum reaction temperature and pH of the cross-linked penicillin G acylase aggregates were 55 ℃ and pH9.0. In addition, they had better thermal and pH stability than the free enzyme. The activity hardly lost after 13 cycles, and there was even 50.9% of the enzyme activity after 20 cycles. Conclusion The cross-linked penicillin G acylase aggregates have good operation stability and potential application as an industrial biocatalyst.

  13. Preparation and Cross-Linking of All-Acrylamide Diblock Copolymer Nano-Objects via Polymerization-Induced Self-Assembly in Aqueous Solution

    Science.gov (United States)

    2017-01-01

    Various carboxylic acid-functionalized poly(N,N-dimethylacrylamide) (PDMAC) macromolecular chain transfer agents (macro-CTAs) were chain-extended with diacetone acrylamide (DAAM) by reversible addition–fragmentation chain transfer (RAFT) aqueous dispersion polymerization at 70 °C and 20% w/w solids to produce a series of PDMAC–PDAAM diblock copolymer nano-objects via polymerization-induced self-assembly (PISA). TEM studies indicate that a PDMAC macro-CTA with a mean degree of polymerization (DP) of 68 or higher results in the formation of well-defined spherical nanoparticles with mean diameters ranging from 40 to 150 nm. In contrast, either highly anisotropic worms or polydisperse vesicles are formed when relatively short macro-CTAs (DP = 40–58) are used. A phase diagram was constructed to enable accurate targeting of pure copolymer morphologies. Dynamic light scattering (DLS) and aqueous electrophoresis studies indicated that in most cases these PDMAC–PDAAM nano-objects are surprisingly resistant to changes in either solution pH or temperature. However, PDMAC40–PDAAM99 worms do undergo partial dissociation to form a mixture of relatively short worms and spheres on adjusting the solution pH from pH 2–3 to around pH 9 at 20 °C. Moreover, a change in copolymer morphology from worms to a mixture of short worms and vesicles was observed by DLS and TEM on heating this worm dispersion to 50 °C. Postpolymerization cross-linking of concentrated aqueous dispersions of PDMAC–PDAAM spheres, worms, or vesicles was performed at ambient temperature using adipic acid dihydrazide (ADH), which reacts with the hydrophobic ketone-functionalized PDAAM chains. The formation of hydrazone groups was monitored by FT-IR spectroscopy and afforded covalently stabilized nano-objects that remained intact on exposure to methanol, which is a good solvent for both blocks. Rheological studies indicated that the cross-linked worms formed a stronger gel compared to linear precursor

  14. Preparation of a Xanthine Sensor Based on the Immobilization of Xanthine Oxidase on a Chitosan Modified Electrode by Cross-linking

    Institute of Scientific and Technical Information of China (English)

    刘玉革; 李伟明; 魏长宾; 吕玲玲

    2012-01-01

    Here in this paper, xanthine oxidase (XOD) was immobilized onto the chitosan (CHT) modified electrode by a simple way of cross-linking with glutaraldehyde (GTD) and 3-aminopropyltriethoxysilane (KH). The electrode displayed a sharp peak to the oxidation of xanthine at a potential about 0.67 V and the optimum of pH for determination was investigated. Under the optimum conditions, the biosensor fabricated on the KH/GTD/XOD/CHT modified electrode showed excellent response to the oxidation of xanthine within the range of 0.5 to 18 μmol/L with a low detection limit of 0.0215 μmol/L, a good stability and a high selectivity. The sensor can also be used for the determination of hypoxantbine. The electrochemical results indicated that the immobilized enzyme still retained its biological activity and this provided a new way for the construction of biosensors and determination of xanthine.

  15. Preparation and characterization of cross-linking PEG/MDI/PE copolymer as solid-solid phase change heat storage material

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wei-Dong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Ding, En-Yong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China)

    2007-05-23

    Phase change materials (PCMs) are a series of functional materials with storing and releasing energy properties. PCMs can impact small environment around them through storing and releasing energy during phase change process. Phase change latent heat of PCMs has two main characters: one is high enthalpy and capacity of per unit volume and the other is that the temperature over phase change process keeps constant or changes slightly. PCMs have been widely used in lots of fields such as solar energy storing, smart housing, thermo-regulated fibers and agricultural greenhouse. In this article, a novel solid-solid phase change heat storage material was synthesized via the two-step condensation reaction of high molecule weight polyethylene glycol (PEG10000) with pentaerythritol (PE) and 4,4'-diphenylmethane diisocyanate (MDI). To characterize the resulting product in comparison with pristine PEG10000, Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA), polarization optical microscopy (POM) and wide-angle X-ray diffraction (WAXD) measurements were employed to investigate their ingredients, thermal properties and crystalline behaviors. The results indicated that the cross-linking PCM showed typical solid-solid phase transition property, and its phase change enthalpy and crystallinity reached 152.97 kJ/kg and 81.76%, respectively. (author)

  16. Collagen cross linking: Current perspectives

    Directory of Open Access Journals (Sweden)

    Srinivas K Rao

    2013-01-01

    Full Text Available Keratoconus is a common ectatic disorder occurring in more than 1 in 1,000 individuals. The condition typically starts in adolescence and early adulthood. It is a disease with an uncertain cause and its progression is unpredictable, but in extreme cases, vision deteriorates and can require corneal transplant surgery. Corneal collagen cross-linking (CCL with riboflavin (C3R is a recent treatment option that can enhance the rigidity of the cornea and prevent disease progression. Since its inception, the procedure has evolved with newer instrumentation, surgical techniques, and is also now performed for expanded indications other than keratoconus. With increasing experience, newer guidelines regarding optimization of patient selection, the spectrum of complications and their management, and combination procedures are being described. This article in conjunction with the others in this issue, will try and explore the uses of collagen cross-linking (CXL in its current form.

  17. 交联明胶为壁材制备复合维生素微胶囊%Preparation of Compound Vitamin Microcapsules Using Cross-linked Gelatin as Wall Material

    Institute of Scientific and Technical Information of China (English)

    井乐刚; 赵新淮

    2013-01-01

    目的 研究以交联明胶为壁材的复合维生素微胶囊的制备工艺及体外释放行为.方法 在过氧化氢存在下,以阿魏酸为交联剂,通过辣根过氧化物酶催化,制备交联明胶,考察反应条件对交联度的影响;然后以交联明胶为壁材,以盐酸硫胺素(维生素B1)、核黄素(维生素B2)、盐酸吡哆醇(维生素B6)、叶酸、烟酰胺的混合物为芯材,采用喷雾干燥工艺,按不同壁材/芯材比,制备复合维生素微胶囊.用扫描电镜和激光粒度仪,对微胶囊进行了表征.用荧光分光光度计,对微胶囊的包埋率、荷载量以及在模拟胃液和模拟肠液中的释放行为,进行了测试和分析.结果 在温度为40℃、pH值为8.0、明胶浓度为9%(W/V)、阿魏酸浓度为40 mmol·L-1、交联时间为24 h的反应条件下,交联明胶的交联度较高,达到10%.以此交联明胶为壁材制备的微胶囊,其中维生素的包埋率在85%以上;少数呈表面光滑的圆球形,大多数表面有凹陷;平均粒径为15.27 μm;当壁材/芯材为10/1(W/W)时,维生素在模拟胃液和模拟肠液中完全释放的时间,分别为30和16 min,都比明胶为壁材时相应延长.结论 以交联明胶为壁材,采用喷雾干燥工艺,可以制备出包埋率高、具有一定的缓释性能的复合维生素微胶囊.%OBJECTIVE To study the preparation and in vitro release profile of compound vitamin microencapsules using crosslinked gelatin as wall material.METHODS At the presence of hydrogen peroxide,the cross-linked gelatin was prepared with ferulic acid as the cross-linking agent.During this reaction,horseradish peroxidase was used as the catalyst.Influences of reaction conditions on the cross-linking degree were investigated.Compound vitamin microcapsules were prepared by spray-drying technique using the obtained cross-linked gelatin as wall material.The core material was the mixture of thiamine hydrochloride (vitamin B1),riboflavin (vitamin B2

  18. Long term in vivo degradation and tissue response to photo-cross-linked elastomers prepared from star-shaped prepolymers of poly(epsilon-caprolactone-co-D,L-lactide).

    Science.gov (United States)

    Chapanian, Rafi; Tse, Man Y; Pang, Stephen C; Amsden, Brian G

    2010-03-01

    Long term in vivo degradation, and tissue response to, cylindrical elastomers made of photo-cross-linked star-poly(epsilon-caprolactone-co-D,L-lactide) triacrylate were investigated through subcutaneous implantation in rats. The elastomers were prepared via UV initiated crosslinking of prepolymers of equimolar amounts of monomers; a high crosslink density elastomer (ELAST 1250) was prepared from a prepolymer of 1250 Da and a low crosslink density elastomer (ELAST 7800) was prepared from a prepolymer of 7800 Da. The elastomers were characterized using cross-polarization magic angle spinning solid state (13)C NMR and attenuated total reflectance fourier transform infrared spectroscopy. The progress of the in vivo degradation process was followed by employing SEM, uniaxial tensile, mass loss, water uptake, and sol content measurements. The rate of in vivo degradation was faster than the rate of in vitro degradation for both ELAST 1250 and ELAST 7800. Long term in vivo degradation studies indicated that both elastomers undergo bulk hydrolysis along with surface erosion occurring due to the physiological environment. In the case of low cross-link density elastomers, the onset of mass loss was accompanied with an increase in both water uptake and sol content, whereas, in the case of high crosslink density elastomers, only the water uptake increased. This degradation pattern was due to crazing of the high crosslink density elastomers. ELAST 7800 cylinders were totally degraded, and ELAST 1250 cylinders had lost 80% of their mass, within 30 weeks. Aminor host reaction with minimal vascularity and inflammation was invoked, with a milder tissue response observed with more highly crosslinked cylinders.

  19. Electrospinning formaldehyde cross-linked zein solutions

    Science.gov (United States)

    In order to develop zein fibers with improved physical properties and solvent resistance, formaldehyde was used as the cross-linking reagent before spinning. The cross-linking reaction was carried out in either acetic acid or ethanolic-HCl where the amount of cross-linking reagent was between 1 and...

  20. Immobilization of 5-aminopyridine-2-tetrazole on cross-linked polystyrene for the preparation of a new adsorbent to remove heavy metal ions from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yu; Chen, Youning; Wang, Chaozhan; Wei, Yinmao, E-mail: ymwei@nwu.edu.cn

    2014-07-15

    Highlights: • Novel chelating resin was prepared using pyridine-2-tetrazole as ligand. • The resin has quite high adsorption capacity for Cu(II), Pb(II) and Hg(II). • The resin shows the different selectivity from the common used IDA resin. • The preparation procedure is a two-step reaction and is easy to carry out. - Abstract: Novel 5-aminopyridine-2-tetrazole-functionalized polystyrene resin (APTZ-PS) was prepared by anchoring 5-aminopyridine-2-carbonitrile onto chloromethylated polystyrene beads (CMPS) and subsequently using the cyano-tetrazole conversion reaction. The APTZ-PS resin was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and specific surface area and pore size analyses. The adsorption experiments of the prepared resin for heavy metal ions were conducted by batch methods. The effects of the experimental conditions, such as pH, contact time and initial metal ion concentration on the adsorption properties of Cu(II), Pb(II) and Hg(II) were investigated. The results showed that the resin possessed perfect adsorption capacities for Cu(II), Pb(II) and Hg(II), and the selectivity was different from the commonly used iminodiacetic acid-chelating resin. The sorption kinetics of the three metal ions followed the pseudo-second-order equation. The adsorption isotherms for Cu(II) and Pb(II) could be better fitted by the Langmuir model than the Freundlich model, whereas the Freundlich model was the best for the Hg(II) ion. Even after five consecutive adsorption–desorption cycles, no obvious change in the adsorption capacity of the resin was found, which implied that the APTZ-PS resin was suitable for the efficient removal of heavy metal ions from aqueous solution.

  1. 青霉素酰化酶交联酶聚体的制备及热失活动力学%Preparation and Thermal Kinetic Deactivation of Cross-linked Enzyme Aggregates of Penicillin Acylase

    Institute of Scientific and Technical Information of China (English)

    慕洋洋; 甄倩楠; 王梦凡; 齐崴; 苏荣欣; 何志敏

    2014-01-01

    以0.53 g/ mL 硫酸铵为沉淀剂,0.35%(体积分数)戊二醛为交联剂制得青霉素酰化酶交联酶聚体(CLEAs),酶活收率30.1%,其最适温度(57℃)比游离酶提高10℃,最适 pH(10.0)向碱性偏移1.7个单位.对比游离酶及其 CLEAs 的热稳定性和热失活动力学模型发现,游离青霉素酰化酶制成 CLEAs 后,其热失活动力学模型由一步失活转变为连串失活,失活反应活化能由248.8 kJ/ mol 增加至549.2 kJ/ mol,对CLEAs 热稳定性大幅提高的原因进行了解释. CLEAs 重复利用7次后,酶活保留56%以上,具有良好的重复利用性.%Cross-linked enzyme aggregates(CLEAs) is an efficient approach to obtain immobilized enzymes without the use of any pre-existing carriers. The preparation of CLEAs usually consisted of two simple steps:precipitation and cross-linking. In this work, CLEAs of penicillin acylase was preparaed using 50% ammo-nium sulphate solution as precipitant and 0. 35% glutaraldehyde as cross-linking agent. The resulting CLEAs obtained an activity yield of 30. 1% and higher optimal temperature (57 ℃) than free penicillin acylase (47 ℃) as well as an obvious shift of optimal pH from 8. 3 to 10. 0. Moreover, compared with free enzyme, the thermal stability of CLEAs was largely enhanced which facilitated the application of penicillin acylase in high-temperature reaction systems. Based on the thermal deactivation kinetics study, it was found that the deactivation model of penicillin acylase changed from one-step model to serial model through immobilizing as CLEAs. The higher deactivation energy of CLEAs(549. 2 kJ/ mol) than free enzyme(248. 8 kJ/ mol) also ex-plained the excellent stability of CLEAs under high temperature environment. In addition, CLEAs exhibited favorable reusability after using 7 times.

  2. 酯化交联木薯糊精的制备及其在微胶囊中的应用%Preparation of cross-linked and esterified cassava dextrin and its application in power oil microcapsules

    Institute of Scientific and Technical Information of China (English)

    陈倩雯; 郑为完; 刘凡; 高媛媛; 葛辉

    2012-01-01

    为获得新型微胶囊粉末油脂的乳化性壁材,以实验室自制的木薯糊精为原料,三偏磷酸钠(STMP)为交联剂进行交联,再进行辛烯基琥珀酸酯化,合成了酯化交联木薯糊精,并研究了其性质及其在微胶囊粉末油脂中的应用。结果表明,制备的酯化交联木薯糊精具有较低的粘度和良好的乳化性;作为乳化性壁材制备微胶囊粉末油脂时,复原乳状液呈乳白色,粒度分布窄;颗粒呈球状,形态均一;包埋率高达94%以上,表面油含量低,包埋效果良好。%To obtain new wall material used in oil microcapsule,the modified dextrin was prepared firstly by the cross-linking cassava dextrin with sodium trimetaphosphate as the sodium trimetaphosphate agent,and then esterified with octenyl succinic anhydride.The properties and application of cross-linked and OSA cassava dextrin was studied.The results showed that the modified dextrin had a lower viscosity and fine emulsification.The synthesized dextrin esters used as wall material in microcapsulation with an embedding ratio of 94%,which the content of surface oil was low.The reconstituted emulsion of microcapsule displayed a narrow particle size distribution spectrum.Microcapsule particles were spherical,smooth,morphological uniformity.

  3. Preparation of Polyester-Based Metal-Cross Linked Polymeric Composites as Novel Materials Resistant to Bacterial Adhesion and Biofilm Formation

    Directory of Open Access Journals (Sweden)

    Mutasem O. Taha

    2011-01-01

    Full Text Available Bacterial biofilms constitute an extremely resistant form of bacterial colonization with dire health and economical implications. Towards achieving polymeric composites capable of resisting bacterial adhesion and biofilm formation, we prepared five 2,6-pyridinedicarboxylate-based polyesters employing five different diol monomers. The resulting polyesters were complexed with copper (II or silver (I. The new polymers were characterized by proton and carbon nuclear magnetic resonance spectroscopy, inherent viscosity, infrared spectroscopy, differential scanning calorimetry and thermogravimetric analysis. The corresponding metal complexes were characterized by differential scanning calorimery and infrared spectroscopy. The amounts of complexed copper and silver were determined by atomic absorption spectrophotometry. Finally, the resulting composites were tested for their antibacterial potential and were found to effectively resist bacterial attachment and growth.

  4. Anisotropic Thermal Conductivity Measurements on Cross-Linked Polybutadienes in Uniaxial Elongation

    Science.gov (United States)

    Venerus, David C.; Kolev, Dimitre

    2008-07-01

    Cross-linked elastomers have numerous applications including automobiles, sporting goods, and biomedical devices. During both their processing and application, these materials experience large mechanical stresses and thermal gradients. In this study, we investigate the mechanical and thermal transport behavior of cross-linked polybutadienes. These materials have been prepared by cross linking well-entangled polybutadienes using an organic peroxide cross-linking agent at low concentration. Samples obtained after nearly complete conversion of the cross-linking agent, which can be characterized as lightly cross-linked (i.e., more than 10 entanglements per cross-link), were subjected to a series of large strain, uniaxial deformations. Measurements of the tensile stress and two components of the thermal conductivity tensor will be reported as a function of elongation. These data are also used to examine the stress-thermal rule in which the stress and thermal conductivity tensors are linearly related.

  5. Corneal collagen cross-linking

    Directory of Open Access Journals (Sweden)

    Jankov II Mirko

    2010-01-01

    Full Text Available Corneal collagen cross-linking (CXL with riboflavin and ultraviolet-A (UVA is a new technique of corneal tissue strengthening by using riboflavin as a photosensitizer and UVA to increase the formation of intra- and interfibrillar covalent bonds by photosensitized oxidation. Keratocyte apoptosis in the anterior segment of the corneal stroma all the way down to a depth of about 300 microns has been described and a demarcation line between the treated and untreated cornea has been clearly shown. It is important to ensure that the cytotoxic threshold for the endothelium has not been exceeded by strictly respecting the minimal corneal thickness. Confocal microscopy studies show that repopulation of keratocytes is already visible 1 month after the treatment, reaching its pre-operative quantity and quality in terms of functional morphology within 6 months after the treatment. The major indication for the use of CXL is to inhibit the progression of corneal ectasias, such as keratoconus and pellucid marginal degeneration. CXL may also be effective in the treatment and prophylaxis of iatrogenic keratectasia, resulting from excessively aggressive photoablation. This treatment has also been used to treat infectious corneal ulcers with apparent favorable results. Combination with other treatments, such as intracorneal ring segment implantation, limited topography-guided photoablation and conductive keratoplasty have been used with different levels of success.

  6. Morphology, mechanical, cross-linking, thermal, and tribological properties of nitrile and hydrogenated nitrile rubber/multi-walled carbon nanotubes composites prepared by melt compounding: The effect of acrylonitrile content and hydrogenation

    Energy Technology Data Exchange (ETDEWEB)

    Likozar, Blaz, E-mail: blaz.likozar@fkkt.uni-lj.si [Polymer Competence Center Leoben GmbH, Montanuniversitaet Leoben, Roseggerstrasse 12, A-8700 Leoben (Austria); Major, Zoltan, E-mail: zoltan.major@jku.at [Polymer Competence Center Leoben GmbH, Montanuniversitaet Leoben, Roseggerstrasse 12, A-8700 Leoben (Austria)

    2010-11-01

    The purpose of this work was to prepare nanocomposites by mixing multi-walled carbon nanotubes (MWCNT) with nitrile and hydrogenated nitrile elastomers (NBR and HNBR). Utilization of transmission electronic microscopy (TEM), scanning electron microscopy (SEM), and small- and wide-angle X-ray scattering techniques (SAXS and WAXS) for advanced morphology observation of conducting filler-reinforced nitrile and hydrogenated nitrile rubber composites is reported. Principal results were increases in hardness (maximally 97 Shore, type A), elastic modulus (maximally 981 MPa), tensile strength (maximally 27.7 MPa), elongation at break (maximally 216%), cross-link density (maximally 7.94 x 10{sup 28} m{sup -3}), density (maximally 1.16 g cm{sup -3}), and tear strength (11.2 kN m{sup -1}), which were clearly visible at particular acrylonitrile contents both for unhydrogenated and hydrogenated polymers due to enhanced distribution of carbon nanotubes (CNT) and their aggregated particles in the applied rubber matrix. Conclusion was that multi-walled carbon nanotubes improved the performance of nitrile and hydrogenated nitrile rubber nanocomposites prepared by melt compounding.

  7. Morphology, mechanical, cross-linking, thermal, and tribological properties of nitrile and hydrogenated nitrile rubber/multi-walled carbon nanotubes composites prepared by melt compounding: The effect of acrylonitrile content and hydrogenation

    Science.gov (United States)

    Likozar, Blaž; Major, Zoltan

    2010-11-01

    The purpose of this work was to prepare nanocomposites by mixing multi-walled carbon nanotubes (MWCNT) with nitrile and hydrogenated nitrile elastomers (NBR and HNBR). Utilization of transmission electronic microscopy (TEM), scanning electron microscopy (SEM), and small- and wide-angle X-ray scattering techniques (SAXS and WAXS) for advanced morphology observation of conducting filler-reinforced nitrile and hydrogenated nitrile rubber composites is reported. Principal results were increases in hardness (maximally 97 Shore, type A), elastic modulus (maximally 981 MPa), tensile strength (maximally 27.7 MPa), elongation at break (maximally 216%), cross-link density (maximally 7.94 × 1028 m-3), density (maximally 1.16 g cm-3), and tear strength (11.2 kN m-1), which were clearly visible at particular acrylonitrile contents both for unhydrogenated and hydrogenated polymers due to enhanced distribution of carbon nanotubes (CNT) and their aggregated particles in the applied rubber matrix. Conclusion was that multi-walled carbon nanotubes improved the performance of nitrile and hydrogenated nitrile rubber nanocomposites prepared by melt compounding.

  8. 交联羧甲基玉米淀粉和交联酯化木薯淀粉的制备与性质研究%Study on preparation and properties of cross-linked carboxymethyl corn starch and cross-linked esterified cassava starch

    Institute of Scientific and Technical Information of China (English)

    史娟; 杨海涛

    2011-01-01

    The optimum synthesis conditions of the cross-linked carboxymethyl corn starch and cross-linked esterified cassava starch and the key factors affecting the degree of substitution were studied. The physical properties of the two kinds of composite-modified starch, such as freeze-melt stability, light transmissivity, expansibility, were determined. The results showed that the freeze-melt stability, light transmissivity, expansibility of composite-modified starch all improved compared to the n-ative starch,and the cross-linked esterified cassava starch could be used in polluted water with better flocculation effect.%研究了制备交联羧甲基玉米淀粉和交联酯化木薯淀粉的最佳工艺条件及影响取代度的关键因素,并测定了两种复合变性淀粉的冻融稳定性、透光率、膨胀度等特性.结果表明:两种复合变性淀粉的冻融稳定性、膨胀度、透光率等性能均优于原淀粉;交联酯化木薯淀粉具有良好的絮凝效果可用于污水处理.

  9. Hyper-cross-linked, hybrid membranes via interfacial polymerization

    NARCIS (Netherlands)

    Raaijmakers, M.J.T.

    2015-01-01

    Hyper-cross-linked, hybrid membranes consist of covalent networks of alternating organic and inorganic, or biological groups. This thesis reports on the preparation of such hybrid networks via interfacial polymerization. The structure-property relationships of the hybrid networks depend strongly on

  10. Computer simulation of randomly cross-linked polymer networks

    CERN Document Server

    Williams, T P

    2002-01-01

    In this work, Monte Carlo and Stochastic Dynamics computer simulations of mesoscale model randomly cross-linked networks were undertaken. Task parallel implementations of the lattice Monte Carlo Bond Fluctuation model and Kremer-Grest Stochastic Dynamics bead-spring continuum model were designed and used for this purpose. Lattice and continuum precursor melt systems were prepared and then cross-linked to varying degrees. The resultant networks were used to study structural changes during deformation and relaxation dynamics. The effects of a random network topology featuring a polydisperse distribution of strand lengths and an abundance of pendant chain ends, were qualitatively compared to recent published work. A preliminary investigation into the effects of temperature on the structural and dynamical properties was also undertaken. Structural changes during isotropic swelling and uniaxial deformation, revealed a pronounced non-affine deformation dependant on the degree of cross-linking. Fractal heterogeneiti...

  11. 交联酶聚集体与仿生硅化技术结合制备固定化脂肪酶%Preparation of Immobilized Lipase through Combination of Cross-Linked Enzyme Aggregates and Biomimetic Silicification

    Institute of Scientific and Technical Information of China (English)

    姜艳军; 王旗; 王温琴; 周丽亚; 高静

    2012-01-01

    The hybrid biocatalyst was prepared by the combination of cross-linked enzyme aggregates (CLEAs) and biotnimetic silicifica-tion, where the lipase Candida sp. 99-125 was used as model enzyme. The preparation conditions of lipase-CLEAs were optimized and the resulting activity of 771 U/g was obtained. Under the optimum conditions, 75% of the activity recovery was obtained. P/CLEAs was prepared by coprecipitation of lipase with polyethylene-imine (PEI), and the resulting activity was 897 U/g. The activity recovery of P/CLEAs was about 88%. The silica coating was formed on the outside surface of P/CLEAs via the induction of PEI. The resulting Coated-CLEAs showed high reusability. The stability of the Coated-CLEAs, including the resistance to trypsin and organic solvents, was also significantly improved.%将交联酶聚集体(CLEAs)与仿生硅化技术相结合,制备了交联脂肪酶Candida sp.99-125杂化生物催化剂.以京尼平为交联剂,在最佳条件下制得的脂肪酶CLEAs的酶活达771U/g,回收率达75%;保护剂聚乙烯亚胺(PEI)与Candida sp.99-125脂肪酶共沉淀制备P/CLEAs,其酶活达897 U/g,回收率约88%;利用PEI的诱导作用,在P/CLEAs表面形成氧化硅涂层,制得的脂肪酶CLEAs (Coated-CLEAs)显示出良好的稳定性,特别是其抗蛋白酶水解能力、有机溶剂耐受能力、重复使用性能等方面明显提高.

  12. Preparation and Biocompatibility Investigation of the Cross-linked Hyaluronic Gel Film%交联透明质酸凝胶膜的制备及其生物相容性的研究

    Institute of Scientific and Technical Information of China (English)

    陈建英; 宋海波; 贺艳丽; 刘杰

    2009-01-01

    制备交联透明质酸凝胶膜并评价其生物相容性.本研究采用己二酸二酰肼作为交联剂制备交联透明质酸凝胶膜,并采用GB/T16886医疗器械生物学评价标准规定的方法,对凝胶膜进行体外溶血试验、细胞毒性试验、急性毒性试验、眼刺激试验、皮内反应试验、致敏试验以及鼠伤寒沙门氏菌回复突变试验、哺乳动物培养细胞染色体畸变试验和小鼠骨髓嗜多染红细胞微核试验等三项遗传毒性试验.结果表明交联透明质酸凝胶膜无溶血性、无眼刺激作用、无皮内刺激和致敏作用,未见急性毒性反应,细胞毒性0~1级;三项遗传毒性试验均为阴性.交联透明质酸凝胶膜具有良好的生物相容性,是一种理想的医用生物材料.%To prepare and evaluate the biocompatibility of the cross-linked hyaluronic gel film, the studies on its cytotoxicity and hemolysis in vitro, acute systemic toxicity, eye stimulation, subcutaneous reactivity,sensitization and genotoxicity of the gel film were executed in compliance with the methods described in GB/T 16886. The experimental results showed that the gel film had no hemolysis,no acute systemic toxicity,no eye irritation,no subcutaneous reactivity,no sensitization, cytotoxicity was scored 0~1 grade. The negative results in Ames test, mammalian cell chromosome aberration and micronucleus test demonstrated that the gel film had no genotoxicity. It's concluded that the cross-linked hyaluronic gel film has reliable biocompatibility and maybe an ideal biomedical material.

  13. Chemical cross-linking of Chlamydia trachomatis

    DEFF Research Database (Denmark)

    Birkelund, Svend; Lundemose, AG; Christiansen, Gunna

    1988-01-01

    Purified elementary bodies (EBs) of Chlamydia trachomatis serovar L2 were analyzed by chemical cross-linking with disuccinimidyl selenodipropionate. The effect of the cross-linking was analyzed by immunoblotting sodium dodecyl sulfate-polyacrylamide gel electrophoresis-separated components which...

  14. Fabrication of Redox-Responsive Degradable Capsule Particles by a Shell-Selective Photoinduced Cross-Linking Approach from Spherical Polymer Particles.

    Science.gov (United States)

    Kitayama, Yukiya; Takeuchi, Toshifumi

    2017-09-18

    In this study, a fabrication route towards functional capsule particles was successfully developed by means of a self-templating shell-selective cross-linking strategy that enables us to prepare shell-cross-linked hollow polymer particles directly from homogeneous spherical polymer particles. To prepare redox-responsive degradable capsule particles, a newly designed monomer bearing a photoinduced post-cross-linking group (cinnamoyl group) and a redox-environment-responsive cleavable group (disulfide group), N-cinnamoyl-N'-methyacryloylcystamine (MCC), was synthesized. Redox-responsive degradable capsule particles were successfully prepared from homogeneous spherical poly(MCC)-based particles by a self-templating shell-selective photoinduced cross-linking approach. Moreover, the cargo loading capability of the shell-cross-linked hollow particles was confirmed through a solvent exchange procedure using dyes, polymer precursors and anticancer reagents. Furthermore, redox-responsive degradability of the capsule polymer particles was also confirmed by adding a reducing agent for cleavage of the disulfide linkage. We hope that the efficient fabrication route of functional capsule particles directly from spherical polymer particles opens efficient routes for the fabrication of a wide range of capsule particles; in particular, this technique is robust, productive, and facile because neither additional sacrificial template particles nor toxic solvents are required. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. The effect of cross-link distributions in axially-ordered, cross-linked networks

    Science.gov (United States)

    Bennett, C. Brad; Kruczek, James; Rabson, D. A.; Matthews, W. Garrett; Pandit, Sagar A.

    2013-07-01

    Cross-linking between the constituent chains of biopolymers has a marked effect on their materials’ properties. In certain of these materials, such as fibrillar collagen, increases in cross-linking lead to an increase in the melting temperature. Fibrillar collagen is an axially-ordered network of cross-linked polymer chains exhibiting a broadened denaturation transition, which has been explained in terms of the successive denaturation with temperature of multiple species. We model axially-ordered, cross-linked materials as stiff chains with distinct arrangements of cross-link-forming sites. Simulations suggest that systems composed of chains with identical arrangements of cross-link-forming sites exhibit critical behavior. In contrast, systems composed of non-identical chains undergo a crossover. This model suggests that the arrangement of cross-link-forming sites may contribute to the broadening of the denaturation transition in fibrillar collagen.

  16. Fabrication of patterned calcium cross-linked alginate hydrogel films and coatings through reductive cation exchange.

    Science.gov (United States)

    Bruchet, Marion; Melman, Artem

    2015-10-20

    Calcium cross-linked alginate hydrogels are widely used in targeted drug delivery, tissue engineering, wound treatment, and other biomedical applications. We developed a method for preparing homogeneous alginate hydrogels cross-linked with Ca(2+) cations using reductive cation exchange in homogeneous iron(III) cross-linked alginate hydrogels. Treatment of iron(III) cross-linked alginate hydrogels with calcium salts and sodium ascorbate results in reduction of iron(III) cations to iron(II) that are instantaneously replaced with Ca(2+) cations, producing homogeneous ionically cross-linking hydrogels. Alternatively, the cation exchange can be performed by photochemical reduction in the presence of calcium chloride using a sacrificial photoreductant. This approach allows fabrication of patterned calcium alginate hydrogels through photochemical patterning of iron(III) cross-linked alginate hydrogel followed by the photochemical reductive exchange of iron cations to calcium.

  17. Mass spectrometric analysis of a UV-cross-linked protein-DNA complex: tryptophans 54 and 88 of E. coli SSB cross-link to DNA

    DEFF Research Database (Denmark)

    Steen, H; Petersen, J; Mann, M

    2001-01-01

    Protein-nucleic acid complexes are commonly studied by photochemical cross-linking. UV-induced cross-linking of protein to nucleic acid may be followed by structural analysis of the conjugated protein to localize the cross-linked amino acids and thereby identify the nucleic acid binding site. Mass....... coli single-stranded DNA binding protein (SSB) that was UV-cross-linked to a 5-iodouracil containing DNA oligomer. Two methods were optimized to circumvent the need for standard liquid chromatography and gel electrophoresis, thereby dramatically increasing the overall sensitivity of the analysis....... Enzymatic degradation of protein and oligonucleotide was combined with miniaturized sample preparation methods for enrichment and desalting of cross-linked peptide-nucleic acid heteroconjugates from complex mixtures prior to mass spectrometric analysis. Detailed characterization of the peptidic component...

  18. Cross-linking chemistry of squid beak.

    Science.gov (United States)

    Miserez, Ali; Rubin, Daniel; Waite, J Herbert

    2010-12-03

    In stark contrast to most aggressive predators, Dosidicus gigas (jumbo squids) do not use minerals in their powerful mouthparts known as beaks. Their beaks instead consist of a highly sclerotized chitinous composite with incremental hydration from the tip to the base. We previously reported l-3,4-dihydroxyphenylalanine (dopa)-histidine (dopa-His) as an important covalent cross-link providing mechanical strengthening to the beak material. Here, we present a more complete characterization of the sclerotization chemistry and describe additional cross-links from D. gigas beak. All cross-links presented in this report share common building blocks, a family of di-, tri-, and tetra-histidine-catecholic adducts, that were separated by affinity chromatography and high performance liquid chromatography (HPLC) and identified by tandem mass spectroscopy and proton nuclear magnetic resonance ((1)H NMR). The data provide additional insights into the unusually high cross-link density found in mature beaks. Furthermore, we propose both a low molecular weight catechol, and peptidyl-dopa, to be sclerotization agents of squid beak. This appears to represent a new strategy for forming hard tissue in animals. The interplay between covalent cross-linking and dehydration on the graded properties of the beaks is discussed.

  19. Electrochemical Characterization of Ultrathin Cross-Linked Metal Nanoparticle Films.

    Science.gov (United States)

    Han, Chu; Percival, Stephen J; Zhang, Bo

    2016-09-06

    Here we report the preparation, characterization, and electrochemical study of conductive, ultrathin films of cross-linked metal nanoparticles (NPs). Nanoporous films ranging from 40 to 200 nm in thickness composed of gold and platinum NPs of ∼5 nm were fabricated via a powerful layer-by-layer spin coating process. This process allows preparation of uniform NP films as large as 2 × 2 cm(2) with precise control over thickness, structure, and electrochemical and electrocatalytic properties. Gold, platinum, and bimetallic NP films were fabricated and characterized using cyclic voltammetry, scanning electron microscopy, and conductance measurements. Their electrocatalytic activity toward the oxygen reduction reaction (ORR) was investigated. Our results show that the electrochemical activity of such NP films is initially hindered by the presence of dense thiolate cross-linking ligands. Both electrochemical cycling and oxygen plasma cleaning are effective means in restoring their electrochemical activity. Gold NP films have higher electric conductivity than platinum possibly due to more uniform film structure and closer particle-particle distance. The electrochemical and electrocatalytic performance of platinum NP films can be greatly enhanced by the incorporation of gold NPs. This work focuses on electrochemical characterization of cross-linked NP films and demonstrates several unique properties. These include quick and easy preparation, ultrathin and uniform film thickness, tunable structure and composition, and transferability to many other substrates.

  20. Shell and core cross-linked poly(L-lysine)/poly(acrylic acid) complex micelles.

    Science.gov (United States)

    Hsieh, Yi-Hsuan; Hsiao, Yung-Tse; Jan, Jeng-Shiung

    2014-12-21

    We report the versatility of polyion complex (PIC) micelles for the preparation of shell and core cross-linked (SCL and CCL) micelles with their surface properties determined by the constituent polymer composition and cross-linking agent. The negatively and positively charged PIC micelles with their molecular structure and properties depending on the mixing weight percentage and polymer molecular weight were first prepared by mixing the negatively and positively charged polyions, poly(acrylic acid) (PAA) and poly(L-lysine) (PLL). The feasibility of preparing SCL micelles was demonstrated by cross-linking the shell of the negatively and positively charged micelles using cystamine and genipin, respectively. The core of the micelles can be cross-linked by silica deposition to stabilize the assemblies. The shell and/or core cross-linked micelles exhibited excellent colloid stability upon changing solution pH. The drug release from the drug-loaded SCL micelles revealed that the controllable permeability of the SCL micelles can be achieved by tuning the cross-linking degree and the SCL micelles exhibited noticeable pH-responsive behavior with accelerated release under acidic conditions. With the versatility of cross-linking strategies, it is possible to prepare a variety of SCL and CCL micelles from PIC micelles.

  1. Hydrogen peroxide and ferulic acid-mediated oxidative cross-linking ...

    African Journals Online (AJOL)

    STORAGESEVER

    2009-12-15

    Dec 15, 2009 ... Oxidative cross-linked casein mediated by hydrogen peroxide and ferulic acid was prepared at ... functional properties of food proteins treated (Motoki and. Seguro, 1998 ..... Team of Northeast Agricultural University (No.

  2. Cross-linked structure of network evolution

    Science.gov (United States)

    Bassett, Danielle S.; Wymbs, Nicholas F.; Porter, Mason A.; Mucha, Peter J.; Grafton, Scott T.

    2014-03-01

    We study the temporal co-variation of network co-evolution via the cross-link structure of networks, for which we take advantage of the formalism of hypergraphs to map cross-link structures back to network nodes. We investigate two sets of temporal network data in detail. In a network of coupled nonlinear oscillators, hyperedges that consist of network edges with temporally co-varying weights uncover the driving co-evolution patterns of edge weight dynamics both within and between oscillator communities. In the human brain, networks that represent temporal changes in brain activity during learning exhibit early co-evolution that then settles down with practice. Subsequent decreases in hyperedge size are consistent with emergence of an autonomous subgraph whose dynamics no longer depends on other parts of the network. Our results on real and synthetic networks give a poignant demonstration of the ability of cross-link structure to uncover unexpected co-evolution attributes in both real and synthetic dynamical systems. This, in turn, illustrates the utility of analyzing cross-links for investigating the structure of temporal networks.

  3. Cross-linked structure of network evolution

    Energy Technology Data Exchange (ETDEWEB)

    Bassett, Danielle S., E-mail: dsb@seas.upenn.edu [Department of Bioengineering, University of Pennsylvania, Philadelphia, Pennsylvania 19104 (United States); Department of Physics, University of California, Santa Barbara, California 93106 (United States); Sage Center for the Study of the Mind, University of California, Santa Barbara, California 93106 (United States); Wymbs, Nicholas F.; Grafton, Scott T. [Department of Psychology and UCSB Brain Imaging Center, University of California, Santa Barbara, California 93106 (United States); Porter, Mason A. [Oxford Centre for Industrial and Applied Mathematics, Mathematical Institute, University of Oxford, Oxford OX2 6GG (United Kingdom); CABDyN Complexity Centre, University of Oxford, Oxford, OX1 1HP (United Kingdom); Mucha, Peter J. [Carolina Center for Interdisciplinary Applied Mathematics, Department of Mathematics, University of North Carolina, Chapel Hill, North Carolina 27599 (United States); Department of Applied Physical Sciences, University of North Carolina, Chapel Hill, North Carolina 27599 (United States)

    2014-03-15

    We study the temporal co-variation of network co-evolution via the cross-link structure of networks, for which we take advantage of the formalism of hypergraphs to map cross-link structures back to network nodes. We investigate two sets of temporal network data in detail. In a network of coupled nonlinear oscillators, hyperedges that consist of network edges with temporally co-varying weights uncover the driving co-evolution patterns of edge weight dynamics both within and between oscillator communities. In the human brain, networks that represent temporal changes in brain activity during learning exhibit early co-evolution that then settles down with practice. Subsequent decreases in hyperedge size are consistent with emergence of an autonomous subgraph whose dynamics no longer depends on other parts of the network. Our results on real and synthetic networks give a poignant demonstration of the ability of cross-link structure to uncover unexpected co-evolution attributes in both real and synthetic dynamical systems. This, in turn, illustrates the utility of analyzing cross-links for investigating the structure of temporal networks.

  4. The cross linking of EPDM and NBR rubber

    Directory of Open Access Journals (Sweden)

    Samardžija-Jovanović Suzana

    2005-01-01

    Full Text Available In the process of macromolecule cross linking, the choice of type and quantity of the components and the experimental conditions are important to obtain the new cross linked materials with better mechanical and chemical characteristics. The cross linking method depends on the rubber type and structure. Intermolecular cross linking results in the formation elastomer network. The basis of the cross linking process, between ethylene propylene diene rubber (EPDM and acrylonitrile butadiene rubber (NBR, is a chemical reaction. Fillers and other additives are present in different mass ratios in the material. The exploitation properties of the cross linked materials depend on the quantity of additive in the cross linked systems.

  5. Evaluation of cross-linked aggregates from purified Bacillus subtilis levansucrase mutants for transfructosylation reactions

    Directory of Open Access Journals (Sweden)

    Munguia Agustin

    2009-07-01

    Full Text Available Abstract Background Increasing attention has been focused on inulin and levan-type oligosaccharides, including fructosyl-xylosides and other fructosides due to their nutraceutical properties. Bacillus subtilis levansucrase (LS catalyzes the synthesis of levan from sucrose, but it may also transfer the fructosyl moiety from sucrose to acceptor molecules included in the reaction medium. To study transfructosylation reactions with highly active and robust derivatives, cross-linked enzyme aggregates (CLEAs were prepared from wild LS and two mutants. CLEAs combine the catalytic features of pure protein preparations in terms of specific activity with the mechanical behavior of industrial biocatalysts. Results Two types of procedures were used for the preparation of biocatalysts from purified wild type LS (WT LS B. subtilis and the R360K and Y429N LS mutants: purified enzymes aggregated with glutaraldehyde (cross-linked enzyme aggregates: CLEAs, and covalently immobilized enzymes in Eupergit C®. The biocatalysts were characterized and used for fructoside synthesis using xylose as an acceptor model. CLEAs were able to catalyze the synthesis of fructosides as efficiently as soluble enzymes. The specific activity of CLEAs prepared from wild type LS (44.9 U/mg of CLEA, R360K (56.5 U/mg of CLEA and Y429N (1.2 U/mg of CLEA mutants were approximately 70, 40 and 200-fold higher, respectively, than equivalent Eupergit C® immobilized enzyme preparations (U/mg of Eupergit, where units refer to global LS activity. In contrast, the specific activity of the free enzymes was 160, 171.2 and 1.5 U/mg of protein, respectively. Moreover, all CLEAs had higher thermal stability than corresponding soluble enzymes. In the long term, the operational stability was affected by levan synthesis. Conclusion This is the first report of cross-linked transglycosidases aggregates. CLEAs prepared from purified LS and mutants have the highest specific activity for immobilized

  6. Preparation of cross-linked transglutaminase crystals and its enzymology characteristics%转谷氨酰胺酶交联酶晶体的制备及其酶学性质研究

    Institute of Scientific and Technical Information of China (English)

    马永强; 韩春然; 张娜; 张毅方; 刘颖; 王强

    2011-01-01

    对转谷氨酰胺酶晶体进行了交联,研究了交联酶的基本酶学性质。结果表明,交联后,酶的耐高温性增强,在酸性、碱性条件下均比原酶更稳定,具有明显抵抗Fe3+、Zn2+及Cu2+的能力,而Ca2+、Mg2+及Ba2+对交联酶晶体没有明显的影响,在有机溶剂中的酶活力损失较小。与游离酶相比较,交联酶晶体在常温下贮存15d后的酶活力保留80%以上,远远地大于游离酶的剩余酶活。%Transglutaminase(MTG)crystals were cross-linked and the basic enzymology characteristics were studied.The results showed that,compared to the original enzyme,cross-linked MTG had better resistance to heat,acid and alkaline,metal ions(Fe3+,Zn2+ and Cu2+)and organic reagent.After storing for 15 days,the activity of the cross-linked MTG remained above 80%,which was much higher than that of the free MTG.

  7. Preparation of Cross-linking Copolymerization of Chitosan and AMPS in Ionic Liquid%离子液体中壳聚糖/AMPS共聚交联微球的制备

    Institute of Scientific and Technical Information of China (English)

    张聪璐; 胡筱敏; 侯晓虹; 陶颖婷

    2013-01-01

    Cross-linking copolymerization of 2-acrylamide-2-methylpro panesulfonic acid (AMPS) and chitosan in ionic liquid was studied using ceric ammonium nitrate (CAN) as an initiator, p-benzoquinone as resistance polymerization retarder, and glycine hydrochloride ionic liquid water solution as reaction medium. The obtained product was characterized by SEM, FTIR and TGA. The results showed that, the reaction rate and grafting ratio were improved greatly by [Gly]Cl as reaction medium. The obtained product was regular spherical , the particle diameter was about 2 μm. And the product had smooth surface, some resistance to acid and alkali.

  8. Modified gum arabic cross-linked gelatin scaffold for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Sarika, P.R. [Department of Chemistry, Indian Institute of Space Science and Technology, Valiamala, Thiruvananthapuram, Kerala 695 547 (India); Cinthya, Kuriakose [Tissue Culture Laboratory, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Poojappura, Thiruvananthapuram, Kerala 695 012 (India); Jayakrishnan, A. [Department of Biotechnology, Indian Institute of Technology Madras, Chennai 600 036 (India); Anilkumar, P.R., E-mail: anilkumarpr@sctimst.ac.in [Tissue Culture Laboratory, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Poojappura, Thiruvananthapuram, Kerala 695 012 (India); James, Nirmala Rachel, E-mail: nirmala@iist.ac.in [Department of Chemistry, Indian Institute of Space Science and Technology, Valiamala, Thiruvananthapuram, Kerala 695 547 (India)

    2014-10-01

    The present work deals with development of modified gum arabic cross-linked gelatin scaffold for cell culture. A new biocompatible scaffold was developed by cross-linking gelatin (Gel) with gum arabic, a polysaccharide. Gum arabic was subjected to periodate oxidation to obtain gum arabic aldehyde (GAA). GAA was reacted with gelatin under appropriate pH to prepare the cross-linked hydrogel. Cross-linking occurred due to Schiff's base reaction between aldehyde groups of oxidized gum arabic and amino groups of gelatin. The scaffold prepared from the hydrogel was characterized by swelling properties, degree of cross-linking, in vitro degradation and scanning electron microscopy (SEM). Cytocompatibility evaluation using L-929 and HepG2 cells confirmed non-cytotoxic and non-adherent nature of the scaffold. These properties are essential for generating multicellular spheroids and hence the scaffold is proposed to be a suitable candidate for spheroid cell culture. - Highlights: • Gum arabic cross-linked gelatin scaffold was developed for tissue engineering. • Cross-linking was achieved by Schiff's base reaction. • The scaffold is non-cytotoxic and non adherent to fibroblast and hepatocytes. • The scaffolds are potential candidates for spheroid cell culture.

  9. [Corneal collagen cross-linking for keratoconus].

    Science.gov (United States)

    Zotov, V V; Pashtaev, N P; Pozdeeva, N A

    2015-01-01

    Over the last decade, corneal collagen cross-linking (CXL) has become a conventional treatment method for progressive keratoconus. Laboratory studies have shown that CXL increases the diameter of collagen fibers and also the number of intra- and interfibrillar cross-links, thus, increasing biomechanical strength of the irradiated cornea. As confirmed by a series of clinical and randomized controlled trials, CXL is able to slow down and, perhaps, to stop the progression of keratoconus. In most post-CXL patients visual acuity improves, while keratometric readings, spherical equivalent, and higher order aberrations reduce. Although published results prove CXL effective in the treatment of progressive keratoconus, its late consequences are yet unknown. This article reviews the stages of CXL development and results of published experimental and clinical studies. Prospects for CXL modifications that do not require epithelial debridement are discussed.

  10. 离子交联法制备壳聚糖/结冷胶可降解复合膜的研究%Study on preparation of chitosan and gellan gum biodegradable composite film by ionic cross-linking

    Institute of Scientific and Technical Information of China (English)

    高翔; 刘炳杰; 李梦琦; 汪东风; 徐莹

    2012-01-01

    A biodegradable composite film without water solubility was made from chitosan and gellan, glycerin as plasticizers,cross-linked by 4% sodium citrate and 2% calcium chloride.Effect of cross-linking time and pH on the mechanical properties and water resistance of composite film were investigated. Besides, infrared spectrum (FT-IR) ,X- ray diffraction ( X- RD), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC) were used to characterize and analyze the structure and thermal stability of the film.The results showed that sodium citrate and calcium chloride cross-linked composite film,and the cross-linking decreased the crystallinity of chitosan and gellan, and then improved thermal stability of composite film.The composite film had the best properties under a cross-linking time of 5min and pH6.0,tensile strength 91.45MPa,water solubility 7.28% ,swelling ratio 416.63% ,water vapor permeability 0.68×10-10g/( Pa·s·m2) ,compounding and ion crossiinking improved mechanical properties and water resistance of single film.%以壳聚糖和结冷胶为成膜材料,甘油为增塑剂,4%柠檬酸钠和2%氯化钙溶液为交联剂,制备水不溶性可降解复合膜。研究交联时间和交联pH对复合膜机械性能和阻水性的影响,并通过扫描电镜、差示扫描量热法、红外光谱和X-射线衍射对其结构和热稳定性进行表征。结果表明,柠檬酸钠和氯化钙对复合膜的交联降低了壳聚糖和结冷胶的结晶度,提高了复合膜的热稳定性;当交联时间为5min、交联溶液pH为6时,复合膜的机械性能最好,抗拉强度达91.45MPa,水溶性为7.28%,溶胀度为416.63%,水蒸气透过率为0.68×10-10g/(Pa·s·m2);复合与离子交联改善了单一膜机械性能不足及阻水性差的缺点。

  11. Characterization of Cross-Linked Lipase Aggregates

    DEFF Research Database (Denmark)

    Prabhavathi Devi, Bethala Lakshmi Anu; Guo, Zheng; Xu, Xuebing

    2009-01-01

    Commercially available microbial lipases from different sources were immobilized as cross-linked enzyme aggregates (CLEAs) using different precipitants and glutaraldehyde as cross-linkers. These CLEAs were assayed based on esterification between lauric acid and n-propanol in solvent-free systems...... change upon CLEA formation. This work presents a characterization of CLEAs based on an esterification activity assay, which is useful for exploring the synthetic application potential of CLEA technology with favorable perspectives....

  12. Thermal Analyse sof Cross-Linked Polyethylene

    Directory of Open Access Journals (Sweden)

    Radek Polansky

    2007-01-01

    Full Text Available The paper summarizes results obtained during the structural analyses measurements (Differential Scanning Calorimetry DSC, Thermogravimetry TG, Thermomechanical analysis TMA and Fourier transform infrared spectroscopy FT-IR. The samples of cross-linked polyethylene cable insulation were tested via these analyses. The DSC and TG were carried out using simultaneous thermal analyzer TA Instruments SDT Q600 with connection of Fourier transform infrared spectrometer Nicolet 380. Thermomechanical analysis was carried out by TMA Q400EM TA Instruments apparatus.

  13. Collagen cross-linking in thin corneas

    Directory of Open Access Journals (Sweden)

    Prema Padmanabhan

    2013-01-01

    Full Text Available Collagen cross-linking (CXL has become the standard of care for progressive keratoconus, after numerous clinical studies have established its efficacy and safety in suitably selected eyes. The standard protocol is applicable in eyes which have a minimum corneal thickness of 400 μm after epithelial debridement. This prerequisite was stipulated to protect the corneal endothelium and intraocular tissues from the deleterious effect of ultraviolet-A (UVA radiation. However, patients with keratoconus often present with corneal thickness of less than 400 μm and could have otherwise benefited from this procedure. A few modifications of the standard procedure have been suggested to benefit these patients without a compromise in safety. Transepithelial cross-linking, pachymetry-guided epithelial debridement before cross-linking, and the use of hypoosmolar riboflavin are some of the techniques that have been attempted. Although clinical data is limited at the present time, these techniques are worth considering in patients with thin corneas. Further studies are needed to scientifically establish their efficacy and safety.

  14. 球状交联壳聚糖树脂的制备及对金属离子吸附研究%Study on preparation and adsorption of metal ions of spherical cross-linked chitosan resin

    Institute of Scientific and Technical Information of China (English)

    郝金丽; 吴艳

    2014-01-01

    以戊二醛为交联剂,利用悬浮聚合法合成了新型壳聚糖树脂,考虑了操作条件对合成树脂性能的影响,通过显微镜显示,树脂的表面结构随着交联剂浓度提高而改善;提高油水体积比,可显著提高树脂粒径;随着搅拌速度的提高,树脂的粒径减小。利用5%壳聚糖溶液,以戊二醛为交联剂可合成较高强度、粒径较小的球状树脂。通过树脂对铜离子的吸附实验可得出树脂具有较好的吸附性能,其最佳吸附pH为5.0,静态吸附容量为2.39 mg/g,吸附率为95.3%,拓展了该天然高分子材料在金属离子的富集与回收,以及在工业废水处理领域的应用前景。%In this paper, using the glutaraldehyde as the cross-linking reagent, a new cross linked chitosan resin was synthesized by a suspension polymerization method. The effect of various operating conditions on the physical properties of the resin was considered. A scanning electron microscopic observation showed that the surface structure of resin was improving with increasing the concentration of cross linker. It can signiifcantly increase the resin size when improving the water volume ratio. While increasing the stirring speed, the size of resin decreased. Using 5%chitosan solution, can synthesize high strengthen and small sized spherical cross-linking chitosan resin. Through the absorption of copper ions, it can show that resin has better properties on absorption. At the pH 5.0, the static adsorption capacity and adsorption rate is 2.39 mg/g and 95.3%. It expands that the enrichment and recovery of natural polymer materials in metal ions, and the application prospect of industrial wastewater treatment.

  15. Synthesis and Characterisation of Novel Cross Linked Biopolyesters from Olive Oil as Eco-friendly Biodegradable Materials

    Directory of Open Access Journals (Sweden)

    J. Shakina

    2012-01-01

    Full Text Available Novel cross linked biopolyesters were synthesised from naturally available olive oil, oligomeric polytriglyceride fumarate (o-PTF was prepared by glycerolysis of the olive oil followed by condensation with maleic anhydride. The (o-PTF was characterised by spectral (FTIR, UV, NMR and physicochemical properties (specific gravity, viscosity, saponification value, iodine value. The molecular weight of o-PTF was estimated using gel permeation chromatography (GPC. The cross linked biopolyesters were prepared by treating o-PTF of olive with N-vinyl-2-pyrrolidone and vinyl acetate. The cross linked biopolyesters were evaluated for spectral properties (FT IR, cross linked density, thermal properties, mechanical properties and biodegradation. The potential antifungal and anti bacterial activities of the newly prepared biopolyesters were evaluated. The environment degradation was assessed by soil burial test. The outcome of the studies has revealed that the newly prepared cross linked biopolyesters are potential biodegradable material for various consumer application like package materials and agricultural applications.

  16. Supermacroporous chemically cross-linked poly(aspartic acid) hydrogels.

    Science.gov (United States)

    Gyarmati, Benjámin; Mészár, E Zsuzsanna; Kiss, Lóránd; Deli, Mária A; László, Krisztina; Szilágyi, András

    2015-08-01

    Chemically cross-linked poly(aspartic acid) (PASP) gels were prepared by a solid-liquid phase separation technique, cryogelation, to achieve a supermacroporous interconnected pore structure. The precursor polymer of PASP, polysuccinimide (PSI) was cross-linked below the freezing point of the solvent and the forming crystals acted as templates for the pores. Dimethyl sulfoxide was chosen as solvent instead of the more commonly used water. Thus larger temperatures could be utilized for the preparation and the drawback of increase in specific volume of water upon freezing could be eliminated. The morphology of the hydrogels was characterized by scanning electron microscopy and interconnectivity of the pores was proven by the small flow resistance of the gels. Compression tests also confirmed the interconnected porous structure and the complete re-swelling and shape recovery of the supermacroporous PASP hydrogels. The prepared hydrogels are of interest for several biomedical applications as scaffolding materials because of their cytocompatibility, controllable morphology and pH-responsive character.

  17. Cross-linking for microbial keratitis

    Directory of Open Access Journals (Sweden)

    Jayesh Vazirani

    2013-01-01

    Full Text Available The success of collagen cross-linking as a clinical modality to modify the clinical course in keratoconus seems to have fueled the search for alternative applications for this treatment. Current clinical data on its efficacy is limited and laboratory data seems to indicate that it performs poorly against resistant strains of bacteria and against slow growing organisms. However, the biological plausibility of crosslinking and the lack of effective strategies in managing infections with these organisms continue to focus attention on this potential treatment. Well-conducted experimental and clinical studies with controls are required to answer the questions of its efficacy in future.

  18. Riboflavin cross-linking of collagen porous scaffolds for periodontal regeneration

    Directory of Open Access Journals (Sweden)

    Seciu A-M.

    2016-05-01

    Full Text Available Periodontitis treatment using occlusive membranes presented variable efficacy due to their rapid degradation in the complex biologic environment of the damaged periodontium. The aim of this study was to prepare novel composites based on collagen, chondroitin sulfate and fibronectin, and to establish the optimal parameters for their photochemical cross-linking using riboflavin and UV exposure. The degree of cross-linking, biodegradability and density of all scaffold variants were investigated. Their cytotoxicity was evaluated in a culture of gingival fibroblasts by MTT assay and light microscopy. The results indicated that the higher the cross-linking degree, the lower was the scaffold biodegradation. Cell culture studies showed that composite scaffolds were favorable for cellular survival. In conclusion, the cross-linking method using riboflavin and UV exposure resulted in stable and biocompatible collagen-based composite scaffolds that could be used for periodontitis treatment.

  19. Glutaraldehyde vapor cross-linked nanofibrous PVA mat with in situ formed silver nanoparticles.

    Science.gov (United States)

    Destaye, Addisu Getachew; Lin, Cheng-Keng; Lee, Cheng-Kang

    2013-06-12

    Polyvinyl alcohol (PVA) nanofibrous mat can be easily prepared via electrospinning its aqueous solution. However, the obtained nanofibrous mat is instantaneously dissolved in water. Therefore, rendering the environmentally friendly nanofibrous mat water insoluble by cross-linking mechanism is of great interest. The electrospun PVA nanofibrous mat with an average fiber diameter of ca. 400 nm could be effectively cross-linked by glutaraldehyde vapor at room temperature. The cross-linking not only resulted in a water-insoluble nanofibrous mat but also generated an excess amount of unreacted aldehyde functional groups that could reduce silver salts into silver nanoparticles. The in situ formed silver nanoparticles along the fibrous surface showed excellent antimicrobial activity against Escherichia coli. The vapor cross-linked nanofibrous mat shows a high potential to be used for efficiently capturing and killing pathogenic bacteria.

  20. Novel thermoplastic vulcanizates (TPVs based on silicone rubber and polyamide exploring peroxide cross-linking

    Directory of Open Access Journals (Sweden)

    K. Naskar

    2014-04-01

    Full Text Available Novel thermoplastic vulcanizates (TPVs based on silicone rubber (PDMS and polyamide (PA12 have been prepared by dynamic vulcanization process. The effect of dynamic vulcanization and influence of various types of peroxides as cross-linking agents were studied in detail. All the TPVs were prepared at a ratio of 50/50 wt% of silicone rubber and polyamide. Three structurally different peroxides, namely dicumyl peroxide (DCP, 3,3,5,7,7-pentamethyl 1,2,4-trioxepane (PMTO and cumyl hydroperoxide (CHP were taken for investigation. Though DCP was the best option for curing the silicone rubber, at high temperature it suffers from scorch safety. An inhibitor 2,2,6,6-tetramethylpiperidinyloxyl (TEMPO was added with DCP to stabilize the radicals in order to increase the scorch time. Though CHP (hydroperoxide had higher half life time than DCP at higher temperature, it has no significant effect on cross-linking of silicone rubber. PMTO showed prolonged scorch safety and better cross-linking efficiency rather than the other two. TPVs of DCP and PMTO were made up to 11 minutes of mixing. Increased values of tensile strength and elongation at break of PMTO cross-linked TPV indicate the superiority of PMTO. Scanning electron micrographs correlate with mechanical properties of the TPVs. High storage modulus (E' and lower loss tangent value of the PMTO cross-linked TPV indicate the higher degree of cross-linking which is also well supported by the overall cross-link density value. Thus PMTO was found to be the superior peroxide for cross-linking of silicone rubber at high temperature.

  1. Synthesis and properties of reprocessable sulfonated polyimides cross-linked via acid stimulation for use as proton exchange membranes

    Science.gov (United States)

    Zhang, Boping; Ni, Jiangpeng; Xiang, Xiongzhi; Wang, Lei; Chen, Yongming

    2017-01-01

    Cross-linked sulfonated polyimides are one of the most promising materials for proton exchange membrane (PEM) applications. However, these cross-linked membranes are difficult to reprocess because they are insoluble. In this study, a series of cross-linkable sulfonated polyimides with flexible pendant alkyl side chains containing trimethoxysilyl groups is successfully synthesized. The cross-linkable polymers are highly soluble in common solvents and can be used to prepare tough and smooth films. Before the cross-linking reaction is complete, the membranes can be reprocessed, and the recovery rate of the prepared films falls within an acceptable range. The cross-linked membranes are obtained rapidly when the cross-linkable membranes are immersed in an acid solution, yielding a cross-linking density of the gel fraction of greater than 90%. The cross-linked membranes exhibit high proton conductivities and tensile strengths under hydrous conditions. Compared with those of pristine membranes, the oxidative and hydrolytic stabilities of the cross-linked membranes are significantly higher. The CSPI-70 membrane shows considerable power density in a direct methanol fuel cell (DMFC) test. All of these results suggest that the prepared cross-linked membranes have great potential for applications in proton exchange membrane fuel cells.

  2. Preparation and Properties of Cross-linking and Esterifying Pregelatinization Starch of Mechanical Activated Maize Starch%交联酯化机械活化玉米复合变性淀粉的制备及其性能研究

    Institute of Scientific and Technical Information of China (English)

    杨家添; 陈渊; 朱万仁; 谭义秋; 黄祖强; 黎宏妃

    2012-01-01

    以机械活化玉米淀粉为原料,三偏磷酸钠为交联剂,醋酸酐为醋化剂进行复合变性,制备机械活化玉米交联酯化复合变性淀粉,考察反应温度、交联剂用量、交联pH值、交联时间、酯化剂用量、酯化pH值、酯化时间等因素对交联酯化淀粉糊冷黏度的影响,与原玉米淀粉合成的交联酯化淀粉进行比较,研究了产物的理化特性,并利用红外光谱、X射线衍射对产物的结构进行表征分析。结果表明:各因素对机械活化玉米淀粉的交联酯化反应均有影响。对于机械活化1.0 h的玉米淀粉,在反应温度40℃、三偏磷酸钠1.0%、交联pH值10.0、交联时间2.0 h、醋酸酐用量0.5 mL、酯化pH值9.0、酯化时间60 min的条件下,所制备的机械活化玉米交联酯化淀粉糊的冷黏度由活化淀粉的466 mPa.s提高到1 629 mPa.s,淀粉糊液黏度的稳定性、抗酸性、抗老化性明显提高。红外光谱和X射线衍射图谱显示,淀粉经过交联酯化复合变性处理后,分子结构上引入新的化学基团,交联酯化淀粉属于V型结晶。%Cross-linking and esterifying starch of mechanical activated maize starch was prepared by mechanical activated maize starch as raw material,and sodium trimetaphosophate as cross-linking agent and acetic anhydride in acetification.The effects of reaction temperature,cross-linking agent and esterifying agent dosage,pH value and cross-linking time on the cold viscosity of cross-linking and esterifying starch paste were investigated.The physical and chemical parameters of the cross-linking and esterifying starch of mechanical activated maize starch and cross-linking and esterifying starch of raw maize starch were studied.The structure of cross-linking and esterifying of mechanical activated maize starch were characterized by using Fourier transform infrared spectrogram(FTIR) and X-ray diffraction(XRD).The results indicated that the reaction conditions affected the

  3. Syntheses of DNA Duplexes That Contain a N4C-alkyl-N4C Interstrand Cross-Link

    Science.gov (United States)

    Miller, Paul S.

    2011-01-01

    A simple procedure is described for preparing short DNA duplexes that contain a single N4C-alkyl-N4C interstrand cross-link. The synthesis is carried out on an automated DNA synthesizer using standard phosphoramidite chemistry. The cross-link is introduced during the synthesis of the duplex. The method can be used to prepare mg quantities of cross-linked duplexes suitable for physical studies and for the preparation of larger DNA molecules that can be used as substrates to study DNA repair in whole cell extracts and in living cells in culture. PMID:21400705

  4. The Cross - linking reaction of HEC

    Institute of Scientific and Technical Information of China (English)

    XIONG Jian; YE Jun; XUAN Zhiyong; XIE Guohui

    2001-01-01

    @@ Cellulose ethers are important components for light industries such as food and papermaking industries. Its modification research is a frontline science to widen their uses and realize their industrialization. The target of modification is to make high production value, low input and meet the needs better in industries. O-(2-hydroxyethl) cellulose (HEC) is one of the best-known cellulose ether derivatives. It is mainly used as thickeners, dispersants, adhesives, extenders, and films because of its water solubility and gel-forming properties. The present research,by means of cross-linking, we study the influence on HEC about rheological behavior.This will provide a feasible scheme for cellulose ethers modification.

  5. The Cross - linking reaction of HEC

    Institute of Scientific and Technical Information of China (English)

    XIONG; Jian

    2001-01-01

    Cellulose ethers are important components for light industries such as food and papermaking industries. Its modification research is a frontline science to widen their uses and realize their industrialization. The target of modification is to make high production value, low input and meet the needs better in industries.  O-(2-hydroxyethl) cellulose (HEC) is one of the best-known cellulose ether derivatives. It is mainly used as thickeners, dispersants, adhesives, extenders, and films because of its water solubility and gel-forming properties. The present research,by means of cross-linking, we study the influence on HEC about rheological behavior.This will provide a feasible scheme for cellulose ethers modification.……

  6. Phosphate uptake studies of cross-linked chitosan bead materials.

    Science.gov (United States)

    Mahaninia, Mohammad H; Wilson, Lee D

    2017-01-01

    A systematic experimental study is reported that provides a molecular based understanding of cross-linked chitosan beads and their adsorption properties in aqueous solution containing phosphate dianion (HPO4(2-)) species. Synthetically modified chitosan using epichlorohydrin and glutaraldehyde cross-linkers result in surface modified beads with variable hydrophile-lipophile character and tunable HPO4(2-) uptake properties. The kinetic and thermodynamic adsorption properties of cross-linked chitosan beads with HPO4(2-) species were studied in aqueous solution. Complementary structure and physicochemical characterization of chitosan beads via potentiometry, Raman spectroscopy, DSC, and dye adsorption measurements was carried out to establish structure-property relationships. The maximum uptake (Qm) of bead systems with HPO4(2-) at equilibrium was 52.1mgg(-1); whereas, kinetic uptake results for chitosan bead/phosphate systems are relatively rapid (0.111-0.113min(-1)) with an intraparticle diffusion rate-limiting step. The adsorption process follows a multi-step pathway involving inner- and outer-sphere complexes with significant changes in hydration. Phosphate uptake strongly depends on the composition and type of cross-linker used for preparation of chitosan beads. The adsorption isotherms and structural characterization of bead systems illustrate the role of surface charge, hydrophile-lipophile balance, adsorption site accessibility, and hydration properties of the chitosan bead surface. Copyright © 2016 Elsevier Inc. All rights reserved.

  7. Covalently Cross-Linked Arabinoxylans Films for Debaryomyces hansenii Entrapment

    Directory of Open Access Journals (Sweden)

    Ramsés González-Estrada

    2015-06-01

    Full Text Available In the present study, wheat water extractable arabinoxylans (WEAX were isolated and characterized, and their capability to form covalently cross-linked films in presence of Debaryomyces hansenii was evaluated. WEAX presented an arabinose to xylose ratio of 0.60, a ferulic acid and diferulic acid content of 2.1 and 0.04 µg∙mg−1 WEAX, respectively and a Fourier Transform Infra-Red (FT-IR spectrum typical of WEAX. The intrinsic viscosity and viscosimetric molecular weight values for WEAX were 3.6 dL∙g−1 and 440 kDa, respectively. The gelation of WEAX (1% w/v with and without D. hansenii (1 × 107 CFU∙cm−2 was rheologically investigated by small amplitude oscillatory shear. The entrapment of D. hansenii decreased gel elasticity from 1.4 to 0.3 Pa, probably by affecting the physical interactions between WEAX chains. Covalently cross-linked WEAX films containing D. hansenii were prepared by casting. Scanning electron microscopy images show that WEAX films containing D. hansenii were porous and consisted of granular-like and fibre microstructures. Average tensile strength, elongation at break and Young’s modulus values dropped when D. hansenii was present in the film. Covalently cross-lined WEAX containing D. hansenii could be a suitable as a functional entrapping film.

  8. Cross-linked chitosan improves the mechanical properties of calcium phosphate-chitosan cement.

    Science.gov (United States)

    Aryaei, Ashkan; Liu, Jason; Jayatissa, Ahalapitiya H; Jayasuriya, A Champa

    2015-09-01

    Calcium phosphate (CaP) cements are highly applicable and valuable materials for filling bone defects by minimally invasive procedures. The chitosan (CS) biopolymer is also considered as one of the promising biomaterial candidates in bone tissue engineering. In the present study, some key features of CaP-CS were significantly improved by developing a novel CaP-CS composite. For this purpose, CS was the first cross-linked with tripolyphosphate (TPP) and then mixed with CaP matrix. A group of CaP-CS samples without cross-linking was also prepared. Samples were fabricated and tested based on the known standards. Additionally, the effect of different powder (P) to liquid (L) ratios was also investigated. Both cross-linked and uncross-linked CaP-CS samples showed excellent washout resistance. The most significant effects were observed on Young's modulus and compressive strength in wet condition as well as surface hardness. In dry conditions, the Young's modulus of cross-linked samples was slightly improved. Based on the presented results, cross-linking does not have a significant effect on porosity. As expected, by increasing the P/L ratio of a sample, ductility and injectability were decreased. However, in the most cases, mechanical properties were enhanced. The results have shown that cross-linking can improve the mechanical properties of CaP-CS and hence it can be used for bone tissue engineering applications.

  9. Effect of cross-linking degree on selected properties of retrograded starch adipate.

    Science.gov (United States)

    Kapelko, M; Zięba, T; Michalski, A; Gryszkin, A

    2015-01-15

    The aim of this study was to determine the effects of the concentration of paste used to produce retrograded starch, and esterification degree, on selected properties of the resultant distarch adipate. Starch paste was prepared from native potato starch (1, 4, 10, 18 or 30 g/100g), frozen, defrosted and dried. Thus produced preparations of retrograded starch were cross-linked with various doses of a cross-linking agent (0.125, 0.25, 0.5, 1.0 or 2.0 ml per 100g of starch). Properties of the produced adipates depended on both the concentration of paste used to produce retrograded starch and the degree of substitution with adipic acid residues. Solubility in water and swelling power of the cross-linked preparations of retrograded starch, as well as pasting temperature and viscosity of produced pastes, all decreased along with the increasing degree of substitution with adipic acid residues.

  10. Study on Chemical Cross-linking Modification of Hyaluronan and the Biocompatibility of its Derivatives

    Institute of Scientific and Technical Information of China (English)

    HU Guo-ying; LIU Xin; GU Han-qing

    2006-01-01

    Objective: Prepare cross-linked HA gels with higher mechanical stability,lower degradation velocity and desirable biocompatibility,so as to extend the usage of HA.Method: 1.Test molecular weight of HA (MrHA) by viscosimetry;2.Prepare cross-linked HA gels by DVS,GTA,DEC;3.Discuss the cross-linking and degradation procedure;4,evaluate the biocompatibility of the best HA gels.Results: The mechanical stability and durability to degradation of HA-DVS gels are superior to those of other gels,and when HA :DVS = 40:1 (g/g),at 35℃ and in 0.2M NaOH solution,the HA-DVS gel shows the best mechanical stability,and its cytotoxicity reaches class I,hemolysis ratio is lower than 5 %.Conclusion:Our HADVS gel can be used to prepare biologic scaffolds.

  11. Preparation and performance study of cross-linked Zein/PVA-SbQ composite nanofibers spun by electrospinning%光交联Zein/PVA-SbQ复合纳米纤维的制备及表征∗

    Institute of Scientific and Technical Information of China (English)

    崔静; 董建成; 赵明明; 王清清; 陈晓东; 魏取福

    2015-01-01

    采用静电纺制备了不同质量比的玉米醇溶蛋白(Zein)/聚乙烯醇-苯乙烯吡啶盐(PVA-SbQ)复合纳米纤维,在紫外光照射下得到光交联 Zein/PVA-SbQ复合纳米纤维。利用扫描电镜(SEM)对复合纳米纤维的形貌和直径分布进行了分析;傅里叶变换红外光谱(FT-IR)曲线表明,Zein/PVA-SbQ 复合纳米纤维保持了两组分原有的化学功能基团;通过差示扫描量热仪(DSC)研究了复合纳米纤维的热学性能,结果表明其具有较高的热稳定性;静态接触角(CA)测试说明,随着 PVA-SbQ 比例增大复合纳米纤维疏水性降低;强力测试表明,PVA-SbQ的加入增大了 Zein 纳米纤维的强度。%Zein/PVA-SbQ composite nanofibers blend with different mass ratios were fabricated by electrospin-ning.Then the nanofibers were irradiated under UV light to get the cross-linked ones.The morphologies and di-ameter distributions of Zein/PVA-SbQ composite nanofibers were observed by SEM.The spectra of FT-IR indi-cated that two compositions of composite nanofibers maintained their own original functional groups.The ther-mal properties of composite nanofibers were studied by DSC,the results from characterizations revealed that the composite nanofibers still maintained superior thermal stability with the addition of PVA-SbQ.The results of CA elucidated the hydrophobicity decreased for composite nanofibers with increasing PVA-SbQ composition. The strength test showed that the addition of PVA-SbQ increased the tensile strength of composite nanofibers.

  12. Synthesis of cross-linked magnetic composite microspheres containing carboxyl groups

    Institute of Scientific and Technical Information of China (English)

    Jili ZHAO; Zhaorang HAN; Qiang SONG; Ying WANG; Dan SUN

    2008-01-01

    Fe3O4 magnetic nano-particles were prepared by a co-precipitation method and were modified using oleic acid. Then, the cross-linked magnetic composite microspheres containing a carboxyl group were prepared by using an improved emulsion polymerization with divinylbenzene (DVB) as the cross-linking agent. The composite microspheres comprised the Fe3O4 magnetic nano-partictes as cores and the copolymer of styrene and acrylic acid as shells. The morphology and structure of the composite microsphere were characterized by FT-IR, transmission electron microscopy (TEM), X-ray diffrac-tion (XRD), X-ray photoelectron spectrum (XPS) and so on. The results show that the composite microspheres were well dispersed in emulsion with uniform sizes and carboxyl groups on their surface. They were cross-linked and stable in 1 mol/L of HCl and DMF.

  13. Cross-linked aromatic cationic polymer electrolytes with enhanced stability for high temperature fuel cell applications

    DEFF Research Database (Denmark)

    Ma, Wenjia; Zhao, Chengji; Yang, Jingshuai

    2012-01-01

    Diamine-cross-linked membranes were prepared from cross-linkable poly(arylene ether ketone) containing pendant cationic quaternary ammonium group (QPAEK) solution by a facile and general thermal curing method using 4,4′-diaminodiphenylmethane with rigid framework and 1,6-diaminohexane with flexible...... framework as cross-linker, respectively. Self-cross-linked cationic polymer electrolytes membranes were also prepared for comparison. The diamines were advantageously distributed within the polymeric matrix and its amine function groups interacted with the benzyl bromide of QPAEK, resulting in a double...... that the diamine-cross-linked membranes using the rigid cross-linker show much improved properties than that using the flexible cross-linker. More properties relating to the feasibility in high temperature proton exchange membrane fuel cell applications were investigated in detail....

  14. Designing of superporous cross-linked hydrogels containing acrylic-based polymer network

    Directory of Open Access Journals (Sweden)

    Ray Debajyoti

    2008-01-01

    Full Text Available Biodegradable cross-linked polymer, 2-hydroxyethyl methacrylate-co-acrylic acid was synthesized by free radical polymerization technique using N,N"-methylene-bis-acrylamide as cross-linker and benzoyl peroxide as reaction initiator. FT-IR, 1 H-NMR, scanning electron microscopy (SEM, and thermogravimetric analysis (TGA studies of the copolymer along with homopolymers were carried out. FT-IR studies showed no interactions on copolymerization. SEM studies of the copolymer were carried out and mean particle size was found to be 50 µm. TGA analysis indicated an increase in thermal stability by cross-linking the polymer network. Swelling behavior of the copolymer showed more swelling by increasing pH of the medum and the prepared polymer was found to be biodegradable. The prepared cross-linked polymer system holds good for further drug delivery studies in connection to its super swelling and biodegradability.

  15. A General Method for Targeted Quantitative Cross-Linking Mass Spectrometry

    Science.gov (United States)

    Chavez, Juan D.; Eng, Jimmy K.; Schweppe, Devin K.; Cilia, Michelle; Rivera, Keith; Zhong, Xuefei; Wu, Xia; Allen, Terrence; Khurgel, Moshe; Kumar, Akhilesh; Lampropoulos, Athanasios; Larsson, Mårten; Maity, Shuvadeep; Morozov, Yaroslav; Pathmasiri, Wimal; Perez-Neut, Mathew; Pineyro-Ruiz, Coriness; Polina, Elizabeth; Post, Stephanie; Rider, Mark; Tokmina-Roszyk, Dorota; Tyson, Katherine; Vieira Parrine Sant'Ana, Debora; Bruce, James E.

    2016-01-01

    Chemical cross-linking mass spectrometry (XL-MS) provides protein structural information by identifying covalently linked proximal amino acid residues on protein surfaces. The information gained by this technique is complementary to other structural biology methods such as x-ray crystallography, NMR and cryo-electron microscopy[1]. The extension of traditional quantitative proteomics methods with chemical cross-linking can provide information on the structural dynamics of protein structures and protein complexes. The identification and quantitation of cross-linked peptides remains challenging for the general community, requiring specialized expertise ultimately limiting more widespread adoption of the technique. We describe a general method for targeted quantitative mass spectrometric analysis of cross-linked peptide pairs. We report the adaptation of the widely used, open source software package Skyline, for the analysis of quantitative XL-MS data as a means for data analysis and sharing of methods. We demonstrate the utility and robustness of the method with a cross-laboratory study and present data that is supported by and validates previously published data on quantified cross-linked peptide pairs. This advance provides an easy to use resource so that any lab with access to a LC-MS system capable of performing targeted quantitative analysis can quickly and accurately measure dynamic changes in protein structure and protein interactions. PMID:27997545

  16. Insights into the swelling process and drug release mechanisms from cross-linked pectin/high amylose starch matrices

    Directory of Open Access Journals (Sweden)

    Fernanda M. Carbinatto

    2014-02-01

    Full Text Available Cross-linked pectin/high amylose mixtures were evaluated as a new excipient for matrix tablets formulations, since the mixing of polymers and cross-linking reaction represent rational tools to reach materials with modulated and specific properties that meet specific therapeutic needs. Objective: In this work the influence of polymer ratio and cross-linking process on the swelling and the mechanism driving the drug release from swellable matrix tablets prepared with this excipient was investigated. Methods: Cross-linked samples were characterized by their micromeritic properties (size and shape, density, angle of repose and flow rate and liquid uptake ability. Matrix tablets were evaluated according their physical properties and the drug release rates and mechanisms were also investigated. Results: Cross-linked samples demonstrated size homogeneity and irregular shape, with liquid uptake ability insensible to pH. Cross-linking process of samples allowed the control of drug release rates and the drug release mechanism was influenced by both polymer ratio and cross-linking process. The drug release of samples with minor proportion of pectin was driven by an anomalous transport and the increase of the pectin proportion contributed to the erosion of the matrix. Conclusion: The cross-linked mixtures of high amylose and pectin showed a suitable excipient for slowing the drug release rates.

  17. Polymer-additive extraction via pressurized fluids and organic solvents of variously cross-linked poly(methylmethacrylates).

    Science.gov (United States)

    Nazem, N; Taylor, L T

    2002-04-01

    Variously cross-linked poly(methylmethacrylates) (PMMAs) are synthesized with three additives incorporated at theoretically 1000 microg of the additive per gram of prepared polymer. The additives are Irganox 1010, Irganox 1076, and Irgafos 168. The in-house" synthesized polyacrylates are then subjected to supercritical fluid extraction (SFE) to determine if additive recovery is a function of percent cross-linking. Although considerable work in this regard has been performed with non-cross-linked polyolefins, the literature is lacking regarding polyacrylates. Some additive degradation apparently occurs during the synthesis, as judged by the increased complexity of the extract high-performance liquid chromatographic trace and the low percent recoveries observed especially for the Irganoxes. For low polymer cross-linking (1%), it appears that both PMMA synthetic reproducibility and readily observed polymer swelling during SFE are serious issues that adversely affect additive percent recovery and precision of results. Higher percent cross-linking yields more consistent analytical data than low percent cross-linking, even though the amount of additive extracted in all PMMA samples (regardless of cross-linking percentage) is essentially the same whether the extraction is via SFE or liquid-solid extraction with methylene chloride. Results for comparably cross-linked poly(ethylmethacrylate) and poly(butylmethacrylate) are similar to PMMA.

  18. Dehydration of an ethanol/water azeotrope through alginate-DNA membranes cross-linked with metal ions by pervaporation.

    Science.gov (United States)

    Uragami, Tadashi; Banno, Masashi; Miyata, Takashi

    2015-12-10

    To obtain high dehydration membranes for an ethanol/water azeotrope, dried blend membranes prepared from mixtures of sodium alginate (Alg-Na) and sodium deoxyribonucleate (DNA-Na) were cross-linked by immersing in a methanol solution of CaCl2 or MaCl2. In the dehydration of an ethanol/water azeotropic mixture by pervaporation, the effects of immersion time in methanol solution of CaCl2 or MaCl2 on the permeation rate and water/ethanol selectivity through Alg-DNA/Ca(2+) and Alg-DNA/Mg(2+) cross-linked membranes were investigated. Alg-DNA/Mg(2+) cross-linked membrane immersed for 12h in methanol solution of MaCl2 exhibited the highest water/ethanol selectivity. This results from depressed swelling of the membranes by formation of a cross-linked structure. However, excess immersion in solution containing cross-linker led to an increase in the hydrophobicity of cross-linked membrane. Therefore, the water/ethanol selectivity of Alg-DNA/Mg(2+) cross-linked membranes with an excess immersion in cross-linking solution was lowered. The relationship between the structure of Alg-DNA/Ca(2+) and Alg-DNA/Mg(2+) cross-linked membranes and their permeation and separation characteristics during pervaporation of an ethanol/water azeotropic mixture is discussed in detail.

  19. Cross Linked Metal Particles for Low Noise Bolometer Materials

    Science.gov (United States)

    2016-12-12

    SECURITY CLASSIFICATION OF: This final report summarizes WSU’s progress from 4/2/2015 to 09/30/2016 on the project, "Cross-linked Metal Particles ...2016 Final Report: Cross-linked Metal Particles for Low-noise Bolometer Materials The views, opinions and/or findings contained in this report are...peer-reviewed journals: Number of Papers published in non peer-reviewed journals: Final Report: Cross-linked Metal Particles for Low-noise Bolometer

  20. Biodegradation of differently cross-linked collagen membranes: an experimental study in the rat.

    Science.gov (United States)

    Rothamel, Daniel; Schwarz, Frank; Sager, Martin; Herten, Monika; Sculean, Anton; Becker, Jürgen

    2005-06-01

    The aim of the present study was to compare the biodegradation of differently cross-linked collagen membranes in rats. Five commercially available and three experimental membranes (VN) were included: (1) BioGide (BG) (non-cross-linked porcine type I and III collagens), (2) BioMend (BM), (3) BioMendExtend (BME) (glutaraldehyde cross-linked bovine type I collagen), (4) Ossix (OS) (enzymatic-cross-linked bovine type I collagen), (5) TutoDent (TD) (non-cross-linked bovine type I collagen, and (6-8) VN(1-3) (chemical cross-linked porcine type I and III collagens). Specimens were randomly allocated in unconnected subcutaneous pouches separated surgically on the back of 40 wistar rats, which were divided into five groups (2, 4, 8, 16, and 24 weeks), including eight animals each. After 2, 4, 8, 16, and 24 weeks of healing, the rats were sacrificed and explanted specimens were prepared for histologic and histometric analysis. The following parameters were evaluated: biodegradation over time, vascularization, tissue integration, and foreign body reaction. Highest vascularization and tissue integration was noted for BG followed by BM, BME, and VN(1); TD, VN(2), and VN(3) showed prolongated, while OS exhibited no vascularization. Subsequently, biodegradation of BG, BM, BME and VN(1) was faster than TD, VN(2), and VN(3). OS showed only a minute amount of superficial biodegradation 24 weeks following implantation. Biodegradation of TD, BM, BME, VN(2), and VN(3) was associated with the presence of inflammatory cells. Within the limits of the present study, it was concluded that cross-linking of bovine and porcine-derived collagen types I and III was associated with (i) prolonged biodegradation, (ii) decreased tissue integration and vascularization, and (iii) in case of TD, BM, BME, VN(2), and VN(3) foreign body reactions.

  1. Graphene oxide-immobilized NH₂-terminated silicon nanoparticles by cross-linked interactions for highly stable silicon negative electrodes.

    Science.gov (United States)

    Sun, Cheng; Deng, Yuanfu; Wan, Lina; Qin, Xusong; Chen, Guohua

    2014-07-23

    There is a great interest in the utilization of silicon-based anodes for lithium-ion batteries. However, its poor cycling stability, which is caused by a dramatic volume change during lithium-ion intercalation, and intrinsic low electric conductivity hamper its industrial applications. A facile strategy is reported here to fabricate graphene oxide-immobilized NH2-terminated silicon nanoparticles (NPs) negative electrode (Si@NH2/GO) directed by hydrogen bonding and cross-linked interactions to enhance the capacity retention of the anode. The NH2-modified Si NPs first form strong hydrogen bonds and covalent bonds with GO. The Si@NH2/GO composite further forms hydrogen bonds and covalent bonds with sodium alginate, which acts as a binder, to yield a stable composite negative electrode. These two chemical cross-linked/hydrogen bonding interactions-one between NH2-modified Si NPs and GO, and another between the GO and sodium alginate-along with highly mechanically flexible graphene oxide, produced a robust network in the negative electrode system to stabilize the electrode during discharge and charge cycles. The as-prepared Si@NH2/GO electrode exhibits an outstanding capacity retention capability and good rate performance, delivering a reversible capacity of 1000 mAh g(-1) after 400 cycles at a current of 420 mA g(-1) with almost 100% capacity retention. The results indicated the importance of system-level strategy for fabricating stable electrodes with improved electrochemical performance.

  2. Characteristic features and biotechnological applications of cross-linked enzyme aggregates (CLEAs)

    NARCIS (Netherlands)

    Sheldon, R.A.

    2011-01-01

    Cross-linked enzyme aggregates (CLEAs) have many economic and environmental benefits in the context of industrial biocatalysis. They are easily prepared from crude enzyme extracts, and the costs of (often expensive) carriers are circumvented. They generally exhibit improved storage and operational

  3. 21 CFR 177.2710 - Styrene-divinylbenzene resins, cross-linked.

    Science.gov (United States)

    2010-04-01

    ... SERVICES (CONTINUED) FOOD FOR HUMAN CONSUMPTION (CONTINUED) INDIRECT FOOD ADDITIVES: POLYMERS Substances..., preparing, treating, packaging, transporting, or holding food, in accordance with the following prescribed... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Styrene-divinylbenzene resins, cross-linked....

  4. Horseradish peroxidase-catalyzed cross-linking of feruloylated arabinoxylans with β-casein

    NARCIS (Netherlands)

    Boeriu, C.G.; Oudgenoeg, G.; Spekking, W.T.J.; Berendsen, L.B.J.M.; Vancon, L.; Boumans, H.; Gruppen, H.; Berkel, W.J.H. van; Laane, C.; Voragen, A.G.J.

    2004-01-01

    Heterologous conjugates of wheat arabinoxylan and β-casein were prepared via enzymatic cross-linking, using sequential addition of the arabinoxylan to a mixture of β-casein, peroxidase, and hydrogen peroxide. The maximal formation of adducts between the β-casein and the feruloylated arabinoxylan was

  5. 1,3-Diphenylethenylcarbazolyl-Based Monomer for Cross-Linked Hole Transporting Layers

    Directory of Open Access Journals (Sweden)

    Maryte Daskeviciene

    2015-05-01

    Full Text Available A new cross-linkable monomer containing 1,3-diphenylethenylcarbazolyl-based hole-transporting moieties and four reactive epoxy groups, was prepared by a multistep synthesis route from 1,3-bis(2,2-diphenylethenyl-9H-carbazol-2-ol and its application for the in situ formation of cross-linked hole transporting layers was investigated. A high concentration of flexible aliphatic epoxy chains ensures good solubility and makes this compound an attractive cross-linking agent. The synthesized compounds were characterized by various techniques, including differential scanning calorimetry, xerographic time of flight, and electron photoemission in air methods.

  6. Bioreducible cross-linked nanoshell enhances gene transfection of polycation/DNA polyplex in vivo.

    Science.gov (United States)

    Piao, Ji-Gang; Ding, Sheng-Gang; Yang, Lu; Hong, Chun-Yan; You, Ye-Zi

    2014-08-11

    In this study, we have prepared a self-cross-linking PEG-based branched polymer, which easily forms a bioreducible nanoshell around polyplexes of cationic polymer and DNA, simply via heating the polyplex dispersions in the presence of this self-cross-linking branched polymer. This nanoshell can prevent the polyplex from dissociation and aggregation in physiological fluids without inhibiting the electrostatic interactions between the polymer and DNA. Furthermore, glutathione (GSH) can act as a stimulus to open the nanoshell after it has entered the cell. The polyplexes coated with the bioreducible nanoshell show an obvious enhancement in gene transfection in vivo compared with bare polyplexes.

  7. Dynamically vulcanized biobased polylactide/natural rubber blend material with continuous cross-linked rubber phase.

    Science.gov (United States)

    Chen, Yukun; Yuan, Daosheng; Xu, Chuanhui

    2014-03-26

    We prepared a biobased material, dynamically vulcanized polylactide (PLA)/natural rubber (NR) blend in which the cross-linked NR phase owned a continuous network-like dispersion. This finding breaks the traditional concept of a sea-island morphology formed after dynamic vulcanization of the blends. The scan electron microscopy and dissolution/swell experiments provided the direct proof of the continuous cross-linked NR phase. This new biobased PLA/NR blend material with the novel structure is reported for the first time in the field of dynamic vulcanization and shows promise for development for various functional applications.

  8. Ice templated and cross-linked xylan/nanocrystalline cellulose hydrogels.

    Science.gov (United States)

    Köhnke, Tobias; Elder, Thomas; Theliander, Hans; Ragauskas, Arthur J

    2014-01-16

    Structured xylan-based hydrogels, reinforced with cellulose nanocrystals (CNCs), have successfully been prepared from water suspensions by cross-linking during freeze-casting. In order to induce cross-linking during the solidification/sublimation operation, xylan was first oxidized using sodium periodate to introduce dialdehydes. The oxidized xylan was then mixed with CNCs after which the suspension was frozen unidirectionally in order to control the ice crystal formation and by that the pore morphology of the material. Finally the ice crystal templates were removed by freeze-drying. During the freeze-casting process hemiacetal bonds are formed between the aldehyde groups and hydroxyl groups, either on other xylan molecules or on CNCs, which cross-links the system. The proposed cross-linking reaction was confirmed by using cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR) spectroscopy. The pore morphology of the obtained materials was analyzed by scanning electron microscopy (SEM). The materials were also tested for compressive strength properties, both in dry and water swollen state. All together this study describes a novel combined freeze-casting/cross-linking process which enables fabrication of nanoreinforced biopolymer-based hydrogels with controlled porosity and 3-D architecture.

  9. Studies on Cross-linking of succinic acid with chitosan/collagen

    Directory of Open Access Journals (Sweden)

    Tapas Mitra

    2013-01-01

    Full Text Available The present study summarizes the cross-linking property of succinic acid with chitosan /collagen. In detail, the chemistry behind the cross-linking and the improvement in mechanical and thermal properties of the cross-linked material were discussed with suitable instruments and bioinformatics tools. The concentration of succinic acid with reference to the chosen polymers was optimized. A 3D scaffold prepared using an optimized concentration of succinic acid (0.2% (w/v with chitosan (1.0% (w/v and similarly with collagen (0.5% (w/v, was subjected to surface morphology, FT-IR analysis, tensile strength assessment, thermal stability and biocompatibility. Results revealed, cross-linking with succinic acid impart appreciable mechanical strength to the scaffold material. In silico analysis suggested the prevalence of non-covalent interactions, which played a crucial role in improving the mechanical and thermal properties of the cross-linked scaffold. The resultant 3D scaffold may find application as wound dressing material, as an implant in clinical applications and as a tissue engineering material.

  10. Genipin Cross-Linked Polymeric Alginate-Chitosan Microcapsules for Oral Delivery: In-Vitro Analysis

    Directory of Open Access Journals (Sweden)

    Hongmei Chen

    2009-01-01

    Full Text Available We have previously reported the preparation of the genipin cross-linked alginate-chitosan (GCAC microcapsules composed of an alginate core with a genipin cross-linked chitosan membrane. This paper is the further investigation on their structural and physical characteristics. Results showed that the GCAC microcapsules had a smooth and dense surface and a networked interior. Cross-linking by genipin substantially reduced swelling and physical disintegration of microcapsules induced by nongelling ions and calcium sequestrants. Strong resistance to mechanical shear forces and enzymatic degradation was observed. Furthermore, the GCAC membranes were permeable to bovine serum albumin and maintained a molecular weight cutoff at 70 KD, analogous to the widely studied alginate-chitosan, and alginate-poly-L-lysine-alginate microcapsules. The release features and the tolerance of the GCAC microcapsules in the stimulated gastrointestinal environment were also investigated. This GCAC microcapsule formulation offers significant potential as a delivery vehicle for many biomedical applications.

  11. Chloroacetamide-Linked Nucleotides and DNA for Cross-Linking with Peptides and Proteins.

    Science.gov (United States)

    Olszewska, Agata; Pohl, Radek; Brázdová, Marie; Fojta, Miroslav; Hocek, Michal

    2016-09-21

    Nucleotides, 2'-deoxyribonucleoside triphosphates (dNTPs), and DNA probes bearing reactive chloroacetamido group linked to nucleobase (cytosine or 7-deazadaenine) through a propargyl tether were prepared and tested in cross-linking with cysteine- or histidine-containing peptides and proteins. The chloroacetamide-modifed dNTPs proved to be good substrates for DNA polymerases in the enzymatic synthesis of modified DNA probes. Modified nucleotides and DNA reacted efficiently with cysteine and cysteine-containing peptides, whereas the reaction with histidine was sluggish and low yielding. The modified DNA efficiently cross-linked with p53 protein through alkylation of cysteine and showed potential for cross-linking with histidine (in C277H mutant of p53).

  12. Radiation cross-linked polyolefin-insulated wire

    Science.gov (United States)

    Sano, K.; Ishitani, H.

    Because radiation cross-linked polyolefin has excellent mechanical heat resistance, its application limit can be expanded extremely by improving the resistance against heat oxidation and flame. This paper is concerning a halogen free radiation cross-linked polyolefin-insulated wire having excellent heat resistance and flameretardant property, which is used for appliances.

  13. Research Progress in Corneal Cross-linking Agents

    Institute of Scientific and Technical Information of China (English)

    Na Li; Xiujun Peng; Zhengjun Fan

    2014-01-01

    Corneal collagen cross-linking with UVA-riboflavin is cur-rently the only method for preventing the progression of kera-toconus from the pathological perspective. Topical application of a direct cross-linking agent is now attracting widespread at-tention in clinical settings..This article reviews the research progress in the application of indirect or direct cross-linking agents (e.g., riboflavin, glucose, ribose, glutaraldehyde, formaldehyde,.glyceraldehyde,.short chain aliphatic β-nitro alcohol, and genipin) in the treatment of corneal diseases and analyzes the cross-linking efficacy,.toxicity,.and merits and disadvantages of each cross-linking agent,.providing clinical information for further studies.

  14. Synthesis of chemically cross-linked polyvinyl alcohol-co-poly (methacrylic acid) hydrogels by copolymerization; a potential graft-polymeric carrier for oral delivery of 5-fluorouracil

    OpenAIRE

    Muhammad Usman Minhas; Mahmood Ahmad; Liaqat Ali; Muhammad Sohail

    2013-01-01

    Background of the Study The propose of the present work was to develop chemically cross-linked polyvinyl alcohol-co-poly(methacrylic acid) hydrogel (PVA-MAA hydrogel) for pH responsive delivery of 5-Fluorouracil (5-FU). Methods PVA based hydrogels were prepared by free radical copolymerization. PVA has been cross-linked chemically with monomer (methacrylic acid) in aqueous medium, cross-linking agent was ethylene glycol di-methacrylate (EGDMA) and benzoyl peroxide was added as reaction initia...

  15. 牛血清白蛋白辅助交联对苯丙氨酸解氨酶交联酶聚体影响的研究%Influence of bovine serum albumin-assisted strategy on preparation of cross-linked enzyme aggregates of Phenylalanine ammonia lyase

    Institute of Scientific and Technical Information of China (English)

    孙立梅; 李连连; 崔建东

    2013-01-01

    通过牛血清白蛋白(BSA)辅助交联,制备了牛血清白蛋白苯丙氨酸解氨酶交联酶聚体(BSA-PAL-CLEAs).优化了BSA-PAL-CLEAs的制备条件,并比较研究了游离酶、苯丙氨酸解氨酶交联酶聚体(PAL-CLEAs)和BSA-PAL-CLEAs的稳定性差异.研究发现,BSA-PAL-CLEAs的最佳制备条件:BSA浓度为5mg/mL,硫酸铵饱和度80%,戊二醛(10% v/v) 10μL,交联时间2h,所得BSA-PAL-CLEAs的酶活回收率(25%)是不加BSA时(13%)的1.92倍.稳定性研究表明,BSA-PAL-CLEAs的温度稳定性、储藏稳定性比PAL-CLEAs都有所提高;但是,游离酶、PAL-CLEAs、BSA-PAL-CLEAs的pH稳定性相差不大;BSA-PAL-CLEAs在有机溶剂中的稳定性比PAL-CLEAs有所下降.%Cross-linked enzyme aggregates of phenylalanine ammonia lyase(BSA-PAL-CLEAs) were prepared by using BSA as an additive.Conditions for the preparation of BSA-PAL-CLEAs were optimized,and the stability of free PAL,PAL-CLEAs and BSA-PAL-CLEAs was also evaluated,respectively.The optimized conditions of BSAPAL-CLEAs preparation were as follows:80%-saturation ammonia sulfate,5mg/mL BSA,10μL glutaraldehyde (10% v/v)and 2h cross-linking time.Under optimized conditions,the activity recovery of prepared BSA-PAL-CLEAs was 1.92-fold than that of PAL-CLEAs.Moreover,the thermal stability and storage stability of BSA-PAL-CLEAs was higher than that of PAL-CLEAs.However,stability against pH of free PAL、PAL-CLEAs and BSA-PAL-CLEAs was similar.In addition,compared with PAL-CLEAs,the stability of BSA-PAL-CLEAs against organic solvents was decreased.

  16. Preparation of cross-linked microcapsules with spherical pores by in-situ polymerization in (W/O/W) emulsion system; (W/O/W) fukugo emulsion no in situ jugo wo riyoshita kakyo chuku microcapsule no chosei

    Energy Technology Data Exchange (ETDEWEB)

    Ijichi, K.; Hatate, Y. [Kagoshima University, Kagoshima (Japan). Faculty of Engineering; Kiyoyama, S.; Shiomori, K.; Baba, Y.; Kawano, Y. [Miyazaki University, Miyazaki (Japan). Faculty of Engineering

    1997-03-10

    The preparation of a microcapsule with submicron order spherical pores in particles was investigated by an in-situ polymerization method in the oil phase of a (W/O/W) emulsion system. Micro-encapsulation is useful as an immobilization method that can maintain or protect functional components in solid and control the emission of them to the air. However, it is hard to fine-control the spherical pores in particles. The toluene solution to which styrene monomer, divinyl-benzene, polymerization initiator, and surface active agent were added was used for oil phase. A sodium chloride or potassium nitrate solution was used for water phase. These solutions were emulsified to obtain W/O emulsion. The W/O emulsion was dispersed and emulsified into the outer water phase (surface active agent and polyvinyl alcohol) to obtain (W/O/W) emulsion. Styrene and divinyl-benzene were polymerized at a temperature of 333 K, then reduced in pressure and dried as a microcapsule. As a result, a microcapsule (of 10 to 20 {mu}m in diameter) with unevenness and spherical pores on the particle surface and in its inside was obtained. 6 refs., 6 figs., 1 tab.

  17. Nondestructive fluorescence-based quantification of threose-induced collagen cross-linking in bovine articular cartilage

    Science.gov (United States)

    Kinnunen, Jussi; Kokkonen, Harri T.; Kovanen, Vuokko; Hauta-Kasari, Markku; Vahimaa, Pasi; Lammi, Mikko J.; Töyräs, Juha; Jurvelin, Jukka S.

    2012-09-01

    Extensive collagen cross-linking affects the mechanical competence of articular cartilage: it can make the cartilage stiffer and more brittle. The concentrations of the best known cross-links, pyridinoline and pentosidine, can be accurately determined by destructive high-performance liquid chromatography (HPLC). We explore a nondestructive evaluation of cross-linking by using the intrinsic fluorescence of the intact cartilage. Articular cartilage samples from bovine knee joints were incubated in threose solution for 40 and 100 h to increase the collagen cross-linking. Control samples without threose were also prepared. Excitation-emission matrices at wavelengths of 220 to 950 nm were acquired from the samples, and the pentosidine and pyridinoline cross-links and the collagen concentrations were determined using HPLC. After the threose treatment, pentosidine and lysyl pyridinole (LP) concentrations increased. The intrinsic fluorescence, excited below 350 nm, decreased and was related to pentosidine [r=-0.90, 240/325 nm (excitation/emission)] or LP (r=-0.85, 235/285 nm) concentrations. Due to overlapping, the changes in emission could not be linked specifically to the recorded cross-links. However, the fluorescence signal enabled a nondestructive optical estimate of changes in the pentosidine and LP cross-linking of intact articular cartilage.

  18. Elasticity of cross-linked semiflexible biopolymers under tension.

    Science.gov (United States)

    von der Heydt, Alice; Wilkin, Daniel; Benetatos, Panayotis; Zippelius, Annette

    2013-09-01

    Aiming at the mechanical properties of cross-linked biopolymers, we set up and analyze a model of two weakly bending wormlike chains subjected to a tensile force, with regularly spaced inter-chain bonds (cross-links) represented by harmonic springs. Within this model, we compute the force-extension curve and the differential stiffness exactly and discuss several limiting cases. Cross-links effectively stiffen the chain pair by reducing thermal fluctuations transverse to the force and alignment direction. The extra alignment due to cross-links increases both with growing number and with growing strength of the cross-links, and is most prominent for small force f. For large f, the additional, cross-link-induced extension is subdominant except for the case of linking the chains rigidly and continuously along their contour. In this combined limit, we recover asymptotically the elasticity of a weakly bending wormlike chain without constraints, stiffened by a factor of 4. The increase in differential stiffness can be as large as 100% for small f or large numbers of cross-links.

  19. 交联壳聚糖磁性微球的制备及固定化果胶酶研究%The Preparation of Magnetic Microsphere of Cross-linked Chitosan and Immobilization of Pectinase

    Institute of Scientific and Technical Information of China (English)

    林建城; 陈燕红; 张雄

    2012-01-01

    Pectinase was immobilized with magnetic microsphere of chitosan and crosslinked with glutaraldehyde. The partial properties of immobilized enzyme were investigated. The magnetic microspheres were prepared with FesO4 magnetic nucleus and chitosan. Pectinase was immobilized while microspheres were crosslinked with glutaraldehyde. The preparation conditions of immobilized enzyme were determined by orthogonal test design. The partial properties of immobilized enzyme and free enzyme were compared and studied. The results showed that, Fe3O4 magnetic nucleus could be made out when Fe2+:Fe3+ was 1:1 (volume ratio). When the amount of Fei3O4 was 1.0 g, chitosan concentration of 3.0%, 3.0 mg/mL pectinase amount, treated with 3.0% glutaraldehyde for 4 h, and the process time was 1 h under pH 4.0, the recovery rate of magnetic immobilized pectinase activity could reach to 68.4%. The optimum pH and optimum temperature of immobilized pectinase for the hydrolysis of pectin were determined to be pH 4.0 and 50℃, respectively. The immobilized pectinase was stable in the pH ranges from 2.6 to 5.6, and had good thermal stability under 70℃, which the residual enzyme activity was also 82.8% after treated at 70℃ for one hour. The apparent Michaelis constant of immobilized pectinase ATmapp equaled to 1.38 mg/mL. The recovery activity of immobilized enzyme was more than 61.0% after repeated six times. The immobilized pectinase prepared with magnetic microsphere of chitosan were good enough for the strength, the flexibility and the recovery rate, and had good operation stability.%以交联壳聚糖磁性微球为载体制备固定化果胶酶,并研究固定化酶的酶学性质与操作稳定性.通过Fe3O4磁核与壳聚糖制备磁性微球载体,戊二醛交联后对果胶酶进行固定,利用正交试验确定固定化酶制备条件,比较研究了固定化酶与游离酶的酶学性质.结果表明:在Fe2+:FC+体积比为1:1的溶液中,制得Fe3O4磁核;1.0gFe3O4磁核,3.0

  20. Cross-Linked Nanoporous Materials from Reactive and Multifunctional Block Polymers

    Energy Technology Data Exchange (ETDEWEB)

    Seo, Myungeun; Amendt, Mark A.; Hillmyer, Marc A. (UMM)

    2012-10-10

    Polylactide-b-poly(styrene-co-2-hydroxyethylmethacrylate) (PLA-b-P(S-co-HEMA)) and polylactide-b-poly(styrene-co-2-hydroxyethylacrylate) (PLA-b-P(S-co-HEA)) were synthesized by combination of ring-opening polymerization and reversible addition-fragmentation chain transfer polymerization. {sup 1}H nuclear magnetic resonance spectroscopy and size exclusion chromatography data indicated that the polymerizations were controlled and that hydroxyl groups were successfully incorporated into the block polymers. The polymers were reacted with 4,4{prime}-methylenebis(phenyl isocyanate) (MDI) to form the corresponding cross-linked materials. The materials were annealed at 150 C to complete the coupling reaction. Robust nanoporous materials were obtained from the cross-linked polymers by treatment with aqueous base to hydrolyze the PLA phase. Small-angle X-ray scattering study combined with scanning electron microscopy showed that MDI-cross-linked PLA-b-P(S-co-HEMA)/PLA-b-P(S-co-HEA) can adopt lamellar, hexagonally perforated lamellar, and hexagonally packed cylindrical morphologies after annealing. In particular, the HPL morphology was found to evolve from lamellae due to increase in volume fraction of PS phase as MDI reacted with hydroxyl groups. The reaction also kinetically trapped the morphology by cross-linking. Bicontinuous morphologies were also observed when dibutyltin dilaurate was added to accelerate reaction between the polymer and MDI.

  1. Solvent Composition is Critical for Carbodiimide Cross-Linking of Hyaluronic Acid as an Ophthalmic Biomaterial

    Directory of Open Access Journals (Sweden)

    Jui-Yang Lai

    2012-10-01

    Full Text Available Hyaluronic acid (HA is one of the most important ophthalmic biomaterials, while also being used for tissue engineering and drug delivery. Although chemical cross-linking is an effective way to improve the material performance, it may as a consequence be detrimental to the living cells/tissues. Given that the cross-linking efficiency is mediated by the solvent composition during the chemical modification, this study aims to explore the stability and biocompatibility of carbodiimide cross-linked HA in relation to material processing conditions by varying the acetone/water volume ratio (from 70:30 to 95:5 at a constant 1-ethyl-3-(3-dimethyl aminopropyl carbodiimide (EDC concentration of 100 mM. Our results indicated that after the EDC treatment in the presence of an acetone/water mixture (85:15, v/v, the HA hydrogel membranes have the lowest equilibrium water content, the highest stress at break and the greatest resistance to hyaluronidase digestion. Live/Dead assays and pro-inflammatory cytokine expression analyses showed that the cross-linked HA hydrogel membranes, irrespective of the solvent composition, are compatible with human RPE cell lines without causing toxicity and inflammation. However, it should be noted that the test samples prepared by the cross-linking in the presence of acetone/water mixtures containing 70, 75, and 95 vol % of acetone slightly inhibit the metabolic activity of viable ARPE-19 cultures, probably due to the alteration in the ionic interaction between the medium nutrients and polysaccharide biomaterials. In summary, the water content, mechanical strength and RPE cell proliferative capacity strongly depends on the solvent composition for carbodiimide cross-linking of HA materials.

  2. Molecular Structures of Isolevuglandin-Protein Cross-Links.

    Science.gov (United States)

    Bi, Wenzhao; Jang, Geeng-Fu; Zhang, Lei; Crabb, John W; Laird, James; Linetsky, Mikhail; Salomon, Robert G

    2016-10-17

    Isolevuglandins (isoLGs) are stereo and structurally isomeric γ-ketoaldehydes produced through free radical-induced oxidation of arachidonates. Some isoLG isomers are also generated through enzymatic cyclooxygenation. Post-translational modification of proteins by isoLGs is associated with loss-of-function, cross-linking and aggregation. We now report that a low level of modification by one or two molecules of isoLG has a profound effect on the activity of a multi subunit protease, calpain-1. Modification of one or two key lysyl residues apparently suffices to abolish catalytic activity. Covalent modification of calpain-1 led to intersubunit cross-linking. Hetero- and homo-oligomers of the catalytic and regulatory subunits of calpain-1 were detected by SDS-PAGE with Western blotting. N-Acetyl-glycyl-lysine methyl ester and β-amyloid(11-17) peptide EVHHQKL were used as models for characterizing the cross-linking of protein lysyl residues resulting from adduction of iso[4]LGE2. Aminal, bispyrrole, and trispyrrole cross-links of these two peptides were identified and fully characterized by mass spectrometry. Aminal and bispyrrole dimers were both detected. Furthermore, a complex mixture of derivatives of the bispyrrole cross-link containing one or more additional atoms of oxygen was found. Interesting differences are evident in the predominant cross-link type generated in the reaction of iso[4]LGE2 with these peptides. More aminal cross-links versus bispyrrole are formed during the reaction of the dipeptide with iso[4]LGE2. In contrast, more bispyrrole versus aminal cross-links are formed during the reaction of EVHHQKL with iso[4]LGE2. It is tempting to speculate that the EVHHQKL peptide-pyrrole modification forms noncovalent aggregates that favor the production of covalent bispyrrole cross-links because β-amyloid(11-17) tends to spontaneously oligomerize.

  3. Current status of accelerated corneal cross-linking

    Directory of Open Access Journals (Sweden)

    Michael Mrochen

    2013-01-01

    Full Text Available Corneal cross-linking with riboflavin is a technique to stabilize or reduce corneal ectasia, in diseases such as keratoconus and post-laser-assisted in situ keratomileusis (LASIK ectasia. There is an interest by patient as well as clinicians to reduce the overall treatment time. Especially, the introduction of corneal cross-linking in combination with corneal laser surgery demands a shorter treatment time to assure a sufficient patient flow. The principles and techniques of accelerated corneal cross-linking is discussed.

  4. Cross-linking staphylococcal enterotoxin A bound to major histocompatibility complex class I is required for TNF-alpha secretion

    Science.gov (United States)

    Wright, A. D.; Chapes, S. K.

    1999-01-01

    The mechanism of how superantigens function to activate cells has been linked to their ability to bind and cross-link the major histocompatibility complex class II (MHCII) molecule. Cells that lack the MHCII molecule also respond to superantigens, however, with much less efficiency. Therefore, the purpose of this study was to confirm that staphylococcal enterotoxin A (SEA) could bind the MHCI molecule and to test the hypothesis that cross-linking SEA bound to MHCII-deficient macrophages would induce a more robust cytokine response than without cross-linking. We used a capture enzyme-linked immunosorbent assay and an immunprecipitation assay to directly demonstrate that MHCI molecules bind SEA. Directly cross-linking MHCI using monoclonal antibodies or cross-linking bound SEA with an anti-SEA antibody or biotinylated SEA with avidin increased TNF-alpha and IL-6 secretion by MHCII(-/-) macrophages. The induction of a vigorous macrophage cytokine response by SEA/anti-SEA cross-linking of MHCI offers a mechanism to explain how MHCI could play an important role in superantigen-mediated pathogenesis. Copyright 1999 Academic Press.

  5. Covalently cross-linked polyetheretherketone proton exchange membrane for DMFC

    CSIR Research Space (South Africa)

    Luo, H

    2009-05-01

    Full Text Available -7 cm2/s) and good electrochemical stability. The results suggested that cross-linked polyetheretherketone membrane is particularly promising to be used as proton exchange membrane for the direct methanol fuel cell application....

  6. Gelation threshold of cross-linked polymer brushes.

    Science.gov (United States)

    Hoffmann, Max; Lang, Michael; Sommer, Jens-Uwe

    2011-02-01

    The cross-linking of polymer brushes is studied using the bond-fluctuation model. By mapping the cross-linking process into a two-dimensional (2D) percolation problem within the lattice of grafting points, we investigate the gelation transition in detail. We show that the particular properties of cross-linked polymer brushes can be reduced to the distribution of bonds which are formed between the grafted chains, and we propose scaling arguments to relate the gelation threshold to the chain length and the grafting density. The gelation threshold is lower than the percolation threshold for 2D bond percolation because of the longer range and broad distribution of bonds formed by the cross-linking process. We term this type of percolation problem star percolation. We observe a broad crossover from mean-field to critical percolation behavior by analyzing the cluster size distribution near the gelation threshold.

  7. Energy harvesting from vibration with cross-linked polypropylene piezoelectrets

    Directory of Open Access Journals (Sweden)

    Xiaoqing Zhang

    2015-07-01

    Full Text Available Piezoelectret films are prepared by modification of the microstructure of polypropylene foam sheets cross-linked by electronic irradiation (IXPP, followed by proper corona charging. Young’s modulus, relative permittivity, and electromechanical coupling coefficient of the fabricated films, determined by dielectric resonance spectra, are about 0.7 MPa, 1.6, and 0.08, respectively. Dynamic piezoelectric d33 coefficients up to 650 pC/N at 200 Hz are achieved. The figure of merit (FOM, d33 ⋅ g33 for a more typical d33 value of 400 pC/N is about 11.2 GPa−1. Vibration-based energy harvesting with one-layer and two-layer stacks of these films is investigated at various frequencies and load resistances. At an optimum load resistance of 9 MΩ and a resonance frequency of 800 Hz, a maximum output power of 120 μW, referred to the acceleration g due to gravity, is obtained for an energy harvester consisting of a one-layer IXPP film with an area of 3.14 cm2 and a seismic mass of 33.7 g. The output power can be further improved by using two-layer stacks of IXPP films in electric series. IXPP energy harvesters could be used to energize low-power electronic devices, such as wireless sensors and LED lights.

  8. Synthesis and Properties of Cross-Linked Polyamide Aerogels

    Science.gov (United States)

    Williams, Jarrod C.; Meador, Mary Ann; McCorkle, Linda

    2015-01-01

    We report the first synthesis of cross-linked polyamide aerogels through step growth polymerization using a combination of diamines, diacid chloride and triacid chloride. Polyamide oligomers endcapped with amines are prepared as stable solutions in N-methylpyrrolidinone from several different diamine precursors and 1,3-benzenedicarbonyl dichloride. Addition of 1,3,5-benzenetricarbonyl trichloride yields gels which form in under five minutes according to the scheme shown. Solvent exchange of the gels into ethanol, followed by drying using supercritical CO2 extraction gives colorless aerogels with densities around 0.1 to 0.2 gcm3. Thicker monolithes of the polyamide aerogels are stiff and strong, while thin films of certain formulations are highly flexible, durable, and even translucent. These materials may have use as insulation for deployable space structures, rovers, habitats or extravehicular activity suits as well as in many terrestrial applications. Strucure property relationships of the aerogels, including surface area, mechanical properties, and thermal conductivity will be discussed.

  9. Energy harvesting from vibration with cross-linked polypropylene piezoelectrets

    Science.gov (United States)

    Zhang, Xiaoqing; Wu, Liming; Sessler, Gerhard M.

    2015-07-01

    Piezoelectret films are prepared by modification of the microstructure of polypropylene foam sheets cross-linked by electronic irradiation (IXPP), followed by proper corona charging. Young's modulus, relative permittivity, and electromechanical coupling coefficient of the fabricated films, determined by dielectric resonance spectra, are about 0.7 MPa, 1.6, and 0.08, respectively. Dynamic piezoelectric d33 coefficients up to 650 pC/N at 200 Hz are achieved. The figure of merit (FOM, d33 ṡ g33) for a more typical d33 value of 400 pC/N is about 11.2 GPa-1. Vibration-based energy harvesting with one-layer and two-layer stacks of these films is investigated at various frequencies and load resistances. At an optimum load resistance of 9 MΩ and a resonance frequency of 800 Hz, a maximum output power of 120 μW, referred to the acceleration g due to gravity, is obtained for an energy harvester consisting of a one-layer IXPP film with an area of 3.14 cm2 and a seismic mass of 33.7 g. The output power can be further improved by using two-layer stacks of IXPP films in electric series. IXPP energy harvesters could be used to energize low-power electronic devices, such as wireless sensors and LED lights.

  10. Energy harvesting from vibration with cross-linked polypropylene piezoelectrets

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiaoqing [Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology & School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); Institute for Telecommunications Technology, Merckstrasse 25, 64283 Darmstadt (Germany); Wu, Liming [Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology & School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); Sessler, Gerhard M., E-mail: g.sessler@nt.tu-darmstadt.de [Institute for Telecommunications Technology, Merckstrasse 25, 64283 Darmstadt (Germany)

    2015-07-15

    Piezoelectret films are prepared by modification of the microstructure of polypropylene foam sheets cross-linked by electronic irradiation (IXPP), followed by proper corona charging. Young’s modulus, relative permittivity, and electromechanical coupling coefficient of the fabricated films, determined by dielectric resonance spectra, are about 0.7 MPa, 1.6, and 0.08, respectively. Dynamic piezoelectric d{sub 33} coefficients up to 650 pC/N at 200 Hz are achieved. The figure of merit (FOM, d{sub 33} ⋅ g{sub 33}) for a more typical d{sub 33} value of 400 pC/N is about 11.2 GPa{sup −1}. Vibration-based energy harvesting with one-layer and two-layer stacks of these films is investigated at various frequencies and load resistances. At an optimum load resistance of 9 MΩ and a resonance frequency of 800 Hz, a maximum output power of 120 μW, referred to the acceleration g due to gravity, is obtained for an energy harvester consisting of a one-layer IXPP film with an area of 3.14 cm{sup 2} and a seismic mass of 33.7 g. The output power can be further improved by using two-layer stacks of IXPP films in electric series. IXPP energy harvesters could be used to energize low-power electronic devices, such as wireless sensors and LED lights.

  11. Cross-linked polyethylenimine–tripolyphosphate nanoparticles for gene delivery

    Directory of Open Access Journals (Sweden)

    Huang XZ

    2014-10-01

    Full Text Available Xianzhang Huang,1 Sujing Shen,2 Zhanfeng Zhang,1 Junhua Zhuang1 1Department of Laboratory Science, Second Affiliated Hospital of Guangzhou University of Chinese Medicine, 2Department of Laboratory Science, Guangdong Second Provincial Traditional Chinese Medicine Hospital, Guangzhou, People’s Republic of China Abstract: The high transfection efficiency of polyethylenimine (PEI makes it an attractive potential nonviral genetic vector for gene delivery and therapy. However, the highly positive charge of PEI leads to cytotoxicity and limits its application. To reduce the cytotoxicity of PEI, we prepared anion-enriched nanoparticles that combined PEI with tripolyphosphate (TPP. We then characterized the PEI-TPP nanoparticles in terms of size, zeta potential, and Fourier-transform infrared (FTIR spectra, and assessed their transfection efficiency, cytotoxicity, and ability to resist deoxyribonuclease (DNase I digestion. The cellular uptake of PEI-TPP with phosphorylated internal ribosome entry site–enhanced green fluorescent protein C1 or FAM (fluorouracil, Adriamycin [doxorubicin] and mitomycin-labeled small interfering ribonucleic acids (siRNAs was monitored by fluorescence microscopy and confocal laser microscopy. The efficiency of transfected delivery of plasmid deoxyribonucleic acid (DNA and siRNA in vitro was 1.11- to 4.20-fold higher with the PEI-TPP particles (7.6% cross-linked than with the PEI, at all N:P ratios (nitrogen in PEI to phosphorus in DNA tested. The cell viability of different cell lines was more than 90% at the chosen N:P ratios of PEI-TPP/DNA complexes. Moreover, PEI-TPP nanoparticles resisted digestion by DNase I for more than 2 hours. The time-dependent absorption experiment showed that 7.6% of cross-linked PEI-TPP particles were internalized by 293T cells within 1 hour. In summary, PEI-TPP nanoparticles effectively transfected cells while conferring little or no toxicity, and thus have potential application in gene

  12. Influence of 1,2-PB matrix cross-linking on structure and properties of selectively etched 1,2-PB-b-PDMS block copolymers

    DEFF Research Database (Denmark)

    Guo, Fengxiao; Andreasen, Jens Wenzel; Vigild, Martin Etchells

    2007-01-01

    A series of samples with varying cross-linking degree were prepared from the same 1,2-polybutadiene-b-polydimethylsiloxane (1,2-PB-b-PDMS) diblock copolymer precursor. The stability of nanopores generated after PDMS cleaving depends on the cross-linking degree of 1,2-PB. The swelling ratio of the...

  13. Cross-linking of bovine and caprine caseins by microbial transglutaminase and their use as microencapsulating agents for n-3 fatty acids

    Science.gov (United States)

    Bovine and caprine caseins were cross-linked with microbial transglutaminase (mTG). The mTG-cross-linked bovine or caprine casein dispersion, mixed with 14.5% maltodextrin (DE = 40), was used to prepare emulsions with 10.5% algae oil. Oxidative stability of emulsions was evaluated by peroxide valu...

  14. Photochemical Patterning of Ionically Cross-Linked Hydrogels

    Directory of Open Access Journals (Sweden)

    Marion Bruchet

    2013-08-01

    Full Text Available Iron(III cross-linked alginate hydrogel incorporating sodium lactate undergoes photoinduced degradation, thus serving as a biocompatible positive photoresist suitable for photochemical patterning. Alternatively, surface etching of iron(III cross-linked hydrogel contacting lactic acid solution can be used for controlling the thickness of the photochemical pattering. Due to biocompatibility, both of these approaches appear potentially useful for advanced manipulation with cell cultures including growing cells on the surface or entrapping them within the hydrogel.

  15. ROLE OF CORNEAL COLLAGEN CROSS LINKING IN KERATOCONUS

    OpenAIRE

    Atul; Superna; Bhimasankar; Vijayleela

    2015-01-01

    To evaluate the outcome of collagen cross linkage using riboflavin 0.1% and ultraviolet A radiation of a wavelength 370nm . PURPOSE : To determine the effect of collagen cross linking for keratoconus on pachymetry , corneal topography, uncorrected visual acuity, specular count, IOP at 1, 3, 6 months . METHODS : The current study was designed as a prospective interventional trial of corneal collagen cross - linking in subjects w...

  16. Elasticity of cross-linked semiflexible biopolymers under tension

    CERN Document Server

    von der Heydt, Alice; Benetatos, Panayotis; Zippelius, Annette

    2013-01-01

    Aiming at the mechanical properties of cross-linked biopolymers, we set up and analyze a model of two weakly bending wormlike chains subjected to a tensile force, with regularly spaced inter-chain bonds (cross-links) represented by harmonic springs. Within this model, we compute the force-extension curve and the differential stiffness exactly and discuss several limiting cases. Cross-links effectively stiffen the chain pair by reducing thermal fluctuations transverse to the force and alignment direction. The extra alignment due to cross-links increases both with growing number and with growing strength of the cross-links, and is most prominent for small force f. For large f, the additional, cross-link-induced extension is subdominant except for the case of linking the chains rigidly and continuously along their contour. In this combined limit, we recover asymptotically the elasticity of a weakly bending wormlike chain without constraints, stiffened by a factor four. The increase in differential stiffness can ...

  17. Design of phosphated cross-linked microspheres of bael fruit gum as a biodegradable carrier.

    Science.gov (United States)

    Mahammed, Nawaz; Gowda, D V; Deshpande, Rohan D; Thirumaleshwar, Shailesh

    2015-01-01

    Present work was aimed at designing of phosphated cross-linked microspheres of bael fruit gum (BFG) by emulsification method using sodium-tri-meta phosphate as a cross-linking agent for treatment of colon cancer using 5-fluorouracil as model drug. Stirring speed was found to be 1,000 rpm for about 5 h to be optimal to obtain reproducible microspheres. It was found that there is an increase in particle size as polymer concentration is increased whereas a reduction in particle size was observed as there is increase in stirring speed. Cross-linked BFG microspheres were successfully prepared by emulsification method. Optimum surfactant concentration was found to be 2 % w/w. Scanning electron microscopy studies showed that the drug-loaded microspheres were non-aggregated and in spherical shape. Differential scanning calorimetry and Fourier transform infrared-spectroscopy studies showed that drug and excipients are compatible. Release studies showed that drug release was more profound in cecal medium induced with enzymes causing degradation of the cross linked BFG than that of the release showed in simulated intestinal fluid. Stability studies showed that there were no significant changes in the drug content and physical appearance of microspheres.

  18. Chemical structure and properties of interstrand cross-links formed by reaction of guanine residues with abasic sites in duplex DNA.

    Science.gov (United States)

    Catalano, Michael J; Liu, Shuo; Andersen, Nisana; Yang, Zhiyu; Johnson, Kevin M; Price, Nathan E; Wang, Yinsheng; Gates, Kent S

    2015-03-25

    A new type of interstrand cross-link resulting from the reaction of a DNA abasic site with a guanine residue on the opposing strand of the double helix was recently identified, but the chemical connectivity of the cross-link was not rigorously established. The work described here was designed to characterize the chemical structure and properties of dG-AP cross-links generated in duplex DNA. The approach involved characterization of the nucleoside cross-link "remnant" released by enzymatic digestion of DNA duplexes containing the dG-AP cross-link. We first carried out a chemical synthesis and complete spectroscopic structure determination of the putative cross-link remnant 9b composed of a 2-deoxyribose adduct attached to the exocyclic N(2)-amino group of dG. A reduced analogue of the cross-link remnant was also prepared (11b). Liquid chromatography-tandem mass spectrometric (LC-MS/MS) analysis revealed that the retention times and mass spectral properties of synthetic standards 9b and 11b matched those of the authentic cross-link remnants released by enzymatic digestion of duplexes containing the native and reduced dG-AP cross-link, respectively. These results establish the chemical connectivity of the dG-AP cross-link released from duplex DNA and provide a foundation for detection of this lesion in biological samples. The dG-AP cross-link in duplex DNA was remarkably stable, decomposing with a half-life of 22 days at pH 7 and 23 °C. The intrinsic chemical stability of the dG-AP cross-link suggests that this lesion in duplex DNA may have the power to block DNA-processing enzymes involved in transcription and replication.

  19. Polymeric Nanocapsule from Silica Nanoparticle@Cross-linked Polymer Nanoparticles via One-Pot Approach

    Directory of Open Access Journals (Sweden)

    Shen Ruoping

    2009-01-01

    Full Text Available Abstract A facile strategy was developed here to prepare cross-linked polymeric nanocapsules (CP nanocapsules with silica nanoparticles as templates. The silica nanoparticle@cross-linked polymer nanoparticles were prepared by the encapsulation of the silica nanoparticles by the one-pot approach via surface-initiated atom transfer radical polymerization of hydroxyethyl acrylate in the presence ofN,N′-methylenebisacrylamide as a cross-linker from the initiator-modified silica nanoparticles. After the silica nanoparticle templates were etched with hydrofluoric acid, the CP nanocapsules with particle size of about 100 nm were obtained. The strategy developed was confirmed with Fourier transform infrared, thermogravimetric analysis and transmission electron microscopy.

  20. Development and Evaluation of Dual Cross-Linked Pulsatile Beads for Chronotherapy of Rheumatoid Arthritis

    Directory of Open Access Journals (Sweden)

    Abanesh kumar Bansal

    2013-01-01

    Full Text Available In the present investigation, pulsatile release beads were prepared by ionic gelation technique. Lornoxicam dual cross-linked beads were prepared by dropping dispersed phase of lornoxicam, pectin, and sodium alginate into the dispersion phase of different concentrations of calcium chloride solution followed by aluminium chloride solution. The formulated beads were further coated by Eudragit L & S 100 in the ratio 1 : 2 w/w in order to achieve desired lag time. In vitro release study showed lag time of 5–8 h before release of lornoxicam from the formulated beads. Thus, formulated dual cross-linked beads when administered at bed time may release lornoxicam when needed most for chronotherapeutics of early morning rheumatoid arthritis attacks in chronic patients.

  1. Comparative study between novel self cross-linking and conventional fluorinated acrylic latex

    Institute of Scientific and Technical Information of China (English)

    Li Jun Chen

    2011-01-01

    Novel self cross-linking fluorinated acrylic latex (SCLFAL) has been successfully prepared via starved seeded semi-batch emulsion polymerization. The resultant SCLFAL is characterized by Fourier transform infrared (FTTR) spectrometry. Contact angle (CA) and glass transition temperature (Tg) of the film are investigated. Results show that CA and Tg of the film can be improved when the moderate amount of HPMA is introduced into the mixed monomers.

  2. Synthesis, Optimization, Property, Characterization, and Application of Dialdehyde Cross-Linking Guar Gum

    Directory of Open Access Journals (Sweden)

    Tang Hongbo

    2016-01-01

    Full Text Available Dialdehyde cross-linking guar gum (DCLGG, as a novel material, was synthesized using phosphorus oxychloride as a cross-linking reagent, sodium periodate as an oxidant, and ethanol as a solvent through keeping the original particle form of guar gum. The process parameters such as the reaction temperature, reaction time, pH, amount of sodium periodate, and amount of ethanol were optimized by the response surface methodology in order to obtain the regression model of the oxidization. The covalent binding of L-asparagine onto the surfaces of DCLGG was further investigated. The results showed that the best technological conditions for preparing DCLGG were as follows: reaction temperature = 40°C, reaction time = 3.0 h, pH = 4.0, and amount of ethanol = 74.5%. The swelling power of DCLGG was intermediate between cross-linking guar gum and dialdehyde guar gum. The cross-linking and dialdehyde oxidization reduced the viscosity of GG. The cross-liking reduced the melting enthalpy of GG. However, the oxidization increased melting enthalpy of ACLGG. The thermal stability of GG was increased by cross-linking or oxidization. The variation of the onset decomposition temperature and end decomposition temperature of GG was not consistent with thermal stability of GG. L-asparagine could be chemically bound well by DCLGG through forming Schiff base under the weak acidity. The maximum adsorption capacity of L-asparagine on DCLGG with aldehyde content of 56.2% reached 21.9 mg/g.

  3. Robustness

    DEFF Research Database (Denmark)

    Sørensen, John Dalsgaard; Rizzuto, Enrico; Narasimhan, Harikrishna

    2012-01-01

    More frequent use of advanced types of structures with limited redundancy and serious consequences in case of failure combined with increased requirements to efficiency in design and execution followed by increased risk of human errors has made the need of requirements to robustness of structures......, a theoretical and risk-based framework is presented which facilitates the quantification of robustness, and thus supports the formulation of pre-normative guidelines....

  4. Collagen/elastin hydrogels cross-linked by squaric acid.

    Science.gov (United States)

    Skopinska-Wisniewska, J; Kuderko, J; Bajek, A; Maj, M; Sionkowska, A; Ziegler-Borowska, M

    2016-03-01

    Hydrogels based on collagen and elastin are very valuable materials for medicine and tissue engineering. They are biocompatible; however their mechanical properties and resistance for enzymatic degradation need to be improved by cross-linking. Up to this point many reagents have been tested but more secure reactants are still sought. Squaric acid (SqAc), 3,4-dihydroxy 3-cyclobutene 1,2-dione, is a strong, cyclic acid, which reacts easily with amine groups. The properties of hydrogels based on collagen/elastin mixtures (95/5, 90/10) containing 5%, 10% and 20% of SqAc and neutralized via dialysis against deionized water were tested. Cross-linked, 3-D, transparent hydrogels were created. The cross-linked materials are stiffer and more resistant to enzymatic degradation than those that are unmodified. The pore size, swelling ability and surface polarity are reduced due to 5% and 10% of SqAc addition. At the same time, the cellular response is not significantly affected by the cross-linking. Therefore, squaric acid would be regarded as a safe, effective cross-linking agent.

  5. Core Cross-linked Star Polymers for Temperature/pH Controlled Delivery of 5-Fluorouracil

    Directory of Open Access Journals (Sweden)

    Elizabeth Sánchez-Bustos

    2016-01-01

    Full Text Available RAFT polymerization with cross-linking was used to prepare core cross-linked star polymers bearing temperature sensitive arms. The arms consisted of a diblock copolymer containing N-isopropylacrylamide (NIPAAm and 4-methacryloyloxy benzoic acid (4MBA in the temperature sensitive block and poly(hexyl acrylate forming the second hydrophobic block, while ethyleneglycol dimethacrylate was used to form the core. The acid comonomer provides pH sensitivity to the arms and also increases the transition temperature of polyNIPAAm to values in the range of 40 to 46°C. Light scattering and atomic force microscopy studies suggest that loose core star polymers were obtained. The star polymers were loaded with 5-fluorouracil (5-FU, an anticancer agent, in values of up to 30 w/w%. In vitro release experiments were performed at different temperatures and pH values, as well as with heating and cooling temperature cycles. Faster drug release was obtained at 42°C or pH 6, compared to normal physiological conditions (37°C, pH 7.4. The drug carriers prepared acted as nanopumps changing the release kinetics of 5-FU when temperatures cycles were applied, in contrast with release rates at a constant temperature. The prepared core cross-linked star polymers represent advanced drug delivery vehicles optimized for 5-FU with potential application in cancer treatment.

  6. Extreme dryness and DNA-protein cross-links

    Science.gov (United States)

    Bieger-Dose, A.; Dose, K.; Meffert, R.; Mehler, M.; Risi, S.

    Exposure of fungal conidia (Aspergillus ochraceus) or spores of Bacillus subtilis to extreme dryness or vacuum induces DNA lesions, including strand breaks and the formation of DNA-protein cross-links. In wet cells only a small amount of protein is bound to DNA, but exposure to conditions of lowered water activity results in an increasing number of cross-links between DNA and proteins. In fungal conidia these cross-links are detected after selective iodination (125J) of the DNA-bound proteins followed by gel electrophoresis and subsequent autoradiography. Another approach is the labelling of DNA with 32p by means of nick translation and the detection of differences in the electrophoretic mobility of DNA before and after digestion with proteinase K of proteins bound to DNA.

  7. FTIR Spectroscopic Studies on Cross Linking of SU-8 Photoresist

    Science.gov (United States)

    Kalaiselvi, S. M. P.; Tan, T. L.; Rawat, R. S.; Lee, P.; Heussler, S. P.; Breese, M. B. H.

    2013-11-01

    The usage of chemically-amplified, negative tone SU-8 photoresist is numerous, spanning industrial, scientific and medical fields. Hence, in this study, some preliminary studies were conducted to understand the dosage and heat treatment requirements of the SU-8 photoresist essential for pattern generation using X-ray lithography. In this work, using Synchrotron as the X-ray source, SU-8 photoresist was characterized for X-ray lithography in terms of its process parameters such as X-ray exposure dose, post exposure bake (PEB) time and temperature for various photoresist thicknesses which is considered worthwhile in view of applications of SU-8 for the fabrication of very high aspect ratio micro structures. The process parameters were varied and the resultant cross linking of the molecular chains of the photoresist was accurately monitored using a Fourier Transform Infra-Red (FTIR) spectrometer and the results are discussed. The infrared absorption peak at 914 cm-1 in the spectrum of the SU-8 photoresist was found to be a useful indicator for the completion of cross linking in the SU-8 photoresist. Results show that the cross linking of the SU-8 photoresist is at a higher rate from 0 J/cm3 to 30 J/cm3 after which the peak almost saturates regardless of the PEB time. It is a good evidence for the validation of dosage requirement of SU-8 photoresist for effective completion of cross linking, which in turn is a requirement for efficient fabrication of micro and nano structures. An analogous behavior was also observed between the extent of cross linking and the PEB time and temperature. The rate of cross linking declines after a certain period of PEB time regardless of PEB temperature. The obtained results also show a definite relation between variation of the absorbance area of the peak at 914 cm-1 and the X-ray exposure dose.

  8. Application of cross-linked and hydrolyzed arabinoxylans in baking of model rye bread.

    Science.gov (United States)

    Buksa, Krzysztof; Nowotna, Anna; Ziobro, Rafał

    2016-02-01

    The role of water extractable arabinoxylan with varying molar mass and structure (cross-linked vs. hydrolyzed) in the structure formation of rye bread was examined using a model bread. Instead of the normal flour, the dough contained starch, arabinoxylan and protein, which were isolated from rye wholemeal. It was observed that the applied mixes of these constituents result in a product closely resembling typical rye bread, even if arabinoxylan was modified (by cross-linking or hydrolysis). The levels of arabinoxylan required for bread preparation depended on its modification and mix composition. At 3% protein, the maximum applicable level of poorly soluble cross-linked arabinoxylan was 3%, as higher amounts of this preparation resulted in an extensively viscous dough and diminished bread volume. On the other hand highly soluble, hydrolyzed arabinoxylan could be used at a higher level (6%) together with larger amounts of rye protein (3% or 6%). Further addition of arabinoxylan leads to excessive water absorption, resulting in a decreased viscosity of the dough during baking and insufficient gas retention. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Thermally Conductive-Silicone Composites with Thermally Reversible Cross-links.

    Science.gov (United States)

    Wertz, J T; Kuczynski, J P; Boday, D J

    2016-06-08

    Thermally conductive-silicone composites that contain thermally reversible cross-links were prepared by blending diene- and dienophile-functionalized polydimethylsiloxane (PDMS) with an aluminum oxide conductive filler. This class of thermally conductive-silicones are useful as thermal interface materials (TIMs) within Information Technology (IT) hardware applications to allow rework of valuable components. The composites were rendered reworkable via retro Diels-Alder cross-links when temperatures were elevated above 130 °C and required little mechanical force to remove, making them advantageous over other TIM materials. Results show high thermal conductivity (0.4 W/m·K) at low filler loadings (45 wt %) compared to other TIM solutions (>45 wt %). Additionally, the adhesion of the material was found to be ∼7 times greater at lower temperatures (25 °C) and ∼2 times greater at higher temperatures (120 °C) than commercially available TIMs.

  10. Anisotropic nanoparticles with controllable morphologies from non-cross-linked seeded emulsion polymerization.

    Science.gov (United States)

    Niu, Qun; Pan, Mingwang; Yuan, Jinfeng; Liu, Xiao; Wang, Xiaomei; Yu, Haifeng

    2013-09-01

    A simple and elegant approach to fabricate anisotropic P(VC-co-AAEM)/PS nanoparticles with controllable morphologies via emulsifier-free seeded emulsion polymerization is presented. Non-cross-linked P(VC-co-AAEM) seeds with hydrophilic surface are first synthesized through copolymerization of vinyl chloride (VC) and acetoacetoxyethyl methacrylate (AAEM), which are used to prepare P(VC-co-AAEM)/PS NPs with multiple bulges by SEP of styrene. Electron microscopy observation indicates that the content of AAEM in seeds is crucial to control the phase separation and morphology of the composite NPs. Moreover, the thermodynamic immiscibility between PVC and PS is the driving force for the formation of PS bulges onto the P(VC-co-AAEM) seeds. The resultant anisotropic NPs with non-cross-linked feature may promisingly serve as compatibilizers for further polymer processing. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Fluorescence imaging of tryptophan and collagen cross-links to evaluate wound closure ex vivo

    Science.gov (United States)

    Wang, Ying; Ortega-Martinez, Antonio; Farinelli, Bill; Anderson, R. R.; Franco, Walfre

    2016-02-01

    Wound size is a key parameter in monitoring healing. Current methods to measure wound size are often subjective, time-consuming and marginally invasive. Recently, we developed a non-invasive, non-contact, fast and simple but robust fluorescence imaging (u-FEI) method to monitor the healing of skin wounds. This method exploits the fluorescence of native molecules to tissue as functional and structural markers. The objective of the present study is to demonstrate the feasibility of using variations in the fluorescence intensity of tryptophan and cross-links of collagen to evaluate proliferation of keratinocyte cells and quantitate size of wound during healing, respectively. Circular dermal wounds were created in ex vivo human skin and cultured in different media. Two serial fluorescence images of tryptophan and collagen cross-links were acquired every two days. Histology and immunohistology were used to validate correlation between fluorescence and epithelialization. Images of collagen cross-links show fluorescence of the exposed dermis and, hence, are a measure of wound area. Images of tryptophan show higher fluorescence intensity of proliferating keratinocytes forming new epithelium, as compared to surrounding keratinocytes not involved in epithelialization. These images are complementary since collagen cross-links report on structure while tryptophan reports on function. HE and immunohistology show that tryptophan fluorescence correlates with newly formed epidermis. We have established a fluorescence imaging method for studying epithelialization processes during wound healing in a skin organ culture model, our approach has the potential to provide a non-invasive, non-contact, quick, objective and direct method for quantitative measurements in wound healing in vivo.

  12. Advanced Corneal Cross-Linking System with Fluorescence Dosimetry

    Directory of Open Access Journals (Sweden)

    Marc D. Friedman

    2012-01-01

    Full Text Available Purpose. This paper describes an advanced system that combines corneal cross-linking with riboflavin with fluorescence dosimetry, the ability to measure riboflavin diffusion within the cornea both before and during UVA treatment. Methods and Results. A corneal cross-linking system utilizing a digital micromirror device (DMD was assembled and used to measure diffusion coefficients of 0.1% riboflavin in 20% dextran in porcine eyes. A value of (3.3±0.2×10−7 cm2/s was obtained for the stroma. Diffusion coefficients for the transepithelial formulation of 0.1% riboflavin in 0.44% saline and 0.02% BAK were also measured to be 4.7±0.3×10−8 cm2/s for epithelium only and (4.6±0.4×10−7 cm2/s for stroma only. Riboflavin consumption during a UVA treatment was also demonstrated. Conclusion. A new advanced corneal cross-linking system with fluorescence dosimetry of riboflavin has been demonstrated. It is hoped that this method may play a significant role in determining the underlying mechanisms of corneal cross-linking and assist with the development of additional riboflavin formulations. Moreover, dosimetry may prove valuable in providing a method to account for the biological differences between individuals, potentially informing cornea-specific UVA treatment doses in real time.

  13. Simulation of Fracture Nucleation in Cross-Linked Polymer Networks

    Science.gov (United States)

    Moller, J. C.; Barr, S. A.; Schultz, E. J.; Breitzman, T. D.; Berry, R. J.

    2013-02-01

    A novel atomistic simulation method is developed whereby polymer systems can undergo strain-rate-controlled deformation while bond scission is enabled. The aim is to provide insight into the nanoscale origins of fracture. Various highly cross-linked epoxy systems including various resin chain lengths and levels of nonreactive dilution were examined. Consistent with the results of physical experiments, cured resin strength increased and ductility decreased with increasing cross-link density. An analysis of dihedral angle activity shows the locations in the molecular network that are most absorptive of mechanical energy. Bond scission occurred principally at cross-link sites as well as between phenyl rings in the bisphenol moiety. Scissions typically occurred well after yield and were accompanied by steady increases in void size and dihedral angle motion between bisphenol moieties and at cross-link sites. The methods developed here could be more broadly applied to explore and compare the atomistic nature of deformation for various polymers such that mechanical and fracture properties could be tuned in a rational way. This method and its results could become part of a solution system that spans multiple length and time scales and that could more completely represent such mechanical events as fracture.

  14. The Database of Ribosomal Cross-links: an update.

    OpenAIRE

    Baranov, P V; Kubarenko, A V; Gurvich, O L; Shamolina, T A; Brimacombe, R

    1999-01-01

    The Database of Ribosomal Cross-links (DRC) was created in 1997. Here we describe new data incorporated into this database and several new features of the DRC. The DRC is freely available via World Wide Web at http://visitweb.com/database/ or http://www. mpimg-berlin-dahlem.mpg.de/ approximately ag_ribo/ag_brimacombe/drc/

  15. Elasticity of Rigidly Cross-Linked Networks of Athermal Filaments

    NARCIS (Netherlands)

    Zagar, Goran; Onck, Patrick R.; Van der Giessen, Erik

    2011-01-01

    Actin filaments assemble into network-like structures and play an important role in various cellular mechanical processes. It is known that the response of actin networks cross-linked by stiff proteins is characterized by two distinct regimes: (i) a linear stress strain response for small deformatio

  16. Molecular mechanisms in deformation of cross-linked hydrogel nanocomposite.

    Science.gov (United States)

    Mathesan, Santhosh; Rath, Amrita; Ghosh, Pijush

    2016-02-01

    The self-folding behavior in response to external stimuli observed in hydrogels is potentially used in biomedical applications. However, the use of hydrogels is limited because of its reduced mechanical properties. These properties are enhanced when the hydrogels are cross-linked and reinforced with nanoparticles. In this work, molecular dynamics (MD) simulation is applied to perform uniaxial tension and pull out tests to understand the mechanism contributing towards the enhanced mechanical properties. Also, nanomechanical characterization is performed using quasi static nanoindentation experiments to determine the Young's modulus of hydrogels in the presence of nanoparticles. The stress-strain responses for chitosan (CS), chitosan reinforced with hydroxyapatite (HAP) and cross-linked chitosan are obtained from uniaxial tension test. It is observed that the Young's modulus and maximum stress increase as the HAP content increases and also with cross-linking process. Load displacement plot from pullout test is compared for uncross-linked and cross-linked chitosan chains on hydroxyapatite surface. MD simulation reveals that the variation in the dihedral conformation of chitosan chains and the evolution of internal structural variables are associated with mechanical properties. Additional results reveal that the formation of hydrogen bonds and electrostatic interactions is responsible for the above variations in different systems.

  17. Porous Cross-Linked Polyimide-Urea Networks

    Science.gov (United States)

    Meador, Mary Ann B. (Inventor); Nguyen, Baochau N. (Inventor)

    2015-01-01

    Porous cross-linked polyimide-urea networks are provided. The networks comprise a subunit comprising two anhydride end-capped polyamic acid oligomers in direct connection via a urea linkage. The oligomers (a) each comprise a repeating unit of a dianhydride and a diamine and a terminal anhydride group and (b) are formulated with 2 to 15 of the repeating units. The subunit was formed by reaction of the diamine and a diisocyanate to form a diamine-urea linkage-diamine group, followed by reaction of the diamine-urea linkage-diamine group with the dianhydride and the diamine to form the subunit. The subunit has been cross-linked via a cross-linking agent, comprising three or more amine groups, at a balanced stoichiometry of the amine groups to the terminal anhydride groups. The subunit has been chemically imidized to yield the porous cross-linked polyimide-urea network. Also provided are wet gels, aerogels, and thin films comprising the networks, and methods of making the networks.

  18. Femtosecond laser collagen cross-linking without traditional photosensitizers

    Science.gov (United States)

    Guo, Yizang; Wang, Chao; Celi, Nicola; Vukelic, Sinisa

    2015-03-01

    Collagen cross-linking in cornea has the capability of enhancing its mechanical properties and thereby providing an alternative treatment for eye diseases such as keratoconus. Currently, riboflavin assisted UVA light irradiation is a method of choice for cross-link induction in eyes. However, ultrafast pulsed laser interactions may be a powerful alternative enabling in-depth treatment while simultaneously diminishing harmful side effects such as, keratocyte apoptosis. In this study, femtosecond laser is utilized for treatment of bovine cornea slices. It is hypothesized that nonlinear absorption of femtosecond laser pulses plays a major role in the maturation of immature cross-links and the promotion of their growth. Targeted irradiation with tightly focused laser pulses allows for the absence of a photosensitizing agent. Inflation test was conducted on half treated porcine cornea to identify the changes of mechanical properties due to laser treatment. Raman spectroscopy was utilized to study subtle changes in the chemical composition of treated cornea. The effects of treatment are analyzed by observing shifts in Amide I and Amide III bands, which suggest deformation of the collagen structure in cornea due to presence of newly formed cross-links.

  19. Scleral lens tolerance after corneal cross-linking for keratoconus

    NARCIS (Netherlands)

    Visser, Esther Simone; Soeters, Nienke; Tahzib, Nayyirih G.

    2015-01-01

    Purpose. Subjective and objective evaluation of scleral lens tolerance and fitting before and after corneal cross-linking (CXL) for progressive keratoconus. Methods. In this prospective cohort, evaluations were made of 18 unilateral eyes in patients who underwent CXL and had been wearing scleral len

  20. Lactoferrin binding to transglutaminase cross-linked casein micelles

    NARCIS (Netherlands)

    Anema, S.G.; de Kruif, C.G.

    2012-01-01

    Casein micelles in skim milk were either untreated (untreated milk) or were cross-linked using transglutaminase (TGA-milk). Added lactoferrin (LF) bound to the casein micelles and followed Langmuir adsorption isotherms. The adsorption level was the same in both milks and decreased the micellar zeta

  1. Polyimide Aerogels with Three-Dimensional Cross-Linked Structure

    Science.gov (United States)

    Meador, Mary Ann B. (Inventor)

    2016-01-01

    A method for creating a three dimensional cross-linked polyimide structure includes dissolving a diamine, a dianhydride, and a triamine in a solvent, imidizing a polyamic acid gel by heating the gel, extracting the gel in a second solvent, supercritically drying the gel, and removing the solvent to create a polyimide aerogel.

  2. 21 CFR 177.2420 - Polyester resins, cross-linked.

    Science.gov (United States)

    2010-04-01

    .... Pentaerythritol. Polyoxypropylene ethers of 4,4′-isopropylide-nediphenol (containing an average of 2-7.5 moles of...-pentanediol. (3) Cross-linking agents: Butyl acrylate. Butyl methacrylate. Ethyl acrylate. Ethylhexyl acrylate... the production of the resins or added thereto to impart desired technical or physical...

  3. Cross-linked enzyme aggregates (CLEAs): stable and recyclable biocatalysts

    NARCIS (Netherlands)

    Sheldon, R.A.

    2007-01-01

    The key to obtaining an optimum performance of an enzyme is often a question of devising an effective method for its immobilization. In the present review, we describe a novel, versatile and effective methodology for enzyme immobilization as CLEAs (cross-linked enzyme aggregates). The method is

  4. A facile cost-effective method for preparing robust self-cleaning transparent superhydrophobic coating

    Science.gov (United States)

    Wang, Peng; Liu, Jie; Chang, Wenkai; Fan, Xiaoliang; Li, Chunyan; Shi, Yu

    2016-10-01

    This paper reports an easy method to prepare transparent superhydrophobic coating by two-step spray-coating method. In order to improve robustness, PDMS oligomers were used to bond the SiO2 nanoparticle/fluoroalkylsilane composite coating to the substrate. The transmittance of coated glass was above 80 % for wavelengths larger than 500 nm. Moreover, the prepared coating exhibited excellent self-cleaning properties in either air or oil environment. Furthermore, this coating retained superhydrophobic properties after three cycles of abrasion test or strong acid/base attack. Therefore, this robust self-cleaning transparent superhydrophobic coating may have a wide range of practical applications in the optical industry.

  5. EGDMA-cross-linked polystyrene resin: An efficient support for gel phase peptide synthesis

    Indian Academy of Sciences (India)

    P K Ajikumar; K S Devaky

    2000-08-01

    This article illustrates the application of a 2% ethyleneglycol dimethacrylate-cross-linked polystyrene support (EGDMA-PS) in manual solid phase peptide synthesis. This copolymer has been characterised and optimised for peptide synthesis by performing the synthesis of a few model peptides and two biologically important peptides. EGDMA-cross-linked polystyrene support was prepared by the suspension polymerisation of the monomers EGDMA and styrene. EGDMA-PS resin undergoes facile swelling in a variety of solvents, both polar and nonpolar, used in peptide synthesis. The polymer was functionalised by Friedel-Crafts chloromethylation reaction. Peptides were assembled on a 2% cross-linked chloromethyl polymer support of capacity 1.63 mmol Cl/g. The biological peptides synthesised are an 11-residue peptide ATP binding site of the CDC2 kinase and a difficult sequence-a nineresidue peptide 34-42 corresponding to a portion of the hydrophobic terminus of the-amyloid protein 1-42. After synthesis, the peptides were cleaved from the support by treating with neat TFA. Purity of the peptides obtained in good yield was checked by TLC and HPLC methods and found to be fairly high.

  6. Cross-linked polystyrene sulfonic acid and polyethylene glycol as a low-fouling material.

    Science.gov (United States)

    Alghunaim, Abdullah; Zhang Newby, Bi-min

    2016-04-01

    A negatively charged hydrophilic low fouling film was prepared by thermally cross-linking a blend consisting of polystyrene sulfonic acid (PSS) and polyethylene glycol (PEG). The film was found to be stable by dip-washing. The fouling resistance of this material toward bacterial (Escherichia coli) and colloidal (polystyrene particles) attachment, non-specific protein (fibronectin) adsorption and cell (3T3 NIH) adhesion was evaluated and was compared with glass slides modified with polyethylene glycol (PEG) brushes, oxidized 3-mercaptopropyltrimethoxysilane (sulfonic acid, SA), and n-octadecyltrichlorosilane (OTS). The extended Derjaguin-Landau-Verwey-Overbeek (XDLVO) theory and thermodynamic models based on surface energy were used to explain the interaction behaviors of E. coli/polystyrene particles-substrate and protein-substrate interactions, respectively. The cross-linked PSS-PEG film was found to be slightly better than SA and PEG toward resisting non-specific protein adsorption, and showed comparable low attachment results as those of PEG toward particle, bacterial and NIH-3T3 cells adhesion. The low-fouling performance of PSS-PEG, a cross-linked film by a simple thermal curing process, could allow this material to be used for applications in aqueous environments, where most low fouling hydrophilic polymers, such as PSS or PEG, could not be easily retained.

  7. Azide-based cross-linking of polymers of intrinsic microporosity (PIMs) for condensable gas separation

    KAUST Repository

    Du, Naiying

    2011-03-11

    Cross-linked polymers of intrinsic microporosity (PIM)s for gas separation membranes, were prepared by a nitrene reaction from a representative PIM in the presence of two different diazide cross-linkers. The reaction temperature was optimized using TGA. The homogenous membranes were cast from THF solutions of different ratios of PIM to azides. The resulting cross-linked structures of the PIMs membranes were formed at 175 °C after 7.5 h and confirmed by TGA, XPS, FT-IR spectroscopy and gel content analysis. These resulting cross-linked polymeric membranes showed excellent gas separation performance and can be used for O 2/N 2 and CO 2/N 2 gas pairs, as well as for condensable gases, such as CO 2/CH 4, propylene/propane separation. Most importantly, and differently from typical gas separation membranes derived from glassy polymers, the crosslinked PIMs showed no obvious CO 2 plasticization up to 20 atm pressure of pure CO 2 and CO 2/CH 4 mixtures. © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Injectable hyaluronic acid/PEG-p(HPMAm-lac)-based hydrogels dually cross-linked by thermal gelling and Michael addition

    NARCIS (Netherlands)

    Dubbini, Alessandra; Censi, Roberta; Butini, Maria Eugenia; Sabbieti, Maria Giovanna; Agas, Dimitrios; Vermonden, Tina; Di Martino, Piera

    2015-01-01

    Fast in situ forming thermosensitive hydrogels consisted of vinyl sulfone bearing p(HPMAm-lac(1-2))-PEG-p(HPMAm-lac(1-2)) triblock copolymers and thiol modified hyaluronic acid were prepared via a dual cross-linking strategy based on thermal gelation at 37 degrees C and simultaneous Michael addition

  9. Study of cross-linking process in grafted polyethylene and ethylene based copolymer using a phase resolved photoacoustic method

    Science.gov (United States)

    Dias, D. T.; Medina, A. N.; Baesso, M. L.; Bento, A. C.; Porto, M. F.; Muniz, E. C.; Rubira, A. F.

    2003-01-01

    In this work, the phase resolved photoacoustic method has been employed to monitor water saturated vapor cross linking in both copolymer and grafted polyethylene. The overtone bands and stretching frequencies combinations of the -Si-OH, =CH2, -CH3, and -CH2-CH3 were monitored and analyzed accordingly to a 32 factorial design with nine samples. The results showed that the cross-linking processes were more efficient when the samples were prepared at 80 °C with the catalyst in the concentration range between 3% and 5% for grafted PE, while 70 °C was the best temperature to obtain copolymer.

  10. Histological response to injected gluteraldehyde cross-linked bovine collagen based implant in a rat model

    Directory of Open Access Journals (Sweden)

    Cağlar Melda

    2006-02-01

    Full Text Available Abstract Background The aim of present study is to investigate the short and long term histopathological alterations caused by submucosal injection of gluteraldehyde cross-linked bovine collagen based on an experimental rat model. Methods Sixty Sprague-Dawley rats were assigned into two groups as group I and II each containing 30 rats. 0.1 ml of saline solution and 0.1 ml of gluteraldehyde cross-linked bovine collagen were injected into the submucosa of bladder of first (control and second groups, respectively. Both group I and II were further subdivided into 3 other groups as Group IA, IB, IC and Group IIA, IIB, IIC according to the sacrification period. Group IA and IIA, IB and IIB, IC and IIC rats (10 rats for each group were sacrificed 3, 6, and 12 months after surgical procedure, respectively. Two slides prepared from injection site of the bladder were evaluated completely for each rat by being unaware of the groups and at random by two independent senior pathologists to determine the fibroblast invasion, collagen formation, capillary ingrowth and inflammatory reaction. Additionally, randomized brain sections from each rat were also examined to detect migration of the injection material. The measurements were made using an ocular micrometer at ×10 magnification. The results were assessed using t-tests for paired and independent samples, with p Results Migration to the brain was not detected in any group. Significant histopathological changes in the gluteraldehyde cross-linked bovine collagen injected groups were fibroblast invasion in 93.3%, collagen formation in 73.3%, capillary ingrowth in 46.6%, inflamatory reaction in 20%. Conclusion We emphasize that the usage of gluteraldehyde cross-linked bovine collagen in children appears to be safe for endoscopic treatment of vesicoureteral reflux.

  11. Fabrication and properties of irradiation-cross-linked poly(vinyl alcohol)/clay aerogel composites.

    Science.gov (United States)

    Chen, Hong-Bing; Liu, Bo; Huang, Wei; Wang, Jun-Sheng; Zeng, Guang; Wu, Wen-Hao; Schiraldi, David A

    2014-09-24

    Poly(vinyl alcohol) (PVOH)/clay aerogel composites were fabricated by an environmentally friendly freeze-drying of the aqueous precursor suspensions, followed by cross-linking induced by gamma irradiation without chemical additives. The influences of cross-linking conditions, i.e., absorbed dose and polymer loading as well as density on the aerogel structure and properties, were investigated. The absorbed dose of 30 kGy was found to be the optimum dose for fabricating strong PVOH composites; the compressive modulus of an aerogel prepared from an aqueous suspension containing 2 wt % PVOH/8 wt % clay increased 10-fold, and that containing 1 wt % PVOH/9 wt % clay increased 12 times upon cross-linking with a dose of 30 kGy. Increasing the solids concentration led to an increase in the mechanical strength, in accordance with the changes in microstructure from layered structure to network structure. The increase of absorbed dose also led to decreased porous size of the network structure. Cross-linking and the increase of the PVOH lead to decreased thermal stability. The strengthened PVOH/clay aerogels possess very low flammability, as measured by cone calorimetry, with heat, smoke, and volatile products release value decreasing as increasing clay content. The mechanism of flame retardation in these materials was investigated with weight loss, FTIR, WAXD, and SEM of the burned residues. The proposed mechanism is that with decreasing fuel content (increasing clay content), increased heat and mass transport barriers are developed; simultaneously low levels of thermal conductivity are maintained during the burning.

  12. Highly stable ionic-covalent cross-linked sulfonated poly(ether ether ketone) for direct methanol fuel cells

    Science.gov (United States)

    Lei, Linfeng; Zhu, Xingye; Xu, Jianfeng; Qian, Huidong; Zou, Zhiqing; Yang, Hui

    2017-05-01

    A novel ionic cross-linked sulfonated poly(ether ether ketone) containing equal content of sulfonic acid and pendant tertiary amine groups (TA-SPEEK) has been initially synthesized for the application in direct methanol fuel cells (DMFCs). By adjusting the ratio of p-xylene dibromide to tertiary amine groups of TA-SPEEK, a series of ionic-covalent cross-linked membranes (C-SPEEK-x) with tunable degree of cross-linking are prepared. Compared with the pristine membrane, the ionic and ionic-covalent cross-linked proton exchange membranes (PEMs) exhibit reduced methanol permeability and improved mechanical properties, dimensional and oxidative stability. The proton conductivity and methanol selectivity of protonated TA-SPEEK and C-SPEEK-x at 25 °C is up to 0.109 S cm-1 and 3.88 × 105 S s cm-3, respectively, which are higher than that of Nafion 115. The DMFC incorporating C-SPEEK-25 exhibits a maximum power density as high as 35.3 mW cm-2 with 4 M MeOH at 25 °C (31.8 mW cm-2 for Nafion 115). Due to the highly oxidative stability of the membrane, no obvious performance degradation of the DMFC is observed after more than 400 h operation, indicating such cost-effective ionic-covalent cross-linked membranes have substantial potential as alternative PEMs for DMFC applications.

  13. Entrapment of methyl parathion hydrolase in cross-linked poly(γ-glutamic acid)/gelatin hydrogel.

    Science.gov (United States)

    Xie, Jianfei; Zhang, Huiwen; Li, Xu; Shi, Yuanliang

    2014-02-10

    Methyl parathion hydrolase (MPH) is an important enzyme in hydrolyzing toxic organophosphorus (OP) compounds. However, MPH is easily deactivated when subjected to extreme environmental conditions and is difficult to recover from the reaction system for reuse, thereby limiting its practical application. To address these shortcomings, we examined the entrapment of MPH in an environment-friendly, biocompatible and biodegradable cross-linked poly(γ-glutamic acid)/gelatin hydrogel. The cross-linked poly(γ-glutamic acid)/gelatin hydrogels were prepared with different gelatin/poly(γ-glutamic acid) mass ratios using water-soluble carbodiimide as the cross-linking agent. The MPH-entrapped cross-linked poly(γ-glutamic acid)/gelatin hydrogel (CPE-MPH) not only possessed improved thermostability, pH stability, and reusability but also exhibited enhanced efficiency in hydrolyzing OP compounds. Furthermore, CPE-MPH possesses high water-absorbing and water-retaining capabilities. We believe that the cross-linked poly(γ-glutamic acid)/gelatin hydrogels are an attractive carrier for the entrapment of diverse enzymes, affording a new approach for enzyme entrapment.

  14. Comparative studies on performance of radiation-induced and thermal cross-linked ion-exchange membrane for water electrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Chakrabarty, Tina; Jasti, Amaranadh [Electro-Membrane Processes Division, Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research (CSIR), G. B. Marg, Bhavnagar 364002, Gujarat (India); Goel, N.K. [Radiation Technology Division, Bhabha Atomic Research Center, Trombay, Mumbai (India); Shahi, Vinod K., E-mail: vkshahi@csmcri.or [Electro-Membrane Processes Division, Central Salt and Marine Chemicals Research Institute, Council of Scientific and Industrial Research (CSIR), G. B. Marg, Bhavnagar 364002, Gujarat (India); Sabharwal, Sunil [Radiation Technology Division, Bhabha Atomic Research Center, Trombay, Mumbai (India)

    2011-07-15

    Radiation-induced and thermal cross-linked sulfonated poly(ether sulfone) (SPS)-sulfonated poly(ether ether ketone) (SPK) composite ion-exchange membranes (SPS/SPK({gamma}) and SPS/SPK(T), respectively) were prepared. Their performances for water electrolysis were comparatively assessed. Thermal cross-linked membrane (SPS/SPK(T)) showed cross-linking of part functional groups (-SO{sub 3}H) and thus deterioration in membrane conductivity. While, radiation-induced cross-linked membrane (SPS/SPK({gamma})) avoided any cross-linking between functional groups and thus conductivity. Electrolysis performances of these membranes were evaluated in comparison with Nafion117 membrane. Relatively low current efficiency (CE) for SPS/SPK and SPS/SPK(T) membranes was due to their high mass transfer (water) via electro-osmotic drag, which was negligible for SPS/SPK({gamma}) membrane. SPS/SPK({gamma}) membrane exhibited comparable stabilities and water splitting performance with Nafion117 membrane, which revealed its suitability as substitute for electrochemical applications.

  15. Comparative studies on performance of radiation-induced and thermal cross-linked ion-exchange membrane for water electrolysis

    Science.gov (United States)

    Chakrabarty, Tina; Jasti, Amaranadh; Goel, N. K.; Shahi, Vinod K.; Sabharwal, Sunil

    2011-07-01

    Radiation-induced and thermal cross-linked sulfonated poly(ether sulfone) (SPS)-sulfonated poly(ether ether ketone) (SPK) composite ion-exchange membranes (SPS/SPK(γ) and SPS/SPK(T), respectively) were prepared. Their performances for water electrolysis were comparatively assessed. Thermal cross-linked membrane (SPS/SPK(T)) showed cross-linking of part functional groups (-SO 3H) and thus deterioration in membrane conductivity. While, radiation-induced cross-linked membrane (SPS/SPK(γ)) avoided any cross-linking between functional groups and thus conductivity. Electrolysis performances of these membranes were evaluated in comparison with Nafion117 membrane. Relatively low current efficiency (CE) for SPS/SPK and SPS/SPK(T) membranes was due to their high mass transfer (water) via electro-osmotic drag, which was negligible for SPS/SPK(γ) membrane. SPS/SPK(γ) membrane exhibited comparable stabilities and water splitting performance with Nafion117 membrane, which revealed its suitability as substitute for electrochemical applications.

  16. Cross-linked PEG via degradable phosphate ester bond: synthesis, water-swelling, and application as drug carrier.

    Science.gov (United States)

    Liu, Zhaoxing; Wang, Lei; Bao, Chunyan; Li, Xinxin; Cao, Lei; Dai, Kerong; Zhu, Linyong

    2011-06-13

    A new series of degradable and water-swellable cross-linked PEG phosphoester polymers (CPPs) based on a facile cross-linked reaction between diphosphoesters of polyethylene glycol (P-PEG-P) and diglycidyl ether of polyethylene glycol (E-PEG-E) has been prepared and characterized. The molecular weights and ratios of the prepolymers played an important role for the properties of CPPs polymers, such as mechanical property, swelling, and degradation rates. In the curing process, the glycidyl ether was consumed by both hydroxyl of the phosphoester (P-OH) and hydroxyl generated from the opened glycidyl ethers (C-OH) with the presence of acid, which generated degradable phosphate esters as cross-linked points and ether bonds as the short branches, respectively. Drug entrapment and release test and biological cytotoxicity studies in vitro suggested that the polymers and generated hydrogels have great potential applications in drug delivery system and biological materials.

  17. pH/sugar dual responsive core-cross-linked PIC micelles for enhanced intracellular protein delivery.

    Science.gov (United States)

    Ren, Jie; Zhang, Yanxin; Zhang, Ju; Gao, Hongjun; Liu, Gan; Ma, Rujiang; An, Yingli; Kong, Deling; Shi, Linqi

    2013-10-14

    Herein, a series of biocompatible, robust, pH/sugar-sensitive, core-cross-linked, polyion complex (PIC) micelles based on phenylboronic acid-catechol interaction were developed for protein intracellular delivery. The rationally designed poly(ethylene glycol)-b-poly(glutamic acid-co-glutamicamidophenylboronic acid) (PEG-b-P(Glu-co-GluPBA)) and poly(ethylene glycol)-b-poly(l-lysine-co-ε-3,4-dihydroxyphenylcarboxyl-L-lysine) (PEG-b-P(Lys-co-LysCA)) copolymers were successfully synthesized and self-assembled under neutral aqueous condition to form uniform micelles. These micelles possessed a distinct core-cross-linked core-shell structure comprised of the PEG outer shell and the PGlu/PLys polyion complex core bearing boronate ester cross-linking bonds. The cross-linked micelles displayed superior physiological stabilities compared with their non-cross-linked counterparts while swelling and disassembling in the presence of excess fructose or at endosomal pH. Notably, either negatively or positively charged proteins can be encapsulated into the micelles efficiently under mild conditions. The in vitro release studies showed that the release of protein cargoes under physiological conditions was minimized, while a burst release occurred in response to excess fructose or endosomal pH. The cytotoxicity of micelles was determined by cck-8 assay in HepG2 cells. The cytochrome C loaded micelles could efficiently delivery proteins into HepG2 cells and exhibited enhanced apoptosis ability. Hence, this type of core-cross-linked PIC micelles has opened a new avenue to intracellular protein delivery.

  18. Transient Anisocoria after Corneal Collagen Cross-Linking

    Science.gov (United States)

    Kymionis, George D.; Grentzelos, Michael A.; Stojanovic, Nela; Paraskevopoulos, Theodore A.; Detorakis, Efstathios T.

    2014-01-01

    Purpose. To report a case with transient anisocoria after corneal collagen cross-linking (CXL). Methods. Case report. Results. A 24-year-old male underwent corneal collagen cross-linking (CXL) in his right eye for keratoconus. At the end of the procedure, the pupil of the treated eye was irregular and dilated, while the pupil of the fellow eye was round, regular, and reactive (anisocoria). The following day, pupils were round, regular, and reactive in both eyes. Conclusion. Anisocoria may be a transient and innocuous complication after CXL. A possible cause for this complication might be the anesthetic drops used before and during the surgical procedure or/and the ultraviolet A irradiation during the treatment. PMID:25276451

  19. Transient Anisocoria after Corneal Collagen Cross-Linking

    Directory of Open Access Journals (Sweden)

    George D. Kymionis

    2014-01-01

    Full Text Available Purpose. To report a case with transient anisocoria after corneal collagen cross-linking (CXL. Methods. Case report. Results. A 24-year-old male underwent corneal collagen cross-linking (CXL in his right eye for keratoconus. At the end of the procedure, the pupil of the treated eye was irregular and dilated, while the pupil of the fellow eye was round, regular, and reactive (anisocoria. The following day, pupils were round, regular, and reactive in both eyes. Conclusion. Anisocoria may be a transient and innocuous complication after CXL. A possible cause for this complication might be the anesthetic drops used before and during the surgical procedure or/and the ultraviolet A irradiation during the treatment.

  20. Cytokines and growth factors cross-link heparan sulfate

    Science.gov (United States)

    Migliorini, Elisa; Thakar, Dhruv; Kühnle, Jens; Sadir, Rabia; Dyer, Douglas P.; Li, Yong; Sun, Changye; Volkman, Brian F.; Handel, Tracy M.; Coche-Guerente, Liliane; Fernig, David G.; Lortat-Jacob, Hugues; Richter, Ralf P.

    2015-01-01

    The glycosaminoglycan heparan sulfate (HS), present at the surface of most cells and ubiquitous in extracellular matrix, binds many soluble extracellular signalling molecules such as chemokines and growth factors, and regulates their transport and effector functions. It is, however, unknown whether upon binding HS these proteins can affect the long-range structure of HS. To test this idea, we interrogated a supramolecular model system, in which HS chains grafted to streptavidin-functionalized oligoethylene glycol monolayers or supported lipid bilayers mimic the HS-rich pericellular or extracellular matrix, with the biophysical techniques quartz crystal microbalance (QCM-D) and fluorescence recovery after photobleaching (FRAP). We were able to control and characterize the supramolecular presentation of HS chains—their local density, orientation, conformation and lateral mobility—and their interaction with proteins. The chemokine CXCL12α (or SDF-1α) rigidified the HS film, and this effect was due to protein-mediated cross-linking of HS chains. Complementary measurements with CXCL12α mutants and the CXCL12γ isoform provided insight into the molecular mechanism underlying cross-linking. Fibroblast growth factor 2 (FGF-2), which has three HS binding sites, was also found to cross-link HS, but FGF-9, which has just one binding site, did not. Based on these data, we propose that the ability to cross-link HS is a generic feature of many cytokines and growth factors, which depends on the architecture of their HS binding sites. The ability to change matrix organization and physico-chemical properties (e.g. permeability and rigidification) implies that the functions of cytokines and growth factors may not simply be confined to the activation of cognate cellular receptors. PMID:26269427

  1. The effect of an additional phosphite stabilizer on the properties of radiation cross-linked vitamin E blends of UHMWPE.

    Science.gov (United States)

    Oral, Ebru; Neils, Andrew; Yabannavar, Pooja; Muratoglu, Orhun K

    2014-06-01

    Antioxidant stabilization of radiation cross-linked ultrahigh molecular weight polyethylene (UHMWPE) has been introduced to improve the oxidative stability of total joint implant bearing surfaces. Blending of an antioxidant with UHMWPE resin powder followed by consolidation and radiation cross-linking has been cleared by the FDA for use in both total hips and total knees for designs incorporating two antioxidants, namely vitamin E and Covernox™ (a medical grade version of Irganox™ 1010). The antioxidants in the polymer are expected to protect the polymer during consolidation, during radiation cross-linking, on the shelf before implantation, and in vivo after implantation. To maximize the protection of the polymer afforded by the antioxidant in vivo, a novel approach may be the use of multiple antioxidants, especially to protect the primary antioxidant for a longer period of time. We hypothesized that the addition of a phosphite stabilizer (Irgafos 168™) commonly used in conjunction with hindered phenolic antioxidants in polymer processing could improve the oxidative stability of radiation cross-linked blends of vitamin E. To test our hypothesis, we prepared UHMWPE blends with 0.05 wt% Irgafos and 0.05 wt% vitamin E and compared its cross-link density, wear resistance, tensile properties, and impact strength to control blends containing only vitamin E. Our hypothesis was not supported; the cross-link density of UHMWPE was significantly decreased by the additive without additional benefit to oxidative stability. To our knowledge, this was the first attempt at using multiple stabilizers in medical grade UHMWPE.

  2. Oxidized pectin cross-linked carboxymethyl chitosan: a new class of hydrogels.

    Science.gov (United States)

    Fan, Lihong; Sun, Yi; Xie, Weiguo; Zheng, Hua; Liu, Shuhua

    2012-01-01

    Oxidation of pectin was performed with sodium periodate to prepare pectin dialdehyde (PD). In this study we used the cross-linking reaction of the active aldehyde of PD and the amino of carboxymethyl chitosan (CMC) to prepare the hydrogels. By controlling the proportion of pectin dialdehyde and CMC we made different kinds of hydrogels. We systematically studied the characters of the hydrogels using Fourier transform infrared spectroscopy analysis of the pectin dialdehyde, CMC and the hydrogels, and also X-ray diffractometry and scanning electron microscopy analysis of the instrument of the hydrogels. Equilibrium swelling showed that the gels retained about 88-93% water. The water vapor transmission rate (WVTR) and the evaporation of water from gels showed that such hydrogels were optimal for maintaining a moist environment conducive for wound healing. Examination of the hemolytic potential showed that the hydrogels were nonhemolytic in nature. The hydrogels were non-toxic and blood-compatible. This hydrogel prepared from oxidized pectin and CMC without employing any extraneous cross-linking agents is expected to have potential as wound-dressing material.

  3. The Influence of Chitosan Cross-linking on the Properties of Alginate Microparticles with Metformin Hydrochloride—In Vitro and In Vivo Evaluation

    Directory of Open Access Journals (Sweden)

    Marta Szekalska

    2017-01-01

    Full Text Available Sodium alginate is a polymer with unique ability to gel with different cross-linking agents in result of ionic and electrostatic interactions. Chitosan cross-linked alginate provides improvement of swelling and mucoadhesive properties and might be used to design sustained release dosage forms. Therefore, the aim of this research was to develop and evaluate possibility of preparing chitosan cross-linked alginate microparticles containing metformin hydrochloride by the spray-drying method. In addition, influence of cross-linking agent on the properties of microparticles was evaluated. Formulation of microparticles prepared by the spray drying of 2% alginate solution cross-linked by 0.1% chitosan was characterized by good mucoadhesive properties, high drug loading and prolonged metformin hydrochloride release. It was shown that designed microparticles reduced rat glucose blood level, delayed absorption of metformin hydrochloride and provided stable plasma drug concentration. Additionally, histopathological studies of pancreas, liver and kidneys indicated that all prepared microparticles improved degenerative changes in organs of diabetic rats. Moreover, no toxicity effect and no changes in rats behavior after oral administration of chitosan cross-linked alginate microparticles were noted.

  4. The Influence of Chitosan Cross-linking on the Properties of Alginate Microparticles with Metformin Hydrochloride-In Vitro and In Vivo Evaluation.

    Science.gov (United States)

    Szekalska, Marta; Sosnowska, Katarzyna; Zakrzeska, Agnieszka; Kasacka, Irena; Lewandowska, Alicja; Winnicka, Katarzyna

    2017-01-22

    Sodium alginate is a polymer with unique ability to gel with different cross-linking agents in result of ionic and electrostatic interactions. Chitosan cross-linked alginate provides improvement of swelling and mucoadhesive properties and might be used to design sustained release dosage forms. Therefore, the aim of this research was to develop and evaluate possibility of preparing chitosan cross-linked alginate microparticles containing metformin hydrochloride by the spray-drying method. In addition, influence of cross-linking agent on the properties of microparticles was evaluated. Formulation of microparticles prepared by the spray drying of 2% alginate solution cross-linked by 0.1% chitosan was characterized by good mucoadhesive properties, high drug loading and prolonged metformin hydrochloride release. It was shown that designed microparticles reduced rat glucose blood level, delayed absorption of metformin hydrochloride and provided stable plasma drug concentration. Additionally, histopathological studies of pancreas, liver and kidneys indicated that all prepared microparticles improved degenerative changes in organs of diabetic rats. Moreover, no toxicity effect and no changes in rats behavior after oral administration of chitosan cross-linked alginate microparticles were noted.

  5. Macrophage response to cross-linked and conventional UHMWPE.

    Science.gov (United States)

    Sethi, Rajiv K; Neavyn, Mark J; Rubash, Harry E; Shanbhag, Arun S

    2003-07-01

    To prevent wear debris-induced osteolysis and aseptic loosening, cross-linked ultra-high molecular weight polyethylene's (UHMWPE) with improved wear resistance have been developed. Hip simulator studies have demonstrated very low wear rates with these new materials leading to their widespread clinical use. However, the biocompatibility of this material is not known. We studied the macrophage response to cross-linked UHMWPE (XLPE) and compared it to conventional UHMWPE (CPE) as well as other clinically used orthopaedic materials such as titanium-alloy (TiAlV) and cobalt-chrome alloy (CoCr). Human peripheral blood monocytes and murine macrophages, as surrogates for cells mediating peri-implant inflammation, were cultured onto custom designed lipped disks fabricated from the test materials to isolate cells. Culture supernatants were collected at 24 and 48h and analyzed for cytokines such as IL-1alpha, IL-1beta, TNF-alpha and IL-6. Total RNA was extracted from adherent cells and gene expression was analyzed using qualitative RT-PCR. In both in vitro models, macrophages cultured on cross-linked and conventional polyethylene released similar levels of cytokines, which were also similar to levels on control tissue culture dishes. Macrophages cultured on TiAlV and CoCr-alloy released significantly higher levels of cytokines. Human monocytes from all donors varied in the magnitude of cytokines released when cultured on identical surfaces. The variability in individual donor responses to TiAlV and CoCr surfaces may reflect how individuals respond differently to similar stimuli and perhaps reveal a predisposed sensitivity to particular materials.

  6. DNA interstrand cross-linking by a mycotoxic diepoxide.

    Science.gov (United States)

    Millard, J T; Katz, J L; Goda, J; Frederick, E D; Pierce, S E; Speed, T J; Thamattoor, D M

    2004-06-01

    The diepoxide mycotoxin (2R, 3R, 8R, 9R)-4,6-decadiyne-2,3:8,9-diepoxy-1,10-diol (repandiol) was both isolated from the mushroom Hydnum repandum and synthesized de novo. Repandiol was found to form interstrand cross-links within a restriction fragment of DNA, linking deoxyguanosines on opposite strands primarily within the 5'-GNC and 5'-GNNC sequences preferred by diepoxyoctane. However, repandiol was a significantly less efficient cross-linker than either of the diepoxyalkanes (diepoxyoctane and diepoxybutane) to which it was compared.

  7. Newer protocols and future in collagen cross-linking

    Directory of Open Access Journals (Sweden)

    Arthur B Cummings

    2013-01-01

    Full Text Available Corneal Cross-Linking (CXL is an established surgical procedure for the treatment of corneal disorders such as corneal ectasia and keratoconus. This method of treatment stabilises the corneal structure and increases rigidity, reducing the requirement for corneal transplantation. Since its development, many scientific studies have been conducted to investigate ways of improving the procedure. Biomechanical stability of the cornea after exposure to UV-A light, and the effect of shortening procedure time has been some of the many topics explored

  8. Cross-linked leucaena seed gum matrix: an affinity chromatography tool for galactose-specific lectins.

    Science.gov (United States)

    Seshagirirao, Kottapalli; Leelavathi, Chaganti; Sasidhar, Vemula

    2005-05-31

    A cross-linked leucaena (Leucaena leucocephala) seed gum (CLLSG) matrix was prepared for the isolation of galactose-specific lectins by affinity chromatography. The matrix was evaluated for affinity with a known galactose-specific lectin from the seeds of snake gourd (Trichosanthes anguina). The matrix preparation was simple and inexpensive when compared to commercial galactose-specific matrices (i.e. about 1.5 US dollars/100 ml of matrix). The current method is also useful for the demonstration of the affinity chromatography technique in laboratories. Since leucaena seeds are abundant and inexpensive, and the matrix preparation is easy, CLLSG appears to be a promising tool for the separation of galactose-specific lectins.

  9. Continuous Sensing Photonic Lab-on-a-Chip Platform Based on Cross-Linked Enzyme Crystals.

    Science.gov (United States)

    Conejero-Muriel, Mayte; Rodríguez-Ruiz, Isaac; Verdugo-Escamilla, Cristóbal; Llobera, Andreu; Gavira, José A

    2016-12-06

    Microfluidics or lab-on-a-chip technology offer clear advantages over conventional systems such as a dramatic reduction of reagent consumption or a shorter analysis time, which are translated into cost-effective systems. In this work, we present a photonic enzymatic lab-on-a-chip reactor based on cross-linked enzyme crystals (CLECs), able to work in continuous flow, as a highly sensitive, robust, reusable, and stable platform for continuous sensing with superior performance as compared to the state of the art. The microreactor is designed to facilitate the in situ crystallization and crystal cross-linking generating enzymatically active material that can be stored for months/years. Thus, and by means of monolithically integrated micro-optics elements, continuous enzymatic reactions can be spectrophotometrically monitored. Lipase, an enzyme with industrial significance for catalyzed transesterification, hydrolysis, and esterification reactions, is used to demonstrate the potential of the microplatforms as both a continuous biosensor and a microreactor for the synthesis of high value compounds.

  10. Probing native protein structures by chemical cross-linking, mass spectrometry, and bioinformatics.

    Science.gov (United States)

    Leitner, Alexander; Walzthoeni, Thomas; Kahraman, Abdullah; Herzog, Franz; Rinner, Oliver; Beck, Martin; Aebersold, Ruedi

    2010-08-01

    Chemical cross-linking of reactive groups in native proteins and protein complexes in combination with the identification of cross-linked sites by mass spectrometry has been in use for more than a decade. Recent advances in instrumentation, cross-linking protocols, and analysis software have led to a renewed interest in this technique, which promises to provide important information about native protein structure and the topology of protein complexes. In this article, we discuss the critical steps of chemical cross-linking and its implications for (structural) biology: reagent design and cross-linking protocols, separation and mass spectrometric analysis of cross-linked samples, dedicated software for data analysis, and the use of cross-linking data for computational modeling. Finally, the impact of protein cross-linking on various biological disciplines is highlighted.

  11. Size-dependent release of fluorescent macromolecules and nanoparticles from radically cross-linked hydrogels.

    Science.gov (United States)

    Henke, Matthias; Brandl, Ferdinand; Goepferich, Achim M; Tessmar, Joerg K

    2010-02-01

    Hydrogels play an important role in drug delivery and tissue engineering applications due to their excellent biocompatibility and their variable mechanical and physical properties, which allow their optimization for many different aspects of the intended use. In this study, we examined the suitability of poly(ethylene glycol) (PEG)-based hydrogels as release systems for nanometer-sized drugs or drug carriers, like nanoparticles, using the radically cross-linkable oligo(poly(ethylene glycol)fumarate) (OPF) together with two cross-linking agents. Different fluorescent nanoparticulate probes with respect to size and physical structure were incorporated in the cross-linked hydrogels, and the obtained release profiles were correlated with the physical properties and the chemical structure of the gels, indicating a strong dependence of the release on the chosen PEG prepolymers. The prepared hydrogels were characterized by oscillatory rheometry and swelling experiments. Release experiments as well as diffusion measurements using fluorescence recovery after photobleaching showed the great potential of this type of hydrogels for the preparation of adjustable release systems by altering the molecular weights of the used PEG molecules.

  12. Swelling Studies of Chitosan-Gelatin Films Cross-Linked by Sulfate

    Institute of Scientific and Technical Information of China (English)

    Xiao Ling; Yu Zu-yu; Yang Chao; Zhu Hua-yue; Du Yu-min

    2004-01-01

    Swelling properties of chitosan-gelatin films cross-linked by sulfate were investigated. Sulfate cross-linked chitosan-gelatin films (SCG) were prepared simply by dipping chitosan-gelatin films into sodium sulfate solution. The swelling behavior of SCG was investigated as a function of pH and ionic strength. Under acidic conditions pH less than 4, SCG swelled less than 120%, while under the conditions pH larger than 7.4, SCG swelled very significantly, the swelling ratio was over 350%. Sodium chloride weakened the electrostatic interaction between sulfate and amine ions of chitosan and gelatin, therefore facilitated the film swelling. The swelling ratio increased with increasing sodium chloride concentration, the SCG dissociated in the sodium chloride concentration of 0.20 mol·L-1. The parameters of film preparation such as sulfate concentration, dipping time, sulfate solution pH, influenced the film swelling behavior. The lower concentration and the higher pH of sulfate solution resulted in a larger swelling ratio.

  13. Entrapment of cross-linked cellulase colloids in alginate beads for hydrolysis of cellulose.

    Science.gov (United States)

    Nguyen, Le Truc; Lau, Yun Song; Yang, Kun-Lin

    2016-09-01

    Entrapment of enzymes in calcium alginate beads is a popular enzyme immobilization method. However, leaching of immobilized enzymes from the alginate beads is a common problem because enzyme molecules are much smaller than the pore size of alginate beads (∼200nm). To address this issue, we employ a millifluidic reactor to prepare cross-linked cellulase aggregate (XCA) colloids with a uniform size (∼300nm). Subsequently, these colloids are immobilized in calcium alginate beads as biocatalysts to hydrolyze cellulose substrates. By using fluorescent microscopy, we conclude that the immobilized XCA colloids distribute uniformly inside the beads and do not leach out from the beads after long-term incubation. Meanwhile, the pore size of the alginate beads is big enough for the cellulose substrates and fibers to diffuse into the beads for hydrolysis. For example, palm oil fiber and microcrystalline cellulose can be hydrolyzed within 48h and release reducing sugar concentrations up to 2.48±0.08g/l and 4.99±0.09g/l, respectively. Moreover, after 10 cycles of hydrolysis, 96.4% of the XCA colloids remain inside the alginate beads and retain 67% of the original activity. In contrast, free cellulase immobilized in the alginate beads loses its activity completely after 10 cycles. The strategy can also be used to prepare other types of cross-linked enzyme aggregates with high uniformity. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Cross-linked comb-shaped anion exchange membranes with high base stability

    Energy Technology Data Exchange (ETDEWEB)

    Li, NW; Wang, LZ; Hickner, M

    2014-01-01

    A unique one-step cross-linking strategy that connects quaternary ammonium centers using Grubbs II-catalyzed olefin metathesis was developed. The cross-linked anion exchange membranes showed swelling ratios of less than 10% and hydroxide conductivities of 18 to 40 mS cm(- 1). Cross-linking improved the membranes' stability to hydroxide degradation compared to their non-cross-linked analogues.

  15. Cross-linking e segmento de anel corneano intraestromal

    Directory of Open Access Journals (Sweden)

    Adimara da Candelaria Renesto

    2011-02-01

    Full Text Available O cross-linking corneano é um procedimento usado para a estabilização mecânica e aumento da rigidez corneana em pacientes com ceratocone (reduzindo a possibilidade de progressão, e também em processos inflamatórios de afinamento corneano. Os segmentos de anéis corneanos intraestromais têm como princípio o aplanamento central da córnea. Inicialmente utilizados para correção de baixa miopia, a principal indicação atual é em pacientes com ceratocone, para melhorar a acuidade visual não corrigida, a acuidade visual corrigida e permitir uma melhor tolerância ao uso de lentes de contato como também retardar a necessidade de um transplante de córnea. O objetivo deste artigo é revisar algumas publicações relacionadas ao cross-linking corneano e à inserção do segmento de anel intraestromal, apresentando suas indicações, resultados e complicações relatadas até o momento.

  16. Fiber optic immunosensor for cross-linked fibrin concentration

    Science.gov (United States)

    Moskowitz, Samuel E.

    2000-08-01

    Working with calcium ions in the blood, platelets produce thromboplastin which transforms prothrombin into thrombin. Removing peptides, thrombin changes fibrinogen into fibrin. Cross-linked insoluble fibrin polymers are solubilized by enzyme plasmin found in blood plasma. Resulting D-dimers are elevated in patients with intravascular coagulation, deep venous thrombosis, pulmonary embolism, myocardial infarction, multiple trauma, cancer, impaired renal and liver functions, and sepsis. Consisting principally of a NIR 780 nm GaAlAs laser diode and a 800 nm avalanche photodiode (APD), the fiber-optic immunosensor can determined D-dimer concentration to levels detected by a second antibody which is labeled with NN 382 fluorescent dye. An evanescent wave traveling on an excitation optical fiber excites the antibody-antigen fluorophore complex. Concentration of cross-linked fibrin is directly proportional to the APD measured intensity of fluorescence. NIR fluorescence has advantages of low background interference, short fluorescence lifetime, and large difference between excitation and emission peaks. Competitive ELISA test for D-dimer concentration requires trained personnel performing a time consuming operation.

  17. Adsorption of methyl orange onto protonated cross-linked chitosan

    Directory of Open Access Journals (Sweden)

    Ruihua Huang

    2017-01-01

    Full Text Available The adsorption of methyl orange (MO from aqueous solutions on protonated cross-linked chitosan was studied in a batch system. The results showed that the adsorption of MO onto protonated cross-linked chitosan was affected significantly by initial MO concentration, adsorbent dosage, adsorption temperature, and contact time. The pH value of solution had a minor impact on the adsorption of MO in a pH range of 1.0–9.1. The equilibrium isotherms at different temperatures (293, 303, and 313 K and pH values (4.5, 6.7, and 9.1 were investigated. Langmuir model was able to describe these Equilibrium data fitted perfectly. The maximum monolayer adsorption capacities obtained from the Langmuir model were 89.29, 130.9, and 180.2 mg/g at 293, 303, and 313 K, respectively. Adsorption kinetics at different concentrations (100, 200 and 300 mg/L and pH values (4.5, 6.7 and 9.1 were also studied. The kinetics was correlated well with the pseudo second-order model.

  18. Microbial Keratitis After Collagen Cross-linking Treatment

    Directory of Open Access Journals (Sweden)

    Banu Torun Acar

    2012-07-01

    Full Text Available A 33-year-old woman presented with pain, redness, and diminution of vision that occurred 2 days after collagen cross-linking had been performed for keratoconus in the right eye. Culture results from the patient's contact lens and corneal scrapings were positive for Staphylococcus epidermidis. According to the results of antibiotic susceptibility testing, the patient was treated with hourly topical fortified vancomycin and exocin. Before collagen cross-linking, the best-corrected visual acuity (BCVA was 4/10, the manifest refraction was -7.00 -1.755 3°. Four months after the procedure, the BCVA was 4/10, the manifest refraction was -5.50 -1.75 10°. Slit-lamp examination revealed a mild residual haze in the upper midperipheral cornea, and stromal opacities had disappeared. Collagen crosslinking is less invasive compared to other methods for treatment of keratoconus, but epithelial debridement and bandage contact lens wearing may lead to the development of bacterial keratitis. (Turk J Oph thal mol 2012; 42: 300-2

  19. One-step electrospinning of cross-linked chitosan fibers.

    Science.gov (United States)

    Schiffman, Jessica D; Schauer, Caroline L

    2007-09-01

    Chitin is a nitrogen-rich polysaccharide that is abundant in crustaceans, mollusks, insects, and fungi and is the second most abundant organic material found in nature next to cellulose. Chitosan, the N-deacetylated derivative of chitin, is environmentally friendly, nontoxic, biodegradable, and antibacterial. Fibrous mats are typically used in industries for filter media, catalysis, and sensors. Decreasing fiber diameters within these mats causes many beneficial effects such as increased specific surface area to volume ratios. When the intrinsically beneficial effects of chitosan are combined with the enhanced properties of nanofibrous mats, applications arise in a wide range of fields, including medical, packaging, agricultural, and automotive. This is particularly important as innovative technologies that focus around bio-based materials are currently of high urgency, as they can decrease dependencies on fossil fuels. We have demonstrated that Schiff base cross-linked chitosan fibrous mats can be produced utilizing a one-step electrospinning process that is 25 times faster and, therefore, more economical than a previously reported two-step vapor-cross-linking method. These fibrous mats are insoluble in acidic, basic, and aqueous solutions for 72 h. Additionally, this improved production method results in a decreased average fiber diameter, which measures 128 +/- 40 nm. Chemical and structural analyses were conducted utilizing Fourier transform infrared spectroscopy, solubility studies, and scanning electron microscopy.

  20. Tea derived galloylated polyphenols cross-link purified gastrointestinal mucins.

    Directory of Open Access Journals (Sweden)

    Pantelis Georgiades

    Full Text Available Polyphenols derived from tea are thought to be important for human health. We show using a combination of particle tracking microrheology and small-angle neutron scattering that polyphenols acts as cross-linkers for purified gastrointestinal mucin, derived from the stomach and the duodenum. Both naturally derived purified polyphenols, and green and black tea extracts are shown to act as cross-linkers. The main active cross-linking component is found to be the galloylated forms of catechins. The viscosity, elasticity and relaxation time of the mucin solutions experience an order of magnitude change in value upon addition of the polyphenol cross-linkers. Similarly small-angle neutron scattering experiments demonstrate a sol-gel transition with the addition of polyphenols, with a large increase in the scattering at low angles, which is attributed to the formation of large scale (>10 nm heterogeneities during gelation. Cross-linking of mucins by polyphenols is thus expected to have an impact on the physicochemical environment of both the stomach and duodenum; polyphenols are expected to modulate the barrier properties of mucus, nutrient absorption through mucus and the viscoelastic microenvironments of intestinal bacteria.

  1. Magnetic Cross-Linked Enzyme Aggregates (mCLEAs) of Candida antarctica lipase: an efficient and stable biocatalyst for biodiesel synthesis.

    Science.gov (United States)

    Cruz-Izquierdo, Álvaro; Picó, Enrique A; López, Carmen; Serra, Juan L; Llama, María J

    2014-01-01

    Enzyme-catalyzed production of biodiesel is the object of extensive research due to the global shortage of fossil fuels and increased environmental concerns. Herein we report the preparation and main characteristics of a novel biocatalyst consisting of Cross-Linked Enzyme Aggregates (CLEAs) of Candida antarctica lipase B (CALB) which are covalently bound to magnetic nanoparticles, and tackle its use for the synthesis of biodiesel from non-edible vegetable and waste frying oils. For this purpose, insolubilized CALB was covalently cross-linked to magnetic nanoparticles of magnetite which the surface was functionalized with -NH2 groups. The resulting biocatalyst combines the relevant catalytic properties of CLEAs (as great stability and feasibility for their reutilization) and the magnetic character, and thus the final product (mCLEAs) are superparamagnetic particles of a robust catalyst which is more stable than the free enzyme, easily recoverable from the reaction medium and reusable for new catalytic cycles. We have studied the main properties of this biocatalyst and we have assessed its utility to catalyze transesterification reactions to obtain biodiesel from non-edible vegetable oils including unrefined soybean, jatropha and cameline, as well as waste frying oil. Using 1% mCLEAs (w/w of oil) conversions near 80% were routinely obtained at 30°C after 24 h of reaction, this value rising to 92% after 72 h. Moreover, the magnetic biocatalyst can be easily recovered from the reaction mixture and reused for at least ten consecutive cycles of 24 h without apparent loss of activity. The obtained results suggest that mCLEAs prepared from CALB can become a powerful biocatalyst for application at industrial scale with better performance than those currently available.

  2. Magnetic Cross-Linked Enzyme Aggregates (mCLEAs of Candida antarctica lipase: an efficient and stable biocatalyst for biodiesel synthesis.

    Directory of Open Access Journals (Sweden)

    Álvaro Cruz-Izquierdo

    Full Text Available Enzyme-catalyzed production of biodiesel is the object of extensive research due to the global shortage of fossil fuels and increased environmental concerns. Herein we report the preparation and main characteristics of a novel biocatalyst consisting of Cross-Linked Enzyme Aggregates (CLEAs of Candida antarctica lipase B (CALB which are covalently bound to magnetic nanoparticles, and tackle its use for the synthesis of biodiesel from non-edible vegetable and waste frying oils. For this purpose, insolubilized CALB was covalently cross-linked to magnetic nanoparticles of magnetite which the surface was functionalized with -NH2 groups. The resulting biocatalyst combines the relevant catalytic properties of CLEAs (as great stability and feasibility for their reutilization and the magnetic character, and thus the final product (mCLEAs are superparamagnetic particles of a robust catalyst which is more stable than the free enzyme, easily recoverable from the reaction medium and reusable for new catalytic cycles. We have studied the main properties of this biocatalyst and we have assessed its utility to catalyze transesterification reactions to obtain biodiesel from non-edible vegetable oils including unrefined soybean, jatropha and cameline, as well as waste frying oil. Using 1% mCLEAs (w/w of oil conversions near 80% were routinely obtained at 30°C after 24 h of reaction, this value rising to 92% after 72 h. Moreover, the magnetic biocatalyst can be easily recovered from the reaction mixture and reused for at least ten consecutive cycles of 24 h without apparent loss of activity. The obtained results suggest that mCLEAs prepared from CALB can become a powerful biocatalyst for application at industrial scale with better performance than those currently available.

  3. Thermally Cross-Linked Anion Exchange Membranes from Solvent Processable Isoprene Containing Ionomers

    Science.gov (United States)

    2015-01-15

    capacities (IECs). Solution cast membranes were thermally cross- linked to form anion exchange membranes. Cross-linking was achieved by taking advantage...distribution is unlimited. Thermally Cross-Linked Anion Exchange Membranes from Solvent Processable Isoprene Containing Ionomers The views...Box 12211 Research Triangle Park, NC 27709-2211 Anion Exchnage Membrane, Polymer synthesis, Morphology, Anion Conductivity REPORT DOCUMENTATION PAGE

  4. Small Strain Topological Effects of Biopolymer Networks with Rigid Cross-Links

    NARCIS (Netherlands)

    Zagar, G.; Onck, P. R.; Van der Giessen, E.; Garikipati, K; Arruda, EM

    2010-01-01

    Networks of cross-linked filamentous biopolymers form topological structures characterized by L, T and X cross-link types of connectivity 2, 3 and 4, respectively. The distribution of cross-links over these three types proofs to be very important for the initial elastic shear stiffness of isotropic

  5. Cross-linking of dermal sheep collagen using a water-soluble carbodiimide

    NARCIS (Netherlands)

    Olde Damink, L.H.H.; Dijkstra, P.J.; Luyn, van M.J.A.; Wachem, van P.B.; Nieuwenhuis, P.; Feijen, J.

    1996-01-01

    A cross-linking method for collagen-based biomaterials was developed using the water-soluble carbodiimide 1-ethyl-3-(3-dimethyl aminopropyl)carbodiimide hydrochloride (EDC). Cross-linking using EDC involves the activation of carboxylic acid groups to give O-acylisourea groups, which form cross-links

  6. Epoxy Cross-Linked Collagen and Collagen-Laminin Peptide Hydrogels as Corneal Substitutes

    Directory of Open Access Journals (Sweden)

    May Griffith

    2013-08-01

    Full Text Available A bi-functional epoxy-based cross-linker, 1,4-Butanediol diglycidyl ether (BDDGE, was investigated in the fabrication of collagen based corneal substitutes. Two synthetic strategies were explored in the preparation of the cross-linked collagen scaffolds. The lysine residues of Type 1 porcine collagen were directly cross-linked using l,4-Butanediol diglycidyl ether (BDDGE under basic conditions at pH 11. Alternatively, under conventional methodology, using both BDDGE and 1-Ethyl-3-(3-dimethyl aminopropyl carbodiimide (EDC/N-hydroxysuccinimide (NHS as cross-linkers, hydrogels were fabricated under acidic conditions. In this latter strategy, Cu(BF42·XH2O was used to catalyze the formation of secondary amine bonds. To date, we have demonstrated that both methods of chemical cross-linking improved the elasticity and tensile strength of the collagen implants. Differential scanning calorimetry and biocompatibility studies indicate comparable, and in some cases, enhanced properties compared to that of the EDC/NHS controls. In vitro studies showed that human corneal epithelial cells and neuronal progenitor cell lines proliferated on these hydrogels. In addition, improvement of cell proliferation on the surfaces of the materials was observed when neurite promoting laminin epitope, IKVAV, and adhesion peptide, YIGSR, were incorporated. However, the elasticity decreased with peptide incorporation and will require further optimization. Nevertheless, we have shown that epoxy cross-linkers should be further explored in the fabrication of collagen-based hydrogels, as alternatives to or in conjunction with carbodiimide cross-linkers.

  7. Thermo-responsive shell cross-linked PMMA-b-P(NIPAAm-co-NAS) micelles for drug delivery.

    Science.gov (United States)

    Chang, Cong; Wei, Hua; Wu, De-Qun; Yang, Bin; Chen, Ni; Cheng, Si-Xue; Zhang, Xian-Zheng; Zhuo, Ren-Xi

    2011-11-28

    Thermo-responsive amphiphilic poly(methyl methacrylate)-b-poly(N-isopropylacrylamide-co-N-acryloxysuccinimide) (PMMA-b-P(NIPAAm-co-NAS)) block copolymer was synthesized by successive RAFT polymerizations. The uncross-linked micelles were facilely prepared by directly dissolving the block copolymer in an aqueous medium, and the shell cross-linked (SCL) micelles were further fabricated by the addition of ethylenediamine as a di-functional cross-linker into the micellar solution. Optical absorption measurements showed that the LCST of uncross-linked and cross-linked micelles was 31.0°C and 40.8°C, respectively. Transmission electron microscopy (TEM) showed that both uncross-linked and cross-linked micelles exhibited well-defined spherical shape in aqueous phase at room temperature, while the SCL micelles were able to retain the spherical shape with relatively smaller dimension even at 40°C due to the cross-linked structure. In vitro drug release study demonstrated a slower and more sustained drug release behavior from the SCL micelles at high temperature as compared with the release profile of uncross-linked micelles, indicating the great potential of SCL micelles developed herein as novel smart carriers for controlled drug release.

  8. Fabrication of cross-linked hydrazone covalent organic frameworks by click chemistry and application to solid phase microextraction.

    Science.gov (United States)

    Wu, Mingxue; Chen, Gang; Ma, Jiutong; Liu, Ping; Jia, Qiong

    2016-12-01

    Covalent organic frameworks (COFs) are an emerging class of porous organic frameworks with diverse promising applications. Herein, we presented the first example of cross-linked hydrazone COFs (cross-linked COFs) coating via thiol-ene click chemistry for solid phase microextraction (SPME). Strong covalent bonds and interlayer of the prepared networks ensured the adsorption capacity and durability of the novel SPME fiber. π-π conjugated structure existed because of abundant phenyl rings and -C=N groups in the cross-lined COFs. A series of characterizations indicated that the cross-linked COFs possessed large surface areas, high porosities and stabilities as well as hydrophobicities. The fiber was applied to SPME of pesticide residues coupled with gas chromatography with an electron capture detector (GC-ECD). Under the optimum experimental conditions, enhancement factors in the range of 2190-10,998 were obtained, illustrating that the cross-linked COFs possessed remarkable preconcentration ability. The low detection limits of 0.0003-0.0023ngkg(-1) were achieved with relative standard deviations (RSDs) in the range of 3.4-7.6% (intra-batch) and 5.7-11.6% (inter-batch), respectively. Recovery values in the range of 78.2-107.0% were obtained when the SPME-GC method was applied to the analysis of pesticides in cucumber samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Novel Spray Dried Glycerol 2-Phosphate Cross-Linked Chitosan Microparticulate Vaginal Delivery System—Development, Characterization and Cytotoxicity Studies

    Science.gov (United States)

    Szymańska, Emilia; Szekalska, Marta; Czarnomysy, Robert; Lavrič, Zoran; Srčič, Stane; Miltyk, Wojciech; Winnicka, Katarzyna

    2016-01-01

    Chitosan microparticulate delivery systems containing clotrimazole were prepared by a spray drying technique using glycerol 2-phosphate as an ion cross-linker. The impact of a cross-linking ratio on microparticle characteristics was evaluated. Drug-free and drug-loaded unmodified or ion cross-linked chitosan microparticles were examined for the in vitro cytotoxicity in VK2/E6E7 human vaginal epithelial cells. The presence of glycerol 2-phosphate influenced drug loading and encapsulation efficacy in chitosan microparticles. By increasing the cross-linking ratio, the microparticles with lower diameter, moisture content and smoother surface were observed. Mucoadhesive studies displayed that all formulations possessed mucoadhesive properties. The in vitro release profile of clotrimazole was found to alter considerably by changing the glycerol 2-phosphate/chitosan ratio. Results from cytotoxicity studies showed occurrence of apoptotic cells in the presence of chitosan and ion cross-linked chitosan microparticles, followed by a loss of membrane potential suggesting that cell death might go through the mitochondrial apoptotic pathway. PMID:27690062

  10. Characterization of Cross-linked Alkaline Lignin/Poly (Vinyl Alcohol Film with a Formaldehyde Cross-linker

    Directory of Open Access Journals (Sweden)

    Ling Su

    2014-06-01

    Full Text Available On the basis of previous experiments, industrial alkaline lignin/poly (vinyl alcohol (PVOH cross-linked films, industrial alkaline lignin/poly (vinyl alcohol blend films, and neat poly (vinyl alcohol films were prepared by casting. The films were investigated by Fourier transform infra-red spectroscopy (FTIR, X-ray diffraction (XRD, thermogravimetry analysis (TGA, and dynamic mechanical analysis (DMA. The water contact angles for the three kinds of films were studied as well. The crosslinking reaction between alkaline lignin and PVOH was strong, which was attributed to the high hydrolysis degree of PVOH and the high reactivity of formaldehyde. Compared with the neat PVOH film, the crystallinity of the cross-linked film decreased slightly; the thermal stability of the cross-linked film was higher; DMA analysis showed that the Tg and the tanδ magnitude of the alkaline lignin/PVOH reaction film both decreased slightly. Lignin and the cross-linking reaction both improved the water resistance of films. Therefore, this research has provided a detailed analysis of the characterization of the films while exploring the potential of direct usage of industrial alkaline lignin in polymer materials.

  11. PERVAPORATION PROPERTIES OF PDMS MEMBRANES CURED WITH DIFFERENT CROSS-LINKING REAGENTS FOR ETHANOL CONCENTRATION FROM AQUEOUS SOLUTIONS

    Institute of Scientific and Technical Information of China (English)

    Xia Zhan; Ji-ding Li; Jun-qi Huang; Cui-xian Chen

    2009-01-01

    Ethanol perm-selective PDMS/PVDF composite membranes were prepared by curing polydimethylsiloxane (PDMS) with various cross-linking reagents, such as tetraethoxylsilane (TEOS), γ-aminopropyltriethoxylsilane (APTEOS), phenyltrimethoxylsilane (PTMOS) and octyltrimethoxylsilane (OTMOS) as well. The cross-linking density and surface properties of the PDMS active layer were adjusted by varying cross-linking reagents. The pervaporation performance of PDMS membranes cured with different cross-linking reagents was investigated in detail. As temperature increased, the total flux of the four kinds of membranes all increased exponentially, and the separation factor followed a reversed order. The increase of thickness of PDMS layers depressed the total flux of composite membranes and had no obvious effect on selectivity of ethanol. It was found that the composite membrane cured by PTMOS showed much better separation performance compared with other membranes. A resistance-in-series model was used to investigate and estimate the overall mass transfer coefficients and boundary layer mass transfer coefficients of ethanol and water according to experimental results. The measured diffusivities of ethanol and water in PDMS membranes had a magnitude of 10-10 m2·s-1 and 10-11 m2·s-1 at 313.15 K, respectively.

  12. Cross-linking immunoprecipitation-MS (xIP-MS): Topological Analysis of Chromatin-associated Protein Complexes Using Single Affinity Purification.

    Science.gov (United States)

    Makowski, Matthew M; Willems, Esther; Jansen, Pascal W T C; Vermeulen, Michiel

    2016-03-01

    In recent years, cross-linking mass spectrometry has proven to be a robust and effective method of interrogating macromolecular protein complex topologies at peptide resolution. Traditionally, cross-linking mass spectrometry workflows have utilized homogenous complexes obtained through time-limiting reconstitution, tandem affinity purification, and conventional chromatography workflows. Here, we present cross-linking immunoprecipitation-MS (xIP-MS), a simple, rapid, and efficient method for structurally probing chromatin-associated protein complexes using small volumes of mammalian whole cell lysates, single affinity purification, and on-bead cross-linking followed by LC-MS/MS analysis. We first benchmarked xIP-MS using the structurally well-characterized phosphoribosyl pyrophosphate synthetase complex. We then applied xIP-MS to the chromatin-associated cohesin (SMC1A/3), XRCC5/6 (Ku70/86), and MCM complexes, and we provide novel structural and biological insights into their architectures and molecular function. Of note, we use xIP-MS to perform topological studies under cell cycle perturbations, showing that the xIP-MS protocol is sufficiently straightforward and efficient to allow comparative cross-linking experiments. This work, therefore, demonstrates that xIP-MS is a robust, flexible, and widely applicable methodology for interrogating chromatin-associated protein complex architectures.

  13. Cross-linked hyaluronic acid in pressure ulcer prevention.

    Science.gov (United States)

    Beniamino, P; Vadalà, M; Laurino, C

    2016-07-02

    Long-term bedridden patients are at high risk of acquring pressure ulcers (PUs). In this group of patients, prevention is necessary to cut the health costs, improve quality of life and reduce the mortality. Here, we evaluated the effectiveness of a cross-linked hyaluronic acid (HA) as plastic bulking-agent filling and remodelling the deep dermis and subcutaneous space of the skin areas exposed to the risk of necrosis. Our work hypothesis has been to inflate a sub-dermal elastic cushion, filled with a natural ECM component, with the aim to induce a stronger tissue background resistant to the ulcerative process. All the patients had an increased risk of PUs, at the sacral, ileum or heel skin. Patients were being nursed accordingly to the standard orthopaedic ward management with a pressure relieveing air mattress. The standard protocol consisted in body mobilisation every 3 hours, 24 hours a day and accurate cleaning of the skin with liquid soap and water without any towel friction and without adding any cream or lotion for the skin protection. Our filling protocol enclosed: accurate disinfection of the skin to be injected with povidone-iodine solution, followed by a local anaesthesia with 28G 13 mm needle, injecting 1.5 ml of 1% xylocaine. Then slow, deep, subcutaneous injection of cross-linked HA was performed with a 18G long needle, in order to deliver a homogeneous, soft gel layer underneath and around the whitish erythematous skin edges at risk of ulceration. Patients' tolerability of the compound and adverse events were also recorded. There were 15 patients (78-94 years old) who participated in the study. All tolerated the procedure very well and no serious side effects were declared. No skin pressure ulceration was detected in the four weeks follow-up Conclusion: We have demonstrated the safety and tolerability of a cross-linked HA subdermal injection in PUs prevention. The compound stratifies in a soft, elastic, interstitial bulk into the deep dermis, thus

  14. Physicochemical characterization of chitosan/nylon6/polyurethane foam chemically cross-linked ternary blends.

    Science.gov (United States)

    Jayakumar, S; Sudha, P N

    2013-03-15

    Chitosan/nylon6/polyurethane foam (CS/Ny6/PUF) ternary blend was prepared and chemically cross-linked with glutaraldehyde. Structural, thermal and morphological studies were performed for the prepared ternary blends. Characterizations of the ternary blends were investigated by Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM). The FTIR results showed that the strong intermolecular hydrogen bonds took place between CS, Ny6 and PUF. TGA and DSC studies reveal that the thermal stability of the blend is enhanced by glutaraldehyde as crosslinking agent. Results of XRD indicated that the relative crystalline of pure CS film was reduced when the polymeric network was reticulated by glutaraldehyde. Finally, the results of scanning electron microscopy (SEM) indicated that the morphology of the blend is rough and heterogeneous, further it confirms the interaction between the functional groups of the blend components.

  15. Physicochemical characterization of chitosan/nylon6/polyurethane foam chemically cross-linked ternary blends

    Science.gov (United States)

    Jayakumar, S.; Sudha, P. N.

    2013-03-01

    Chitosan/nylon6/polyurethane foam (CS/Ny6/PUF) ternary blend was prepared and chemically cross-linked with glutaraldehyde. Structural, thermal and morphological studies were performed for the prepared ternary blends. Characterizations of the ternary blends were investigated by Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM). The FTIR results showed that the strong intermolecular hydrogen bonds took place between CS, Ny6 and PUF. TGA and DSC studies reveal that the thermal stability of the blend is enhanced by glutaraldehyde as crosslinking agent. Results of XRD indicated that the relative crystalline of pure CS film was reduced when the polymeric network was reticulated by glutaraldehyde. Finally, the results of scanning electron microscopy (SEM) indicated that the morphology of the blend is rough and heterogeneous, further it confirms the interaction between the functional groups of the blend components.

  16. Flammability of radiation cross-linked low density polyethylene as an insulating material for wire and cable

    Science.gov (United States)

    Basfar, A. A.

    2002-03-01

    Various formulations of low-density polyethylene blended with ethylene vinyl acetate were prepared to improve the flame retardancy for wire and cable applications. The prepared formulations were cross-linked by γ-rays to 50, 100, 150 and 200 kGy in the presence of trimethylolpropane triacrylate (TMPTA). The effect of thermal aging on mechanical properties of these formulations were investigated. In addition, the influence of various combinations of aluminum trihydroxide and zinc borate as flame retardant fillers on the flammability was explored. Limiting oxygen index (LOI) and average extent of burning were used to characterize the flammability of investigated formulations. An improved flame retardancy of low density polyethylene was achieved by various combinations of flame ratardant fillers and cross-linking by gamma radiation.

  17. Biocatalytic cross-linking of pectic polysaccharides for designed food functionality

    DEFF Research Database (Denmark)

    Zaidel, Dayang Norulfairuz Abang; Meyer, Anne S.

    2012-01-01

    Recent research has demonstrated how cross-linking of pectic polysaccharides to obtain gel formation can be promoted by enzymatic catalysis reactions, and provide opportunities for functional upgrading of pectic polysaccharides present in agro-industrial sidestreams. This review highlights...... the mechanisms of formation of functional pectic polysaccharide cross-links, including covalent cross-links (notably phenolic esters and uronyl ester linkages) and non-covalent, ionic cross-links (which involve calcium and borate ester links). The treatise examines how such cross-links can be designed via...

  18. Preparation of High Strength Silicon Nitride Ceramic Fibers From Polycarbosilane Fibers byγ-Ray Irradiation and Thermal Cross-Linking%γ辐照联合热交联聚碳硅烷先驱丝热解制备高强度氮化硅陶瓷纤维

    Institute of Scientific and Technical Information of China (English)

    黎阳; 高家诚; 许云书

    2014-01-01

    在空气气氛中采用γ射线辐照处理聚碳硅烷(PCS)先驱丝,辐照先驱丝经 Ar中热交联、NH3中热解氨化、N2中高温氮化处理制备了氮化硅陶瓷纤维。研究了热交联处理对辐照先驱丝化学结构、凝胶含量、氨化陶瓷产率、抗拉强度、微观形貌及氧含量的影响。结果表明:热交联处理生成了 Si—CH2—Si 和 Si—O—Si 桥连结构,桥连结构使PCS先驱丝实现凝胶化;热交联处理不仅大幅提高了辐照 PCS先驱丝的氨化陶瓷产率,还提高了热解所得氮化硅陶瓷纤维的抗拉强度,而且还降低了陶瓷纤维的氧含量;吸收剂量为1.0 MGy的辐照丝经热交联处理后,其热解所得氮化硅陶瓷纤维抗拉强度达2.05 GPa,氧质量分数仅为9.5%。%Polycarbosilane (PCS)precursor fibers were irradiated byγ-ray in air.Silicon nitride ceramic fibers were obtained from the irradiated PCS fibers by process of thermal cross-linking treatment in Ar,ammoniation pyrolysis in NH3 and high temperature nitriding treatment in N2 .The effects of thermal cross-linking treatment on chemical structure,gel content,ammoniation ceramic yield,tensile strength,microstructure and oxygen content were studied.The results show that bridge structures of Si—CH2—Si and Si—O—Si are formed in the PCS fibers by thermal cross-linking treatment and make the PCS fibers become gelling.The ammoniation ceramic yield of the irradiated PCS fibers increases sharply after thermal cross-linking treatment.The tensile strength of the silicon nitride ceramic fibers increases sharply, while the oxygen content decreases. After thermal cross-linking treatment,the tensile strength of the silicon nitride ceramic fibers derived from the PCS fibers with absorbed dose of 1.0 MGy reaches 2.05 GPa and the oxygen mass fraction is 9.5%.

  19. Stiffening of semiflexible biopolymers and cross-linked networks

    CERN Document Server

    Van Dillen, T; Van der Giessen, E

    2006-01-01

    We study the mechanical stiffening behavior in two-dimensional (2D) cross-linked networks of semiflexible biopolymer filaments under simple shear. Filamental constituents immersed in a fluid undergo thermally excited bending motions. Pulling out these undulations results in an increase in the axial stiffness. We analyze this stiffening behavior of 2D semiflexible filaments in detail: we first investigate the average, {static} force-extension relation by considering the initially present undulated configuration that is pulled straight under a tensile force, and compare this result with the average response in which undulation dynamics is allowed during pulling, as derived earlier by MacKintosh and coworkers. We will show that the resulting mechanical behavior is rather similar, but with the axial stiffness being a factor 2 to 4 larger in the dynamic model. Furthermore, we study the stretching contribution in case of extensible filaments and show that, for 2D filaments, the mechanical response is dominated by {...

  20. Swelling properties of cross-linked DNA gels.

    Science.gov (United States)

    Costa, Diana; Miguel, M Graça; Lindman, Björn

    2010-07-12

    This work represents our contribution to the field of physical chemistry of DNA gels, and concerns the synthesis and study of novel chemically cross-linked DNA gels. The use of covalent DNA gels is a very promising way to study DNA-cosolute interactions, as well as the dynamic behaviour of DNA and cationic compacting agents, like lipids, surfactants and polycations. Manipulating DNA in new ways, like DNA networks, allows a better understanding and characterization of DNA-cosolute complexes at the molecular level, and also allows us to follow the assembly structures of these complexes. The use of responsive polymer gels for targeted delivery of toxic and/or labile drugs has, during the past few years, shown to be a promising concept. The features found in the proposed system would find applications in a broader field of gel/drug interaction, for the development of controlled release and targeted delivery devices.

  1. Conventional Versus Cross-Linked Polyethylene for Total Hip Arthroplasty.

    Science.gov (United States)

    Surace, Michele F; Monestier, Luca; Vulcano, Ettore; Harwin, Steven F; Cherubino, Paolo

    2015-09-01

    The clinical and radiographic outcomes of 88 patients who underwent primary total hip arthroplasty with either conventional polyethylene or cross-linked polyethylene (XLPE) from the same manufacturer were compared. There were no significant differences between the 2 subpopulations regarding average age, gender, side affected, or prosthetic stem and cup size. The average follow-up was 104 months (range, 55 to 131 months). To the authors' knowledge, this is the longest follow-up for this particular insert. Clinical and radiographic evaluations were performed at 1, 3, 6, and 12 months and then annually. Results showed that XLPE has a significantly greater wear reduction than that of standard polyethylene in primary total hip arthroplasty. At the longest available follow-up for these specific inserts, XLPE proved to be effective in reducing wear.

  2. Studies on N-vinylformamide cross-linked copolymers

    Science.gov (United States)

    Świder, Joanna; Tąta, Agnieszka; Sokołowska, Katarzyna; Witek, Ewa; Proniewicz, Edyta

    2015-12-01

    Copolymers of N-vinylformamide (NVF) cross-linked with three multifunctional monomers, including divinylbenzene (DVB), ethylene glycol dimethacrylate (EGDMA), and N,N‧-methylenebisacrylamide (MBA) were synthetized by a three-dimensional free radical polymerization in inverse suspension using 2,2‧-azobis(2-methylpropionamide) dihydrochloride (AIBA) as an initiator. Methyl silicon oil was used as the continuous phase during the polymerization processes. Fourier-transform adsorption infrared (FT-IR) spectra revealed the presence of silicone oil traces and suggested that silicone oil strongly interacted with the copolymers surface. Purification procedure allowed to completely remove the silicon oil traces from P(NVF-co-DVB) only. The morphology and the structure of the investigated copolymers were examined by optical microscopy, FT-IR, and FT-Raman (Fourier-transform Raman spectroscopy) methods.

  3. High-throughput preparation methods of crude extract for robust cell-free protein synthesis.

    Science.gov (United States)

    Kwon, Yong-Chan; Jewett, Michael C

    2015-03-02

    Crude extract based cell-free protein synthesis (CFPS) has emerged as a powerful technology platform for high-throughput protein production and genetic part characterization. Unfortunately, robust preparation of highly active extracts generally requires specialized and costly equipment and can be labor and time intensive. Moreover, cell lysis procedures can be hard to standardize, leading to different extract performance across laboratories. These challenges limit new entrants to the field and new applications, such as comprehensive genome engineering programs to improve extract performance. To address these challenges, we developed a generalizable and easily accessible high-throughput crude extract preparation method for CFPS based on sonication. To validate our approach, we investigated two Escherichia coli strains: BL21 Star™ (DE3) and a K12 MG1655 variant, achieving similar productivity (defined as CFPS yield in g/L) by varying only a few parameters. In addition, we observed identical productivity of cell extracts generated from culture volumes spanning three orders of magnitude (10 mL culture tubes to 10 L fermentation). We anticipate that our rapid and robust extract preparation method will speed-up screening of genomically engineered strains for CFPS applications, make possible highly active extracts from non-model organisms, and promote a more general use of CFPS in synthetic biology and biotechnology.

  4. Enzymatic cross-linking of soy proteins within non-fat set yogurt gel.

    Science.gov (United States)

    Soleymanpuori, Rana; Madadlou, Ashkan; Zeynali, Fariba; Khosrowshahi, Asghar

    2014-08-01

    Soy proteins as the health-promoting ingredients and candidate fat substitutes in dairy products are good substrates for the cross-linking action of the enzyme transglutaminase. Non-fat set yogurt samples were prepared from the milks enriched with soy protein isolate (SPI) and/or treated with the enzyme transglutaminase. The highest titrable acidity was recorded for the yogurt enriched with SPI and treated with the enzyme throughout the cold storage for 21 d. SPI-enrichment of yogurt milk increased the water holding capacity. Although enrichment with SPI did not influence the count of Streptococcus themophilus, increased that of Lactobacillus bulgaricus ∼3 log cycles. The enzymatic treatment of SPI-enriched milk however, suppressed the bacteria growth-promoting influence of SPI due probably to making the soy proteins inaccessible for Lactobacillus. SPI-enrichment and enzymatic treatment of milk decreased the various organic acids content in yoghurt samples; influence of the former was more significant. The cross-linking of milk proteins to soy proteins was confirmed with the gel electrophoresis results.

  5. Mapping the miRNA interactome by cross-linking ligation and sequencing of hybrids (CLASH).

    Science.gov (United States)

    Helwak, Aleksandra; Tollervey, David

    2014-03-01

    RNA-RNA interactions have critical roles in many cellular processes, but studying them is difficult and laborious. Here we describe an experimental procedure, termed cross-linking ligation and sequencing of hybrids (CLASH), which allows high-throughput identification of sites of RNA-RNA interaction. During CLASH, a tagged bait protein is UV-cross-linked in cell cultures to stabilize RNA interactions, and it is purified under denaturing conditions. RNAs associated with the bait protein are partially truncated, and the ends of RNA duplexes are ligated together. After linker addition, cDNA library preparation and high-throughput sequencing, the ligated duplexes give rise to chimeric cDNAs, which unambiguously identify RNA-RNA interaction sites independent of bioinformatic predictions. This protocol is optimized for studying miRNA targets bound by Argonaute (AGO) proteins, but it should be easily adapted for other RNA-binding proteins and classes of RNA. The protocol requires ∼5 d to complete, excluding the time required for high-throughput sequencing and bioinformatic analyses.

  6. Genipin-cross-linked fucose-chitosan/heparin nanoparticles for the eradication of Helicobacter pylori.

    Science.gov (United States)

    Lin, Yu-Hsin; Tsai, Shih-Chang; Lai, Chih-Ho; Lee, Che-Hsin; He, Zih Sian; Tseng, Guan-Chin

    2013-06-01

    Helicobacter pylori is a significant human pathogen that recognizes specific carbohydrate receptors, such as the fucose receptor, and produces the vacuolating cytotoxin, which induces inflammatory responses and modulates the cell-cell junction integrity of the gastric epithelium. The clinical applicability of topical antimicrobial agents was needed to complete the eradication of H. pylori in the infected fundal area. In the present study, we combined fucose-conjugated chitosan and genipin-cross-linking technologies in preparing multifunctional genipin-cross-linked fucose-chitosan/heparin nanoparticles to encapsulate amoxicillin of targeting and directly make contact with the region of microorganism on the gastric epithelium. The results show that the nanoparticles effectively reduced drug release at gastric acids and then released amoxicillin in an H. pylori survival situation to inhibit H. pylori growth and reduce disruption of the cell-cell junction protein in areas of H. pylori infection. Furthermore, with amoxicillin-loaded nanoparticles, a more complete H. pylori clearance effect was observed, and H. pylori-associated gastric inflammation in an infected animal model was effectively reduced.

  7. Multivalent anchoring and cross-linking of mussel-inspired antifouling surface coatings.

    Science.gov (United States)

    Wei, Qiang; Becherer, Tobias; Mutihac, Radu-Cristian; Noeske, Paul-Ludwig Michael; Paulus, Florian; Haag, Rainer; Grunwald, Ingo

    2014-08-11

    In this work, we combine nature's amazing bioadhesive catechol with the excellent bioinert synthetic macromolecule hyperbranched polyglycerol (hPG) to prepare antifouling surfaces. hPG can be functionalized by different amounts of catechol groups for multivalent anchoring and cross-linking because of its highly branched architecture. The catecholic hPGs can be immobilized on various surfaces including metal oxides, noble metals, ceramics, and polymers via simple incubation procedures. The effect of the catechol amount on the immobilization, surface morphology, stability, and antifouling performance of the coatings was studied. Both anchoring and cross-linking interactions provided by catechols can enhance the stability of the coatings. When the catechol groups on the hPG are underrepresented, the tethering of the coating is not effective; while an overrepresentation of catechol groups leads to protein adsorption and cell adhesion. Thus, only a well-balanced amount of catechols as optimized and described in this work can supply the coatings with both good stability and antifouling ability.

  8. Synthesis and antimicrobial activity of some novel cross-linked chitosan hydrogels.

    Science.gov (United States)

    Mohamed, Nadia Ahmed; Fahmy, Mona Mohamed

    2012-01-01

    Four novel hydrogels based on chitosan were synthesized via a cross-linking reaction of chitosan with different concentrations of oxalyl bis 4-(2,5-dioxo-2H-pyrrol- 1(5H)-yl)benzamide. Their structures were confirmed by fourier transform infrared X-ray (FTIR), scanning electron microscopy (SEM) and X-ray diffraction. The antimicrobial activities of the hydrogels against two crop-threatening pathogenic fungi namely: Aspergillus fumigatus (A. fumigatus, RCMBA 06002), and Aspergillus niger (A. niger, RCMBA 06106), and five bacterial species namely: Bacillis subtilis (B. subtilis, RCMBA 6005), Staphylococcus aureus (S. aureus, RCMBA 2004), Streptococcus pneumoniae (S. pneumonia, RCMB 000101) as Gram positive bacteria, and Salmonella typhimurium (S. typhimurium, RCMB 000104), and Escherichia coli (E. coli, RCMBA 5003) as Gram negative bacteria have been investigated. The prepared hydrogels showed much higher antimicrobial activities than that of the parent chitosan. The hydrogels were more potent in case of Gram-positive bacteria than Gram-negative bacteria. Increasing the degree of cross-linking in the hydrogels resulted in a weaker antimicrobial activity.

  9. Synthesis and Antimicrobial Activity of Some Novel Cross-Linked Chitosan Hydrogels

    Directory of Open Access Journals (Sweden)

    Mona Mohamed Fahmy

    2012-09-01

    Full Text Available Four novel hydrogels based on chitosan were synthesized via a cross-linking reaction of chitosan with different concentrations of oxalyl bis 4-(2,5-dioxo-2H-pyrrol-1(5H-ylbenzamide. Their structures were confirmed by fourier transform infrared X-ray (FTIR, scanning electron microscopy (SEM and X-ray diffraction. The antimicrobial activities of the hydrogels against two crop-threatening pathogenic fungi namely: Aspergillus fumigatus (A. fumigatus, RCMBA 06002, and Aspergillus niger (A. niger, RCMBA 06106, and five bacterial species namely: Bacillis subtilis (B. subtilis, RCMBA 6005, Staphylococcus aureus (S. aureus, RCMBA 2004, Streptococcus pneumoniae (S. pneumonia, RCMB 000101 as Gram positive bacteria, and Salmonella typhimurium (S. typhimurium, RCMB 000104, and Escherichia coli (E. coli, RCMBA 5003 as Gram negative bacteria have been investigated. The prepared hydrogels showed much higher antimicrobial activities than that of the parent chitosan. The hydrogels were more potent in case of Gram-positive bacteria than Gram-negative bacteria. Increasing the degree of cross-linking in the hydrogels resulted in a weaker antimicrobial activity.

  10. Alkaline membrane fuel cells with in-situ cross-linked ionomers

    Energy Technology Data Exchange (ETDEWEB)

    Leng, YJ; Wang, LZ; Hickner, MA; Wang, CY

    2015-01-10

    Improving cell performance and durability through both new materials and membrane electrode processing optimization is needed for the commercialization of alkaline membrane fuel cell (AMFC) technologies. In this work, we adopted an in-situ cross-linking strategy of an anion-conducting block copolymer to prepare durable ionomers for use in alkaline membrane fuel cells (AMFCs). Our goal was to use new ionomers and binders with an aim at improving long-term stability of AMFCs, especially at high operation temperatures. At 80 degrees C, AMFCs with in-situ cross-linked ionomers showed promising stability with an operating life time of more than 350 hours at 100 mA/cm(2). We found that the optimized electrode fabrication process and operating conditions can significantly improve the durability performance of AMFCs. For example, a suitable electrode binder in addition to the ion-conducting ionomer can greatly enhance the durability performance of AMFCs. Operating fuel cells under a cathode over-humification condition can also enhance the long-term stability of AMFCs. (C) 2014 Elsevier Ltd. All rights reserved.

  11. Characterization of Chemical and Physical Properties of Hydroxypropylated and Cross-linked Arrowroot (Marantha arundinacea Starch

    Directory of Open Access Journals (Sweden)

    Rijanti Rahaju Maulani

    2013-12-01

    Full Text Available The modern food industry and a variety of food products require tolerant starch as raw material for processing in a broad range of techniques, from preparation to storage and distribution. Dual modification of arrowroot starch using hydroxypropylation and cross-linking was carried out to overcome the lack of native arrowroot starch in food processing application. The modifications applied were: combined propylene oxide (8%, 10%, and 12%; sodium tri meta phosphate/STMP (1%, 2%, and 3%; and sodium tri poly phosphate/STPP (4%, 5%, and 6%. These modifications significantly affected the composition of the amylose and amylopectin and the amount of phosphorus in the granules. Higher amounts of phosphate salt gave a higher phosphorus content, which increased the degree of substitution (DS and the degree of cross-link. Arrowroot starch that was modified using a concentration of 8-10% propylene oxide and 1-2% STMP : 3-5% STPP produced a starch with < 0.4% phosphorus content. A higher concentration of propylene oxide provided a higher degree of hydroxypropyl. The changed physical properties of the modified granular arrowroot starch were examined through SEM testing, and its changed crystalline patterns through X-ray diffraction measurements. Especially, provision of a high concentration of propylene oxide (12% combined with 3% STMP : 6% STPP affected the granular morphology and the crystallinity.

  12. Degradable Cross-Linked Nanoassemblies as Drug Carriers for Heat Shock Protein 90 Inhibitor 17-N-Allylamino-17-demethoxy-geldanamycin.

    Science.gov (United States)

    Ponta, Andrei; Akter, Shanjida; Bae, Younsoo

    2011-09-26

    Cross-linked nanoassemblies (CNAs) with a degradable core were prepared for sustained release of 17-N-allylamino-17-demethoxygeldanamycin (17-AAG), a potent inhibitor of heat shock protein 90 (HSP90). The particle size of CNAs ranged between 100 and 250 nm, which changed depending on the cross-linking yields and drug entrapment method. CNAs with a 1% cross-linking yield entrapped 17-AAG in aqueous solutions, yet degraded in 3 hrs. CNAs entrapped 5.2 weight% of 17-AAG as the cross-linking yield increased to 10%, retaining more than 80% of particles for 24 hrs. CNAs with drugs entrapped after the cross-linking reactions were 100 nm and remained stable in both pH 7.4 and 5.0, corresponding to the physiological, tumoral, and intracellular environments. Drug was completely released from CNAs in 48 hrs, which would potentially maximize drug delivery and release efficiency within tumor tissues. Drug release patterns were not negatively affected by changing the cross-linking yields of CNAs. CNAs entrapping 17-AAG suppressed the growth of human non-small cell lung cancer A549 cells as equally effective as free drugs. The results demonstrated that CNAs would be a promising formulation that can be used in aqueous solutions for controlled delivery and release of 17-AAG.

  13. Degradable Cross-Linked Nanoassemblies as Drug Carriers for Heat Shock Protein 90 Inhibitor 17-N-Allylamino-17-demethoxy-geldanamycin

    Directory of Open Access Journals (Sweden)

    Andrei Ponta

    2011-09-01

    Full Text Available Cross-linked nanoassemblies (CNAs with a degradable core were prepared for sustained release of 17-N-allylamino-17-demethoxygeldanamycin (17-AAG, a potent inhibitor of heat shock protein 90 (HSP90. The particle size of CNAs ranged between 100 and 250 nm, which changed depending on the cross-linking yields and drug entrapment method. CNAs with a 1% cross-linking yield entrapped 17-AAG in aqueous solutions, yet degraded in 3 hrs. CNAs entrapped 5.2 weight% of 17-AAG as the cross-linking yield increased to 10%, retaining more than 80% of particles for 24 hrs. CNAs with drugs entrapped after the cross-linking reactions were 100 nm and remained stable in both pH 7.4 and 5.0, corresponding to the physiological, tumoral, and intracellular environments. Drug was completely released from CNAs in 48 hrs, which would potentially maximize drug delivery and release efficiency within tumor tissues. Drug release patterns were not negatively affected by changing the cross-linking yields of CNAs. CNAs entrapping 17-AAG suppressed the growth of human non-small cell lung cancer A549 cells as equally effective as free drugs. The results demonstrated that CNAs would be a promising formulation that can be used in aqueous solutions for controlled delivery and release of 17-AAG.

  14. Nafion-assisted cross-linking of sulfonated poly(arylene ether ketone) bearing carboxylic acid groups and their composite membranes for fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Haidan; Zhao, Chengji; Na, Hui [Alan G. MacDiarmid Institute, College of Chemistry, Jilin University, Qianjin street 2699, Changchun 130012, Jilin (China)

    2010-06-01

    In this study, a new type of cross-linked composite membrane is prepared and considered for its potential applications in direct methanol fuel cell. Nafion and sulfonated poly(arylene ether ketone) bearing carboxylic acid groups (SPAEK-C) are blended and subsequently cross-linked by a Friedel-Craft reaction using the carboxylic acid groups in the SPAEK-C to achieve lower methanol permeability. The perfluoroalkyl sulfonic acid groups of Nafion act as a benign solid catalyst, which assist the cross-linking of SPAEK-C. The physical and chemical characterizations of the cross-linked composite membranes are performed by varying the contents of SPAEK-C. The c-Nafion-15% membrane exhibits appropriate water uptake (10.49-25.22%), low methanol permeability (2.57 x 10{sup -7} cm{sup 2} s{sup -1}), and high proton conductivity (0.179 S cm{sup -1} at 80 C). DSC and FTIR analyze suggest the cross-linking reaction. These results show that the self-cross-linking of SPAEK-C in the Nafion membrane can effectively reduce methanol permeability while maintaining high proton conductivity. (author)

  15. Grass Cell Walls: A Story of Cross-Linking

    Science.gov (United States)

    Hatfield, Ronald D.; Rancour, David M.; Marita, Jane M.

    2017-01-01

    Cell wall matrices are complex composites mainly of polysaccharides, phenolics (monomers and polymers), and protein. We are beginning to understand the synthesis of these major wall components individually, but still have a poor understanding of how cell walls are assembled into complex matrices. Valuable insight has been gained by examining intact components to understand the individual elements that make up plant cell walls. Grasses are a prominent group within the plant kingdom, not only for their important roles in global agriculture, but also for the complexity of their cell walls. Ferulate incorporation into grass cell wall matrices (C3 and C4 types) leads to a cross-linked matrix that plays a prominent role in the structure and utilization of grass biomass compared to dicot species. Incorporation of p-coumarates as part of the lignin structure also adds to the complexity of grass cell walls. Feruoylation results in a wall with individual hemicellulosic polysaccharides (arabinoxylans) covalently linked to each other and to lignin. Evidence strongly suggests that ferulates not only cross-link arabinoxylans, but may be important factors in lignification of the cell wall. Therefore, the distribution of ferulates on arabinoxylans could provide a means of structuring regions of the matrix with the incorporation of lignin and have a significant impact upon localized cell wall organization. The role of other phenolics in cell wall formation such as p-coumarates (which can have concentrations higher than ferulates) remains unknown. It is possible that p-coumarates assist in the formation of lignin, especially syringyl rich lignin. The uniqueness of the grass cell wall compared to dicot sepcies may not be so much in the gross composition of the wall, but how the distinctive individual components are organized into a functional wall matrix. These features are discussed and working models are provided to illustrate how changing the organization of feruoylation and p

  16. Peptidoglycan Cross-Linking in Glycopeptide-Resistant Actinomycetales

    Science.gov (United States)

    Hugonnet, Jean-Emmanuel; Haddache, Nabila; Veckerlé, Carole; Dubost, Lionel; Marie, Arul; Shikura, Noriyasu; Mainardi, Jean-Luc; Rice, Louis B.

    2014-01-01

    Synthesis of peptidoglycan precursors ending in d-lactate (d-Lac) is thought to be responsible for glycopeptide resistance in members of the order Actinomycetales that produce these drugs and in related soil bacteria. More recently, the peptidoglycan of several members of the order Actinomycetales was shown to be cross-linked by l,d-transpeptidases that use tetrapeptide acyl donors devoid of the target of glycopeptides. To evaluate the contribution of these resistance mechanisms, we have determined the peptidoglycan structure of Streptomyces coelicolor A(3)2, which harbors a vanHAX gene cluster for the production of precursors ending in d-Lac, and Nonomuraea sp. strain ATCC 39727, which is devoid of vanHAX and produces the glycopeptide A40296. Vancomycin retained residual activity against S. coelicolor A(3)2 despite efficient incorporation of d-Lac into cytoplasmic precursors. This was due to a d,d-transpeptidase-catalyzed reaction that generated a stem pentapeptide recognized by glycopeptides by the exchange of d-Lac for d-Ala and Gly. The contribution of l,d-transpeptidases to resistance was limited by the supply of tetrapeptide acyl donors, which are essential for the formation of peptidoglycan cross-links by these enzymes. In the absence of a cytoplasmic metallo-d,d-carboxypeptidase, the tetrapeptide substrate was generated by hydrolysis of the C-terminal d-Lac residue of the stem pentadepsipeptide in the periplasm in competition with the exchange reaction catalyzed by d,d-transpeptidases. In Nonomuraea sp. strain ATCC 39727, the contribution of l,d-transpeptidases to glycopeptide resistance was limited by the incomplete conversion of pentapeptides into tetrapeptides despite the production of a cytoplasmic metallo-d,d-carboxypeptidase. Since the level of drug production exceeds the level of resistance, we propose that l,d-transpeptidases merely act as a tolerance mechanism in this bacterium. PMID:24395229

  17. The wear of cross-linked polyethylene against itself.

    Science.gov (United States)

    Joyce, T J; Ash, H E; Unsworth, A

    1996-01-01

    Cross-linked polyethylene (XLPE) may have an application as a material for an all-plastic surface replacement finger joint. It is inexpensive, biocompatible and can be injection-moulded into the complex shapes that are found on the ends of the finger bones. Further, the cross-linking of polyethylene has significantly improved its mechanical properties. Therefore, the opportunity exists for an all-XLPE joint, and so the wear characteristics of XLPE sliding against itself have been investigated. Wear tests were carried out on both reciprocating pin-on-plate machines and a finger function simulator. The reciprocating pin-on-plate machines had pins loaded at 10 N and 40 N. All pin-on-plate tests show wear factors from the plates very much greater than those of the pins. After 349 km of sliding, a mean wear factor of 0.46 x 10(-6) mm3/N m was found for the plates compared with 0.021 x 10(-6) mm3/N m for the pins. A fatigue mechanism may be causing this phenomenon of greater plate wear. Tests using the finger function simulator give an average wear rate of 0.22 x 10(-6) mm3/N m after 368 km. This sliding distance is equivalent to 12.5 years of use in vivo. The wear factors found were comparable with those of ultra-high molecular weight polyethylene (UHMWPE) against a metallic counterface and, therefore, as the loads across the finger joint are much less than those across the knee or the hip, it is probable that an all-XLPE finger joint will be viable from a wear point of view.

  18. Yield and Failure Behavior Investigated for Cross-Linked Phenolic Resins Using Molecular Dynamics

    Science.gov (United States)

    Monk, Joshua D.; Lawson, John W.

    2016-01-01

    Molecular dynamics simulations were conducted to fundamentally evaluate the yield and failure behavior of cross-linked phenolic resins at temperatures below the glass transition. Yield stress was investigated at various temperatures, strain rates, and degrees of cross-linking. The onset of non-linear behavior in the cross-linked phenolic structures was caused by localized irreversible molecular rearrangements through the rotation of methylene linkers followed by the formation or annihilation of neighboring hydrogen bonds. The yield stress results, with respect to temperature and strain rate, could be fit by existing models used to describe yield behavior of amorphous glasses. The degree of cross-linking only indirectly influences the maximum yield stress through its influence on glass transition temperature (Tg), however there is a strong relationship between the degree of cross-linking and the failure mechanism. Low cross-linked samples were able to separate through void formation, whereas the highly cross-linked structures exhibited bond scission.

  19. Short-range and long-range cross-linking effects of polygenipin on gelatin-based composite materials.

    Science.gov (United States)

    Ge, Liming; Xu, Yongbin; Liang, Weijie; Li, Xinying; Li, Defu; Mu, Changdao

    2016-11-01

    Genipin is an ideal cross-linking agent in biomedical applications, which can undergo ring-opening polymerization in alkaline condition. The polygenipin can create short-range and long-range intermolecular cross-linking between protein chains. In this article, the polygenipin with different degree of polymerization was successfully prepared and used to fix gelatin composite materials. The short-range and long-range cross-linking effects of polygenipin were systematically studied. The results show that the composite materials present porous structure with tunable pore sizes in the gel state, which can be easily controlled by adjusting the degree of polymerization of polygenipin. Long-range cross-linking can increase the pore size of the gel. However, during the drying process, the composite films cross-linked by polygenipin with higher degree of polymerization shrank to smaller size to create more compact structure, resulting in the improvement of water resistance properties, thermal stability, tensile strength, and darker color for the composite films. It is interesting that the composite films can partly swell to the original gel structure when in contact with water and saturated water vapor. All the composite films have excellent barrier properties against UV light. However, the compatibility of gelatin and polygenipin is reduced when the degree of polymerization of polygenipin increases to a certain extent, which will result in the formation of phase separation structure. The obtained composite films are ideal candidates for food and pharmaceutical packaging materials. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2712-2722, 2016.

  20. Self-reinforcement and protein sustained delivery of hyaluronan hydrogel by tailoring a dually cross-linked network

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Chunhong; Xu, Guoguang; Wang, Xinghui [Department of Materials Science and Engineering, College of Science and Engineering, Jinan University, Guangzhou 510632 (China); Tu, Mei; Zeng, Rong; Rong, Jianhua [Department of Materials Science and Engineering, College of Science and Engineering, Jinan University, Guangzhou 510632 (China); Engineering Research Center of Artificial Organs and Materials, Ministry of Education, Guangzhou 510632 (China); Zhao, Jianhao, E-mail: jhzhao@jnu.edu.cn [Department of Materials Science and Engineering, College of Science and Engineering, Jinan University, Guangzhou 510632 (China); Engineering Research Center of Artificial Organs and Materials, Ministry of Education, Guangzhou 510632 (China)

    2015-01-01

    A series of self-reinforcing hyaluronan hydrogels were developed to improve mechanical properties and protein sustained delivery thanks to a dually cross-linked network. Hyaluronan gel particles (HGPs, 1–5 μm in diameter) with different cross-linking densities, i.e. HGPs-1.5, HGPs-3 and HGPs-15, were prepared in an inverse emulsion system and used as the reinforcing phase after glycidyl methacrylation, while glycidyl methacrylated hyaluronan with a substitution degree of 45.2% was synthesized as the matrix phase. These two phases were cross-linked under ultraviolet irradiation to form self-reinforcing hyaluronan hydrogels (srHAs) that showed typical cross-linked structure of HGPs connecting the matrix phase by cross-section observation. In comparison to hyaluronan bulk gels and their blends with HGPs, srHAs distinctly enhanced the mechanical properties and BSA long-term sustained delivery, especially srHA-1.5 showed the highest compressive modulus of 220 ± 15 kPa and the slowest BSA delivery (67% release at 14 d). The 3T3 fibroblast cell culture showed that all the srHAs had no cytotoxicity. - Highlights: • New self-reinforcing HA hydrogels with a dually cross-linked network were developed. • Self-reinforcing HA hydrogels greatly enhanced the mechanical properties. • Self-reinforcing HA hydrogels prolonged the sustained delivery of BSA. • The self-reinforcing mechanism and BSA diffusion mechanism were discussed. • Self-reinforcing HA hydrogels had no cytotoxicity to 3T3 fibroblast cells.

  1. Photo-cross-linking of amniotic membranes for limbal epithelial cell cultivation

    Energy Technology Data Exchange (ETDEWEB)

    Lai, Jui-Yang, E-mail: jylai@mail.cgu.edu.tw

    2014-12-01

    In the present study, we developed photo-cross-linked amniotic membrane (AM) as a limbal stem cell niche. After ultraviolet (UV) irradiation for varying time periods, the biological tissues were studied by determinations of cross-linking structure, degradability, and nutrient permeation ability. Our results showed that the number of cross-links per unit mass of AM significantly increased with increasing illumination time from 5 to 50 min. However, the cross-link formation was inhibited by longer irradiation time (i.e., 150 min), probably due to the scission of tissue collagen chains through irradiation. The biological stability and matrix permeability of photo-cross-linked AM materials strongly depended on their cross-linking densities affected by the UV irradiation. In vitro biocompatibility studies including cell viability and pro-inflammatory gene expression analyses demonstrated that, irrespective of the irradiation time employed, the physically cross-linked biological tissues exhibited negligible cytotoxicity and similar interleukin-6 (IL-6) mRNA levels. The data clearly indicate that these AM matrices do not cause potential harm to the corneal epithelial cells. After the growth of limbal epithelial cells (LECs) on AM substrates, Western blot analyses were conducted to examine the expression of ABCG2. It was found that the ability of UV-irradiated AM to maintain the undifferentiated precursor cell phenotype was significantly enhanced with increasing extent of photo-cross-linking. In summary, the UV irradiation time may have a profound influence on the fabrication of photo-cross-linked AM matrices for LEC cultivation. - Highlights: • We report the development of photo-cross-linked AM as a limbal stem cell niche. • Cross-linked structure of tissue materials was controlled by UV irradiation time. • Biostability and matrix permeability of AM depended on cross-linking density. • All the studied photo-cross-linked AM showed good in vitro biocompatibility.

  2. General, robust, and stereocomplementary preparation of alpha,beta-disubstituted alpha,beta-unsaturated esters.

    Science.gov (United States)

    Nakatsuji, Hidefumi; Nishikado, Hiroshi; Ueno, Kanako; Tanabe, Yoo

    2009-10-01

    An (E)- and (Z)-stereocomplementary preparative method for alpha,beta-disubstituted alpha,beta-unsaturated esters is performed via three general and robust reaction sequences: (i) Ti-Claisen condensation (formylation) of esters to give alpha-formyl esters (12 examples, 60-99%), (ii) (E)- and (Z)-stereocomplementary enol p-toluenesulfonylation (tosylation) using TsCl-N-methylimidazole (NMI)-Et(3)N and LiOH (24 examples, 82-99%), and (iii) stereoretentive Suzuki-Miyaura cross-coupling (18 examples, 64-96%).

  3. A robust ligand exchange approach for preparing hydrophilic, biocompatible photoluminescent quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Sujuan; Zhou, Changhua [Key Laboratory for Special Functional Materials of the Ministry of Education, Henan University, Kaifeng 475004 (China); Yuan, Hang [Life Science Division, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Shen, Huaibin [Key Laboratory for Special Functional Materials of the Ministry of Education, Henan University, Kaifeng 475004 (China); Zhao, Wenxiu [Life Science Division, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Ma, Lan, E-mail: malan@sz.tsinghua.edu.cn [Life Science Division, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Li, Lin Song, E-mail: lsli@henu.edu.cn [Key Laboratory for Special Functional Materials of the Ministry of Education, Henan University, Kaifeng 475004 (China)

    2013-08-01

    Graphical abstract: - Highlights: • Aqueous CdSe/ZnS QDs were prepared using polymaleic anhydrides as capping ligand. • Effect of reaction temperature and time were systematically studied in the synthesis process. • Water-soluble QDs exhibited a good stability in physiological relevant environment. • The aqueous QDs were applied as biological probe to detect human embryonic stem cell. - Abstract: This paper describes a robust ligand exchange approach for preparing biocompatible CdSe/ZnS quantum dots (QDs) to make bioprobe for effective cell imaging. In this method, polymaleic anhydride (PMA) ligand are first used to replace original hydrophobic ligand (oleic acid) and form a protection shell with multiple hydrophilic groups to coat and protect CdSe/ZnS QDs. The as-prepared aqueous QDs exhibit small particle size, good colloidal stability in aqueous solutions with a wide range of pH, salt concentrations and under thermal treatment, which are necessary for biological applications. The use of this new class of aqueous QDs for effective cell imaging shows strong fluorescence signal to human embryonic stem cell, which demonstrate that PMA coated QDs are fully satisfied with the requirements of preparing high quality biological probe.

  4. Characterization of Interstrand DNA-DNA Cross-Links Using the α-Hemolysin Protein Nanopore.

    Science.gov (United States)

    Zhang, Xinyue; Price, Nathan E; Fang, Xi; Yang, Zhiyu; Gu, Li-Qun; Gates, Kent S

    2015-12-22

    Nanopore-based sensors have been studied extensively as potential tools for DNA sequencing, characterization of epigenetic modifications such as 5-methylcytosine, and detection of microRNA biomarkers. In the studies described here, the α-hemolysin protein nanopore embedded in a lipid bilayer was used for the detection and characterization of interstrand cross-links in duplex DNA. Interstrand cross-links are important lesions in medicinal chemistry and toxicology because they prevent the strand separation that is required for read-out of genetic information from DNA in cells. In addition, interstrand cross-links are used for the stabilization of duplex DNA in structural biology and materials science. Cross-linked DNA fragments produced unmistakable current signatures in the nanopore experiment. Some cross-linked substrates gave irreversible current blocks of >10 min, while others produced long current blocks (10-100 s) before the double-stranded DNA cross-link translocated through the α-hemolysin channel in a voltage-driven manner. The duration of the current block for the different cross-linked substrates examined here may be dictated by the stability of the duplex region left in the vestibule of the nanopore following partial unzipping of the cross-linked DNA. Construction of calibration curves measuring the frequency of cross-link blocking events (1/τon) as a function of cross-link concentration enabled quantitative determination of the amounts of cross-linked DNA present in samples. The unique current signatures generated by cross-linked DNA in the α-HL nanopore may enable the detection and characterization of DNA cross-links that are important in toxicology, medicine, and materials science.

  5. Thermally cross-linked superparamagnetic iron oxide nanoparticles: synthesis and application as a dual imaging probe for cancer in vivo.

    Science.gov (United States)

    Lee, Haerim; Yu, Mi Kyung; Park, Sangjin; Moon, Sungmin; Min, Jung Jun; Jeong, Yong Yeon; Kang, Hae-Won; Jon, Sangyong

    2007-10-24

    We report the fabrication and characterization of thermally cross-linked superparamagnetic iron oxide nanoparticles (TCL-SPION) and their application to the dual imaging of cancer in vivo. Unlike dextran-coated cross-linked iron oxide nanoparticles, which are prepared by a chemical cross-linking method, TCL-SPION are prepared by a simple, thermal cross-linking method using a Si-OH-containing copolymer. The copolymer, poly(3-(trimethoxysilyl)propyl methacrylate-r-PEG methyl ether methacrylate-r-N-acryloxysuccinimide), was synthesized by radical polymerization and used as a coating material for as-synthesized magnetite (Fe3O4) SPION. The polymer-coated SPION was further heated at 80 degrees C to induce cross-linking between the -Si(OH)3 groups in the polymer chains, which finally generated TCL-SPION bearing a carboxyl group as a surface functional group. The particle size, surface charge, presence of polymer-coating layers, and the extent of thermal cross-linking were characterized and confirmed by various measurements, including dynamic light scattering, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The carboxyl TCL-SPION was converted to amine-modified TCL-SPION and then finally to Cy5.5 dye-conjugated TCL-SPION for use in dual (magnetic resonance/optical) in vivo cancer imaging. When the Cy5.5 TCL-SPION was administered to Lewis lung carcinoma tumor allograft mice by intravenous injection, the tumor was unambiguously detected in T2-weighted magnetic resonance images as a 68% signal drop as well as in optical fluorescence images within 4 h, indicating a high level of accumulation of the nanomagnets within the tumor site. In addition, ex vivo fluorescence images of the harvested tumor and other major organs further confirmed the highest accumulation of the Cy5.5 TCL-SPION within the tumor. It is noteworthy that, despite the fact that TCL-SPION does not bear any targeting ligands on its surface, it was highly effective for tumor

  6. A novel method for immobilization of proteins via entrapment of magnetic nanoparticles through epoxy cross-linking.

    Science.gov (United States)

    Iype, Tessy; Thomas, Jaiby; Mohan, Sangeetha; Johnson, Kochurani K; George, Ligi E; Ambattu, Lizebona A; Bhati, Aniruddha; Ailsworth, Kristen; Menon, Bindu; Rayabandla, Sunayana M; Jesudasan, Rachel A; Santhosh, Sam; Ramchand, Chaniyilparampu N

    2017-02-15

    A method for immobilization of functional proteins by chemical cross-linking of the protein of interest and uncoated iron oxide nanoparticles in the presence of Epichlorohydrin is described. As a result of the cross-linking, the proteins form a matrix in which the particles get entrapped. The optimum concentration of Epichlorohydrin that facilitates immobilization of protein without affecting the functional properties of the protein was determined. This method was used to immobilize several functional proteins and the development and functional activity of Protein A-magnetic nanoparticles (MNPs) is described here in detail. The Protein A-MNPs possess high binding capacity due to the increased surface area of uncoated nanoparticles and robust magnetic separation due to the absence of polymeric coating materials. Protein A-MNPs were successfully used for purification of antibodies and also for immunoprecipitation. We also immobilized enzymes such as horse radish peroxidase and esterase and found that by providing the optimum incubation time, temperature and protein to nanoparticle ratio, we can retain the activity and improve the stability of the enzyme. This study is the first demonstration that Epichlorohydrin can be used to entrap nanoparticles in a cross-linked matrix of protein without impairing the activity of immobilized protein.

  7. Riboflavin-ultraviolet a corneal cross-linking for keratoconus

    Directory of Open Access Journals (Sweden)

    El-Raggal Tamer

    2009-01-01

    Full Text Available Purpose: To evaluate the safety, efficacy of riboflavin-ultraviolet A irradiation (UVA corneal cross-linking and present refractive changes induced by the treatment in cases of keratoconus. Materials and Methods: The study includes 15 eyes of 9 patients with keratoconus with an average keratometric (K reading less than 54 D and minimal corneal thickness greater than 420 microns. The corneal epithelium was removed manually within the central 8.5 mm diameter area and the cornea was soaked with riboflavin eye drops (0.1% in 20% dextran t-500 for 30 minutes followed by exposure to UVA radiation (365 nm, 3 mW/cm 2 for 30 minutes. During the follow-up period, uncorrected visual acuity (UCVA, best spectacle-corrected visual acuity (BSCVA, manifest refraction, slit lamp examination and topographic changes were recorded at the first week, first month, 3 and 6 months. Results: There was statistically significant improvement of UCVA from a preoperative mean of 0.11 ± 0.07 (range 0.05-0.3 to a postoperative mean of 0.15 ± 0.06 (range 0.1-0.3 (P < 0.05. None of the eyes lost lines of preoperative UCVA but 1 eye lost 1 line of preoperative BSCVA. The preoperative mean K of 49.97 ± 2.81 D (range 47.20-51.75 changed to 48.34 ± 2.64 D (range 45.75-50.40. This decrease in K readings was statistically significant (P < 0.05. All eyes developed minimal faint stromal haze that cleared in 14 eyes within 1 month. In only 1 eye, this resulted in a very faint corneal scar. Other sight threatening complications were not encountered in this series. Progression of the original disease was not seen in any of the treated eyes within 6 months of follow-up. Conclusion: Riboflavin-UVA corneal cross-linking is a safe and promising method for keratoconus. Larger studies with longer follow up are recommended.

  8. A core cross-linked polymeric micellar platium(IV) prodrug with enhanced anticancer efficiency.

    Science.gov (United States)

    Hou, Jie; Shang, Jincai; Jiao, Chengbin; Jiang, Peiyue; Xiao, Huijie; Luo, Lan; Liu, Tongjun

    2013-07-01

    A core cross-linked polymeric micellar cisplatin(IV) conjugate prodrug is prepared by attaching the cisplatin(IV) to mPEG-b-PLL biodegradable copolymers to form micellar nanoparticles that can disintegrate to release the active anticancer agent cisplatin(II) in a mild reducing environment. Moreover, in vitro studies show that this cisplatin(IV) conjugate prodrug displays enhanced cytotoxicity against HepG2 cancer cells compared with cisplatin(II). Further studies demonstrate that the high cellular uptake and platinum-DNA adduct of this cisplatin(IV) conjugate prodrug can induce more cancer-cell apoptosis than cisplatin(II), which is responsible for its enhanced anticancer activity.

  9. Fabrication and morphology of spongelike polymer material based on cross-linked sulfonated polystyrene particles.

    Science.gov (United States)

    Ji, Xiang; Wang, Mozhen; Xu, Dezhi; Ge, Xuewu; Liu, Huarong; Tang, Tao

    2012-04-03

    A novel spongelike polymer material has been fabricated by γ-ray induced polymerization of methylmethacrylate (MMA) in an emulsion containing cross-linked sulfonated polystyrene (CSP) particles. Scanning electron microscopy (SEM) images reveal that the spongelike structure is made up of interlinked nanosized PMMA particles with micrometer-sized CSP-PMMA particles embedded inside. The nitrogen adsorption isotherm discloses that the spongelike material has a high specific surface area of 29 m(2)/g and a narrow pore size distribution of 60-120 nm. The formation mechanism is discussed in this paper, which indicates that the key steps to form the spongelike material include a Pickering emulsion stabilized by the CSP particles, followed by the swelling process of MMA into these particles. This approach offers a more convenient alternative to prepare polymeric spongelike material without any etching procedure.

  10. Highly cross-linked polyethylene in hip resurfacing arthroplasty: long-term follow-up.

    Science.gov (United States)

    Amstutz, Harlan C; Takamura, Karren M; Ebramzadeh, Edward; Le Duff, Michel J

    2015-01-01

    Highly cross-linked polyethylene (XLPE) has improved wear properties. This study reports the results of a small series of patients treated over 10 years ago with a metal-on-XLPE hip resurfacing.A total of 21 hips in 20 patients received a hip resurfacing with a cobalt-chromium metal femoral head and metal-backed acetabular cup lined with a XLPE insert and were retrospectively studied. Kaplan-Meier Survivorship was calculated.Five patients who had initial extreme cystic disease in the femoral head failed due to femoral loosening. Survivorship was 95.2% at 5 years and 81.0% at 10 years.We found that XLPE wear was not implicated in these failures, which were primarily attributed to poor bone quality of the femoral head, early bone preparation, cementing technique and excessive head reaming to near the neck diameter, necessitated for the implantation of a thick two-part socket.

  11. Stabilization of human prostate acid phosphatase by cross-linking with diimidoesters.

    Science.gov (United States)

    Wasylewska, E; Dulińska, J; Trubetskoy, V S; Torchilin, V P; Ostrowski, W S

    1987-01-01

    1. Modification of dimeric human prostate acid phosphatase (EC 3.1.3.2) by diimidoesters leads to the formation of water-soluble preparations of high enzymatic activity, resistant to denaturing agents. 2. Monomeric, dimeric, trimeric and tetrameric species were found in SDS-polyacrylamide gel electrophoresis of the phosphatase cross-linked with dimethyl-suberimidate, and dimeric, trimeric and tetrameric enzymatically active species on thin-layer Sephadex 200 gel filtration. This molecular pattern evidenced formation of the inter-subunit covalent linkages. All molecular forms are immunoreactive against the polyclonal rabbit anti-phosphatase antibodies. 3. The catalytic properties of the modified phosphatase are almost the same as those of the native enzyme. Differences in the optical properties between the modified and the native enzymes point to slight conformational transitions in the modified enzyme.

  12. Effect of cross linking of PVA/starch and reinforcement of modified barley husk on the properties of composite films.

    Science.gov (United States)

    Mittal, Aanchal; Garg, Sangeeta; Kohli, Deepak; Maiti, Mithu; Jana, Asim Kumar; Bajpai, Shailendra

    2016-10-20

    Barley husk (BH) was graft copolymerized by palmitic acid. The crystalline behavior of BH decreased after grafting. Poly vinyl alcohol (PVA)/starch (St) blend film, urea formaldehyde cross linked PVA/St films and composite films containing natural BH, grafted BH were prepared separately. The effect of urea/starch ratio, content of BH and grafted BH on the mechanical properties, water uptake (%), and biodegradability of the composite films was observed. With increase in urea: starch ratio from 0 to 0.5 in the blend, tensile strength of cross linked film increased by 40.23% compared to the PVA/St film. However, in grafted BH composite film, the tensile strength increased by 72.4% than PVA/St film. The degradation rate of natural BH composite film was faster than PVA/St film. Various films were characterized by SEM, FT-IR and thermal analysis.

  13. Synthesis of G-N2-(CH2)3-N2-G Trimethylene DNA interstrand cross-links

    Science.gov (United States)

    Gruppi, Francesca; Salyard, Tracy L. Johnson; Rizzo, Carmelo J.

    2014-01-01

    The synthesis of G-N2-(CH2)3-N2-G trimethylene DNA interstrand cross-links (ICLs) in a 5′-CG-3′ and 5′-GC-3′ sequence from oligodeoxynucleotides containing N2-(3-aminopropyl)-2′-deoxyguanosine and 2-fluoro-O6-(trimethylsilylethyl)inosine is presented. Automated solid-phase DNA synthesis was used for unmodified bases and modified nucleotides were incorporated via their corresponding phosphoramidite reagent by a manual coupling protocol. The preparation of the phosphoramidite reagents for incorporation of N2-(3-aminopropyl)-2′-deoxyguanosine is reported. The high-purity trimethylene DNA interstrand cross-link product is obtained through a nucleophilic aromatic substitution reaction between the N2-(3-aminopropyl)-2′-deoxyguanosine and 2-fluoro-O6-(trimethylsilylethyl)inosine containing oligodeoxynucleotides. PMID:25431636

  14. DNA-Protein Cross-Links: Formation, Structural Identities, and Biological Outcomes.

    Science.gov (United States)

    Tretyakova, Natalia Y; Groehler, Arnold; Ji, Shaofei

    2015-06-16

    complexity complicates structural and biological studies of DPC lesions. Two general strategies have been developed for creating DNA strands containing structurally defined, site-specific DPCs. Enzymatic methodologies that trap DNA modifying proteins on their DNA substrate are site specific and efficient, but do not allow for systematic studies of DPC lesion structure on their biological outcomes. Synthetic methodologies for DPC formation are based on solid phase synthesis of oligonucleotide strands containing protein-reactive unnatural DNA bases. The latter approach allows for a wider range of protein substrates to be conjugated to DNA and affords a greater flexibility for the attachment sites within DNA. In this Account, we outline the chemistry of DPC formation in cells, describe our recent efforts to identify the cross-linked proteins by mass spectrometry, and discuss various methodologies for preparing DNA strands containing structurally defined, site specific DPC lesions. Polymerase bypass experiments conducted with model DPCs indicate that the biological outcomes of these bulky lesions are strongly dependent on the peptide/protein size and the exact cross-linking site within DNA. Future studies are needed to elucidate the mechanisms of DPC repair and their biological outcomes in living cells.

  15. Cross-linking da cornea: protocolo padrão

    Directory of Open Access Journals (Sweden)

    Marcony R. Santhiago

    Full Text Available RESUMO O objetivo desta revisão é de determinar as indicações e eficácia da cirurgia que promove novas ligações covalentes entre as fibras de colágeno da córnea, conhecida como Cross-Linking (CXL, assim como esclarecer seus objetivos. O ceratocone é uma doença ectasica da córnea, bilateral, assimétrica, que, principalmente, cursa com encurvamento e afinamentos progressivo, e se inicia em geral na segunda década de vida. O uso primário do CXL tem sido na interrupção da progressão do Ceratocone. Apesar do conhecido encurvamento no estroma da córnea ocorrer nesses pacientes, a fisiopatologia por trás do ceratocone ainda é desconhecida e parece ser multifatorial. Pela evidencia literária disponível até o momento, o CXL da córnea esta, portanto indicado nos pacientes com doença em progressão. Concluímos que existe evidencia suficiente para afirmar que o CXL da córnea é eficaz na estabilização da doença ectásica da cornea.

  16. Cross-linking of polytetrafluoroethylene during room-temperature irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Pugmire, David L [Los Alamos National Laboratory; Wetteland, Chris J [Los Alamos National Laboratory; Duncan, Wanda S [Los Alamos National Laboratory; Lakis, Rollin E [Los Alamos National Laboratory; Schwartz, Daniel S [Los Alamos National Laboratory

    2008-01-01

    Exposure of polytetrafluoroethylene (PTFE) to {alpha}-radiation was investigated to detennine the physical and chemical effects, as well as to compare and contrast the damage mechanisms with other radiation types ({beta}, {gamma}, or thermal neutron). A number of techniques were used to investigate the chemical and physical changes in PTFE after exposure to {alpha}-radiation. These techniques include: Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and fluorescence spectroscopy. Similar to other radiation types at low doses, the primary damage mechanism for the exposure of PTFE to {alpha}-radiation appears to be chain scission. Increased doses result in a change-over of the damage mechanism to cross-linking. This result is not observed for any radiation type other than {alpha} when irradiation is performed at room temperature. Finally, at high doses, PTFE undergoes mass-loss (via smallfluorocarbon species evolution) and defluorination. The amount and type of damage versus sample depth was also investigated. Other types of radiation yield damage at depths on the order of mm to cm into PTFE due to low linear energy transfer (LET) and the correspondingly large penetration depths. By contrast, the {alpha}-radiation employed in this study was shown to only induce damage to a depth of approximately 26 {mu}m, except at very high doses.

  17. Subclinical inflammatory response after accelerated corneal cross-linking

    Institute of Scientific and Technical Information of China (English)

    Hassan Hashemi; Nahid Ashraf; Ebrahim Jafarzadehpur; Alireza Hedayatfar; Soheila Asgari

    2016-01-01

    Background: To evaluate the inlfammatory response after accelerated collagen cross-linking (CXL) in eyes with keratoconus. Methods: Consecutive eyes with keratoconus undergoing CXL surgery were included in this non-randomized interventional study. Aqueous lfare was measured pre- and post-operatively with a laser lfare photometer at 1 week, 1, 3 and 6 months after CXL. Results: Sixty eyes of 60 patients were entered into the study. Before CXL, the mean lfare value was 4.5 photons per millisecond (ph/ms). The lfare values observed at week 1 (7.1 ph/ms; P=0.008), month 1 (6.5 ph/ms; P=0.04), month 3 (6.7 ph/ms; P=0.004) and month 6 (6.7 ph/ms; P=0.004) were signiifcantly higher compared to baseline. Flare values were not signiifcantly different from week 1 up to 6 months after CXL (P=0.930). No statistically significant correlation was detected between the amount of inlfammation and keratometric indices. Conclusions: Accelerated CXL in patients with keratoconus may cause a subclinical inflammatory response which is evident as slight but rather long-lasting rise of aqueous lfare.

  18. Pyridinium cross-links in heritable disorders of collagen

    Energy Technology Data Exchange (ETDEWEB)

    Pasquali, M.; Still, M.J.; Dembure, P.P. [Emory Univ., Atlanta, GA (United States)] [and others

    1995-12-01

    Ehlers-Danlos syndrome (EDS) is a heterogeneous group of inherited disorders of collagen that is characterized by skin fragility, skin hyperextensibility, and joint hypermobility. EDS type VI is caused by impaired collagen lysyl hydroxylase (procollagen-lysine, 2-oxoglutarate 5-dioxygenase; E.C.1.14.11.4), the ascorbate-dependent enzyme that hydroxylates lysyl residues on collagen neopeptides. Different alterations in the gene for collagen lysyl hydroxylase have been reported in families with EDS type VI. In EDS type VI, impairment of collagen lysyl hydroxylase results in a low hydroxylysine content in mature collagen. Hydroxylysine is a precursor of the stable, covalent, intermolecular cross-links of collagen, pyridinoline (Pyr), and deoxypyridinoline (Dpyr). Elsewhere we reported in preliminary form that patients with EDS type VI had a distinctive alteration in the urinary excretion of Pyr and Dpyr. In the present study, we confirm that the increased Dpyr/Pyr ratio is specific for EDS type VI and is not observed in other inherited or acquired collagen disorders. In addition, we find that skin from patients with EDS type VI has reduced Pyr and increased Dpyr, which could account for the organ pathology. 19 refs., 1 tab.

  19. Analysis of protein-nucleic acid interactions by photochemical cross-linking and mass spectrometry

    DEFF Research Database (Denmark)

    Steen, Hanno; Jensen, Ole Nørregaard

    2002-01-01

    Photochemical cross-linking is a commonly used method for studying the molecular details of protein-nucleic acid interactions. Photochemical cross-linking aids in defining nucleic acid binding sites of proteins via subsequent identification of cross-linked protein domains and amino acid residues....... Mass spectrometry (MS) has emerged as a sensitive and efficient analytical technique for determination of such cross-linking sites in proteins. The present review of the field describes a number of MS-based approaches for the characterization of cross-linked protein-nucleic acid complexes...... and for sequencing of peptide-nucleic acid heteroconjugates. The combination of photochemical cross-linking and MS provides a fast screening method to gain insights into the overall structure and formation of protein-oligonucleotide complexes. Because the analytical methods are continuously refined and protein...

  20. Characterization of the deoxyguanosine-lysine cross-link of methylglyoxal.

    Science.gov (United States)

    Petrova, Katya V; Millsap, Amy D; Stec, Donald F; Rizzo, Carmelo J

    2014-06-16

    Methylglyoxal is a mutagenic bis-electrophile that is produced endogenously from carbohydrate precursors. Methylglyoxal has been reported to induce DNA-protein cross-links (DPCs) in vitro and in cultured cells. Previous work suggests that these cross-links are formed between guanine and either lysine or cysteine side chains. However, the chemical nature of the methylglyoxal induced DPC have not been determined. We have examined the reaction of methylglyoxal, deoxyguanosine (dGuo), and Nα-acetyllysine (AcLys) and determined the structure of the cross-link to be the N2-ethyl-1-carboxamide with the lysine side chain amino group (1). The cross-link was identified by mass spectrometry and the structure confirmed by comparison to a synthetic sample. Further, the cross-link between methylglyoxal, dGuo, and a peptide (AcAVAGKAGAR) was also characterized. The mechanism of cross-link formation is likely to involve an Amadori rearrangement.

  1. An Open Data Format for Visualization and Analysis of Cross-Linked Mass Spectrometry Results.

    Science.gov (United States)

    Hoopmann, Michael R; Mendoza, Luis; Deutsch, Eric W; Shteynberg, David; Moritz, Robert L

    2016-11-01

    Protein-protein interactions are an important element in the understanding of protein function, and chemical cross-linking shotgun mass spectrometry is rapidly becoming a routine approach to identify these specific interfaces and topographical interactions. Protein cross-link data analysis is aided by dozens of algorithm choices, but hindered by a lack of a common format for representing results. Consequently, interoperability between algorithms and pipelines utilizing chemical cross-linking remains a challenge. pepXML is an open, widely-used format for representing spectral search algorithm results that has facilitated information exchange and pipeline development for typical shotgun mass spectrometry analyses. We describe an extension of this format to incorporate cross-linking spectral search results. We demonstrate application of the extension by representing results of multiple cross-linking search algorithms. In addition, we demonstrate adapting existing pepXML-supporting software pipelines to analyze protein cross-linking results formatted in pepXML. Graphical Abstract ᅟ.

  2. Tailoring the properties of cholecyst-derived extracellular matrix using carbodiimide cross-linking.

    LENUS (Irish Health Repository)

    Burugapalli, Krishna

    2009-01-01

    Modulation of properties of extracellular matrix (ECM) based scaffolds is key for their application in the clinical setting. In the present study, cross-linking was used as a tool for tailoring the properties of cholecyst-derived extracellular matrix (CEM). CEM was cross-linked with varying cross-linking concentrations of N,N-(3-dimethyl aminopropyl)-N\\'-ethyl carbodiimide (EDC) in the presence of N-hydroxysuccinimide (NHS). Shrink temperature measurements and ATR-FT-IR spectra were used to determine the degree of cross-linking. The effect of cross-linking on degradation was tested using the collagenase assay. Uniaxial tensile properties and the ability to support fibroblasts were also evaluated as a function of cross-linking. Shrink temperature increased from 59 degrees C for non-cross-linked CEM to 78 degrees C for the highest EDC cross-linking concentration, while IR peak area ratios for the free -NH(2) group at 3290 cm(-1) to that of the amide I band at 1635 cm(-1) decreased with increasing EDC cross-linking concentration. Collagenase assay demonstrated that degradation rates for CEM can be tailored. EDC concentrations 0 to 0.0033 mmol\\/mg CEM were the cross-linking concentration range in which CEM showed varied susceptibility to collagenase degradation. Furthermore, cross-linking concentrations up to 0.1 mmol EDC\\/mg CEM did not have statistically significant effect on the uniaxial tensile strength, as well as morphology, viability and proliferation of fibroblasts on CEM. In conclusion, the degradation rates of CEM can be tailored using EDC-cross-linking, while maintaining the mechanical properties and the ability of CEM to support cells.

  3. In vitro cross-linking of elastin peptides and molecular characterization of the resultant biomaterials.

    Science.gov (United States)

    Heinz, Andrea; Ruttkies, Christoph K H; Jahreis, Günther; Schräder, Christoph U; Wichapong, Kanin; Sippl, Wolfgang; Keeley, Fred W; Neubert, Reinhard H H; Schmelzer, Christian E H

    2013-04-01

    Elastin is a vital protein and the major component of elastic fibers which provides resilience to many vertebrate tissues. Elastin's structure and function are influenced by extensive cross-linking, however, the cross-linking pattern is still unknown. Small peptides containing reactive allysine residues based on sequences of cross-linking domains of human elastin were incubated in vitro to form cross-links characteristic of mature elastin. The resultant insoluble polymeric biomaterials were studied by scanning electron microscopy. Both, the supernatants of the samples and the insoluble polymers, after digestion with pancreatic elastase or trypsin, were furthermore comprehensively characterized on the molecular level using MALDI-TOF/TOF mass spectrometry. MS(2) data was used to develop the software PolyLinX, which is able to sequence not only linear and bifunctionally cross-linked peptides, but for the first time also tri- and tetrafunctionally cross-linked species. Thus, it was possible to identify intra- and intermolecular cross-links including allysine aldols, dehydrolysinonorleucines and dehydromerodesmosines. The formation of the tetrafunctional cross-link desmosine or isodesmosine was unexpected, however, could be confirmed by tandem mass spectrometry and molecular dynamics simulations. The study demonstrated that it is possible to produce biopolymers containing polyfunctional cross-links characteristic of mature elastin from small elastin peptides. MALDI-TOF/TOF mass spectrometry and the newly developed software PolyLinX proved suitable for sequencing of native cross-links in proteolytic digests of elastin-like biomaterials. The study provides important insight into the formation of native elastin cross-links and represents a considerable step towards the characterization of the complex cross-linking pattern of mature elastin. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Radiation cross-linking in ultra-high molecular weight polyethylene for orthopaedic applications

    OpenAIRE

    Oral, Ebru; Muratoglu, Orhun K.

    2007-01-01

    The motivation for radiation cross-linking of ultra-high molecular weight polyethylene (UHMWPE) is to increase its wear resistance to be used as bearing surfaces for total joint arthroplasty. However, radiation also leaves behind long-lived residual free radicals in this polymer, the reactions of which can detrimentally affect mechanical properties. In this review, we focus on the radiation cross-linking and oxidative stability of first and second generation highly cross-linked UHMWPEs develo...

  5. Effect of Cross-Linking and Enzymatic Hydrolysis Composite Modification on the Properties of Rice Starches

    Directory of Open Access Journals (Sweden)

    Gao-Qiang Liu

    2012-07-01

    Full Text Available Native rice starch lacks the versatility necessary to function adequately under rigorous industrial processing, so modified starches are needed to meet the functional properties required in food products. This work investigated the impact of enzymatic hydrolysis and cross-linking composite modification on the properties of rice starches. Rice starch was cross-linked with epichlorohydrin (EPI with different concentrations (0.5%, 0.7%, 0.9% w/w, on a dry starch basis, affording cross-linked rice starches with the three different levels of cross-linking that were named R1, R2, and R3, respectively. The cross-linked rice starches were hydrolyzed by α-amylase and native, hydrolyzed, and hydrolyzed cross-linked rice starches were comparatively studied. It was found that hydrolyzed cross-linked rice starches showed a lower the degree of amylase hydrolysis compared with hydrolyzed rice starch. The higher the degree of cross-linking, the higher the capacity to resist enzyme hydrolysis. Hydrolyzed cross-linked rice starches further increased the adsorptive capacities of starches for liquids and decreased the trend of retrogradation, and it also strengthened the capacity to resist shear compared to native and hydrolyzed rice starches.

  6. Release effect of the active ingredients using a radiation cross linking technology

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, Seung Hyun; Ahn, Sung Jun; Park, Jong Seok; Jeong, Sung In; Gwon, Hui Jeong; Lim, Youn Mook [Research Division for Industry and Environment, Korea Atomic Energy Research Institute, Jeongeup (Korea, Republic of); Lee, Dong Yun [Dept. of Bioengineering, Division of Applied Chemical and Bio Engineering, Hanyang University, Seoul (Korea, Republic of)

    2015-12-15

    Typical radiation cross-linked hydrogels has the characteristic that high water content, but low emission efficiency of active ingredients. Therefore, the hydrogel was prepared by the addition to collagen, which is closely related to the formation of skin wrinkles in biocompatibility and highly water-soluble carboxymethyl cellulose sodium salt (CMC) in order to preparation of hydrogels has excellent emission efficiency of active ingredients. Hydrogels were prepared by dissolving CMC and collagen each of 0.5%, 10% concentration in deionized water. Then, prepared hydrogels are performed by gamma-radiation at 1, 3, 5 kGy irradiation dose. The results showed that the gel fraction of after irradiated 3 kGy hydrogel was higher than before irradiated gelation as long as the 55.3%. The swelling rate of irradiated 3 kGy hydrogel was lower than the non-irradiated sample. The compressive strength of 3 kGy irradiated hydrogel was the highest. The visco-elastic did not show any significant differences, even after irradiation. The CMC hydrogel in this study suggested a potential use as a material for the mask pack for improved emission efficiency of the active ingredient and anti-wrinkles.

  7. Electrochemical Study of Biotin-Modified Self-Assembled Monolayers: Recommendations for Robust Preparation

    Directory of Open Access Journals (Sweden)

    Richard J.C. Brown

    2006-01-01

    Full Text Available The development of the underpinning methodology for the production of robust, well-formed, and densely packed biotin-HPDP functionalised gold surfaces, the crucial first step in immobilising bimolecules on surfaces, is described. Self-assembled monolayers (SAMs with biotin end-groups were prepared on polycrystalline gold surfaces according to a published method. The layers formed were studied using cyclic voltammetry to determine the composition of the layer and its quality. Crystal impedance spectroscopy was also applied as a complimentary indicator of the composition of the layer.For the first time, the effect of assembly time on the properties of the layer was studied along with the composition of the layer and the ability of the precursor molecule to self-assemble by oxidative addition.

  8. Alkaline battery containing a separator of a cross-linked copolymer of vinyl alcohol and unsaturated carboxylic acid

    Science.gov (United States)

    Hsu, L. C.; Philipp, W. H.; Sheibley, D. W.; Gonzalez-Sanabria, O. D. (Inventor)

    1985-01-01

    A battery separator for an alkaline battery is described. The separator comprises a cross linked copolymer of vinyl alcohol units and unsaturated carboxylic acid units. The cross linked copolymer is insoluble in water, has excellent zincate diffusion and oxygen gas barrier properties and a low electrical resistivity. Cross linking with a polyaldehyde cross linking agent is preferred.

  9. ROLE OF CORNEAL COLLAGEN CROSS LINKING IN KERATOCONUS

    Directory of Open Access Journals (Sweden)

    Atul

    2015-09-01

    Full Text Available To evaluate the outcome of collagen cross linkage using riboflavin 0.1% and ultraviolet A radiation of a wavelength 370nm . PURPOSE : To determine the effect of collagen cross linking for keratoconus on pachymetry , corneal topography, uncorrected visual acuity, specular count, IOP at 1, 3, 6 months . METHODS : The current study was designed as a prospective interventional trial of corneal collagen cross - linking in subjects with progressive keratoconus between a period of J anuary 2013 to J uly 2014 including 50 eyes of 30 patients. This study rece ived approval from Ethics committee. Informed written consent was obtained from all patients prior to treatment. RESULTS: Mean follow up period of 6 months. There was statistically significant decline in effective k readings from mean pre op (51.7D to pos t op value (49.65D . Pachymetry showed initial increase post operatively followed by reduction in corneal thickness in 3 month s follow up , followed by gradual increase in thickness over a period of 6 months though it was not equivalent to pre - operative values. paired t test p value was 0.00 1 in 1 n 3 month and 0. 043 in 6 month, concluding significant reduction in early post op period with im provement over time . Specular count reduced from pre - op (2673.80 levels to post - op (2654.60 levels ,the reduction in specular count was not statistically significant P value (0.014 The uncorrected visual acuity showed decrease in refractive error with in crease in visual acuity gradually over 6 months, log MAR scale visual acuity was used for statistical analysis with P value (0.001 which was statistically significant .visual acuity improved by 1.5 lines in snellens equivalence or from 0.5 to 0.4 in log MA R char y ± 20cells/mm 3 , P value(0. 001 . IOP statically show ed no significant change in pre - operative and post operatively , paired t test p value was 0. 44 showing it was not significant . CONCLUSIONS : 1. Visual acuity improved in

  10. Encapsulation of volatiles by homogenized partially-cross linked alginates.

    Science.gov (United States)

    Inguva, Pavan K; Ooi, Shing Ming; Desai, Parind M; Heng, Paul W S

    2015-12-30

    Cross-linked calcium alginate gels are too viscous to be efficaciously incorporated into spray dried formulations. Thus, viscosity reduction is essential to ensure the processability of calcium alginate gels to be sprayed. Viscosity reduction by high pressure homogenization can open new formulation possibilities. Presently, testing of microcapsule integrity is also limited because either single particle tests neglect collective particle behaviours in bulk or bulk testing methods are often associated with single compressions which may not fully characterize individual particle strengths. The aim of this study was sub-divided into three objectives. First objective was to evaluate the impact of high pressure homogenization on gel viscosity. Second objective was to explore the use of the homogenized gels with modified starch for microencapsulation by spray drying. The final objective was to develop a stamping system as microcapsule strength tester that can assess microcapsules in bulk and evaluate the impact of multiple compressions. Collectively, this study would lead towards developing a pressure-activated patch of microcapsules with encapsulated volatiles and the method to assess the patch efficacy. The alginate gels largely experienced an exponential decay in viscosity when homogenized. Furthermore, the homogenized gels were successfully incorporated in spray drying formulations for microencapsulation. The custom-designed microcapsule strength tester was successfully used and shown to possess the required sensitivity to discern batches of microcapsules containing volatiles to have different release profiles. Addition of homogenized gels strengthened the microcapsules only at high wall to core ratios with low mass-load alginate gels. High mass-load gels weaken the microcapsules, exhibiting a higher release at low stamping pressures and wrinkling on the microcapsules surface.

  11. Integrated Cryogenic Satellite Communications Cross-Link Receiver Experiment

    Science.gov (United States)

    Romanofsky, R. R.; Bhasin, K. B.; Downey, A. N.; Jackson, C. J.; Silver, A. H.; Javadi, H. H. S.

    1995-01-01

    An experiment has been devised which will validate, in space, a miniature, high-performance receiver. The receiver blends three complementary technologies; high temperature superconductivity (HTS), pseudomorphic high electron mobility transistor (PHEMT) monolithic microwave integrated circuits (MMIC), and a miniature pulse tube cryogenic cooler. Specifically, an HTS band pass filter, InP MMIC low noise amplifier, HTS-sapphire resonator stabilized local oscillator (LO), and a miniature pulse tube cooler will be integrated into a complete 20 GHz receiver downconverter. This cooled downconverter will be interfaced with customized signal processing electronics and integrated onto the space shuttle's 'HitchHiker' carrier. A pseudorandom data sequence will be transmitted to the receiver, which is in low Earth orbit (LEO), via the Advanced Communication Technology Satellite (ACTS) on a 20 GHz carrier. The modulation format is QPSK and the data rate is 2.048 Mbps. The bit error rate (BER) will be measured in situ. The receiver is also equipped with a radiometer mode so that experiment success is not totally contingent upon the BER measurement. In this mode, the receiver uses the Earth and deep space as a hot and cold calibration source, respectively. The experiment closely simulates an actual cross-link scenario. Since the receiver performance depends on channel conditions, its true characteristics would be masked in a terrestrial measurement by atmospheric absorption and background radiation. Furthermore, the receiver's performance depends on its physical temperature, which is a sensitive function of platform environment, thermal design, and cryocooler performance. This empirical data is important for building confidence in the technology.

  12. The theory and art of corneal cross-linking

    Directory of Open Access Journals (Sweden)

    Rebecca McQuaid

    2013-01-01

    Full Text Available Before the discovery of corneal cross-linking (CXL, patients with keratoconus would have had to undergo corneal transplantation, or wear rigid gas permeable lenses (RGPs that would temporarily flatten the cone, thereby improving the vision. The RGP contact lens (CL would not however alter the corneal stability and if the keratoconus was progressive, the continued steepening of the cone would occur under the RGP CL. To date, the Siena Eye has been the largest study to investigate long term effects of standard CXL. Three hundred and sixty-three eyes were treated and monitored over 4 years, producing reliable long-term results proving long-term stability of the cornea by halting the progression of keratoconus, and proving the safety of the procedure. Traditionally, CXL requires epithelial removal prior to corneal soakage of a dextran-based 0.1% riboflavin solution, followed by exposure of ultraviolet-A (UV-A light for 30 min with an intensity of 3 mW/cm2. A series of in vitro investigations on human and porcine corneas examined the best treatment parameters for standard CXL, such as riboflavin concentration, intensity, wavelength of UV-A light, and duration of treatment. Photochemically, CXL is achieved by the generation of chemical bonds within the corneal stroma through localized photopolymerization, strengthening the cornea whilst minimizing exposure to the surrounding structures of the eye. In vitro studies have shown that CXL has an effect on the biomechanical properties of the cornea, with an increased corneal rigidity of approximately 70%. This is a result of the creation of new chemical bonds within the stroma.

  13. Transglutaminases: widespread cross-linking enzymes in plants.

    Science.gov (United States)

    Serafini-Fracassini, Donatella; Del Duca, Stefano

    2008-08-01

    Transglutaminases have been studied in plants since 1987 in investigations aimed at interpreting some of the molecular mechanisms by which polyamines affect growth and differentiation. Transglutaminases are a widely distributed enzyme family catalysing a myriad of biological reactions in animals. In plants, the post-translational modification of proteins by polyamines forming inter- or intra-molecular cross-links has been the main transglutaminase reaction studied. The few plant transglutaminases sequenced so far have little sequence homology with the best-known animal enzymes, except for the catalytic triad; however, they share a possible structural homology. Proofs of their catalytic activity are: (a) their ability to produce glutamyl-polyamine derivatives; (b) their recognition by animal transglutaminase antibodies; and (c) biochemical features such as calcium-dependency, etc. However, many of their fundamental biochemical and physiological properties still remain elusive. It has been detected in algae and in angiosperms in different organs and sub-cellular compartments, chloroplasts being the best-studied organelles. Possible roles concern the structural modification of specific protein substrates. In chloroplasts, transglutaminases appear to stabilize the photosynthetic complexes and Rubisco, being regulated by light and other factors, and possibly exerting a positive effect on photosynthesis and photo-protection. In the cytosol, they modify cytoskeletal proteins. Preliminary reports suggest an involvement in the cell wall construction/organization. Other roles appear to be related to fertilization, abiotic and biotic stresses, senescence and programmed cell death, including the hypersensitive reaction. The widespread occurrence of transglutaminases activity in all organs and cell compartments studied suggests a relevance for their still incompletely defined physiological roles. At present, it is not possible to classify this enzyme family in plants owing to

  14. Biopolymers from vegetable oils via catalyst- and solvent-free "click" chemistry: effects of cross-linking density.

    Science.gov (United States)

    Hong, Jian; Luo, Qiang; Wan, Xianmei; Petrović, Zoran S; Shah, Bipin K

    2012-01-09

    New monomers were prepared by introducing the azide groups in castor, canola, corn, soybean, and linseed oils. Polymerization of the azidated oils with alkynated soybean oil under thermal "click" chemistry conditions (without using a solvent or a catalyst) yielded fully cross-linked elastomers (1-5) of almost the same density (1.05 × 10(-3) kg/m(3)). The degree of cross-linking gradually increased from the castor-derived polymer (220 mol/m(3)) to the linseed-derived polymer (683 mol/m(3)). A systematic correlation between the degree of cross-linking and the thermal and mechanical properties was observed in these biopolymers. Tensile strength (0.62-3.39 MPa) and glass transition temperature (-5 to 16 °C) increased and the linear thermal expansion coefficient decreased in the series from the canola-derived polymer (2) to the linseed-derived polymer (5). The castor-derived polymer (1) that possesses an additional hydroxyl group per fatty acid chain behaved differently.

  15. Adsorptive removal of lead and cadmium ions using Cross -linked CMC Schiff base: Isotherm, Kinetics and Catalytic Activity

    Directory of Open Access Journals (Sweden)

    P. Moganavally

    2016-03-01

    Full Text Available Water plays a vital role to human and other living organisms. Due to the effluent coming from chemical industries, the industrial activity, contamination of ground water level is goes on increasing nowadays. Therefore, there is a need to develop technologies that can remove toxic pollutants in wastewater. Hence the cross linked Carboxymethyl chitosan(CMC/ 2,3-dimethoxy Benzaldehyde Schiff base complex has been synthesized and characterized by using FT-IR and SEM analysis. All these results revealed that cross linked Schiff base has formed with high adsorption capacity. The prepared effective adsorbent used for the removal of heavy metals like lead (II and cadmium (II ions from aqueous solution and the adsorption data follow the Freundlich model, which follows pseudo first order kinetics. Effect of various parameters like solution pH, adsorbent dose and contact time for the removal of heavy metals has been studied. The synthesized sample undergoes catalytic oxidation process significantly at 24 hrs. The results showed that cross linked Schiff base is an effective, eco-friendly, low-cost adsorbent.

  16. Polysiloxane Functionalized Carbon Dots and Their Cross-Linked Flexible Silicone Rubbers for Color Conversion and Encapsulation of White LEDs.

    Science.gov (United States)

    Wang, Yunfeng; Yin, Zhengmao; Xie, Zheng; Zhao, Xinxin; Zhou, Chuanjian; Zhou, Shuyun; Chen, Ping

    2016-04-20

    In this work, aminopropylmethylpolysiloxane (AMS) functionalized luminescent carbon dots (AMS-CDs) were prepared via a one-step solvothermal method. AMS-CDs could be self- or co-cross-linking with AMS to form 3D flexible transparent silicone rubbers (SRs) where CDs acted as cross-linking points, so the loading fraction of AMS-CDs could be adjusted from 10 to 100 wt %, thus modulating fluorescence properties and flexibility of silicone rubbers. Because of the self-curing property and high thermal stability, AMS-CDs were also studied in white LEDs (WLEDs), serving as a color conversion and encapsulation layer of GaN based blue LEDs simultaneously that would avoid the traditional problem of poor compatibility between emitting and packaging materials. And the color coordinate of AMS-CDs based WLEDs (0.33, 0.28) was very close to the pure white light. In addition, the obtained CDs cross-linked SRs had good transparency (T > 80%) at 510-1400 nm and high refractive indexes (1.33-1.54) that could meet the need of commercial packaging materials and optical application. AMS-CDs were also promising to be used in the UV LEDs based WLEDs according to their wide wavelength emission and flexible optoelectronic device.

  17. Shell-cross-linked micelles from PNIPAM-b-(PLL)2 Y-shaped miktoarm star copolymer as drug carriers.

    Science.gov (United States)

    Li, Li-Ying; He, Wei-Dong; Li, Jian; Zhang, Bo-Yu; Pan, Ting-Ting; Sun, Xiao-Li; Ding, Zong-Lei

    2010-07-12

    Well-defined AB2 Y-shaped miktoarm star copolymers of PNIPAM-b-(PZLL)2 and PNIPAM-b-(PLL)2 were synthesized through the combination of atom transfer radical polymerization (ATRP), ring-opening polymerization (ROP), and click chemistry, where PNIPAM, PZLL, and PLL are poly(N-isopropylacrylamide), poly(epsilon-benzyloxy-carbonyl-L-lysine), and poly(L-lysine), respectively. Propargyl amine was employed as ROP initiator for the preparation of alkynyl-terminated PZLL. Diazide-terminated PNIPAM was obtained with an azide-containing ATRP initiator. The subsequent click reaction led to the formation of PNIPAM-b-(PZLL)2. After the removal of the benzyloxycarbonyl group, water-soluble PNIPAM-b-(PLL)2 was obtained. The core-shell micelles of PNIPAM-b-(PLL)2 were formed above lower critical solution temperature of PNIPAM block. At this temperature, the shell cross-linking was performed through the reaction between glutaraldehyde and the primary amine groups of the PLL shell, affording the micelles with the endurance to temperature and pH changes. These shell-cross-linked micelles were used as drug nanocarriers and the release profile was dually controlled by the solution temperature and the cross-linking degree.

  18. Zr(IV) loaded cross-linked chitosan beads with enhanced surface area for the removal of nitrate and phosphate.

    Science.gov (United States)

    Sowmya, Appunni; Meenakshi, Sankaran

    2014-08-01

    In this work, a new method namely silica dissolution method, has been adapted to increase the surface area of the cross-linked chitosan beads. Zr(IV) was loaded in the cross-linked chitosan beads in order to make it selective for the nitrate and phosphate anions from aqueous solutions. Zr(IV) loaded cross-linked chitosan beads prepared by normal method (ZrCB) and silica dissolution method (SD-ZrCB) were characterised using N2 adsorption/desorption studies, SEM, EDAX, XRD, FTIR, TGA, DTA and water regain property. The SD-ZrCB exhibited higher N2 adsorption, water regain property as well as anion adsorption capacity than ZrCB. Batch method was adapted for the adsorption studies. The nitrate and phosphate adsorbed SD-ZrCB was regenerated using 0.025M NaCl solution. There was not much drop in adsorption capacities up to 10th regeneration cycle. Freundlich adsorption isotherm was the best fit adsorption isotherm among Freundlich, Langmuir and Dubinin-Radushkevich (D-R) isotherms which have been used to fit the nitrate and phosphate adsorption data. Thermodynamic parameters such as ΔG°, ΔH° and ΔS° were calculated in order to understand the nature of adsorption process.

  19. Feruloylated arabinoxylans are oxidatively cross-linked by extracellular maize peroxidase but not by horseradish peroxidase.

    Science.gov (United States)

    Burr, Sally J; Fry, Stephen C

    2009-09-01

    Covalent cross-linking of soluble extracellular arabinoxylans in living maize cultures, which models the cross-linking of wall-bound arabinoxylans, is due to oxidation of feruloyl esters to oligoferuloyl esters and ethers. The oxidizing system responsible could be H2O2/peroxidase, O2/laccase, or reactive oxygen species acting non-enzymically. To distinguish these possibilities, we studied arabinoxylan cross-linking in vivo and in vitro. In living cultures, exogenous, soluble, extracellular, feruloylated [pentosyl-3H]arabinoxylans underwent cross-linking, beginning abruptly 8 d after sub-culture. Cross-linking was suppressed by iodide, an H2O2 scavenger, indicating dependence on endogenous H2O2. However, exogenous H2O2 did not cause precocious cross-linking, despite the constant presence of endogenous peroxidases, suggesting that younger cultures contained natural cross-linking inhibitors. Dialysed culture-filtrates cross-linked [3H]arabinoxylans in vitro only if H2O2 was also added, indicating a peroxidase requirement. This cross-linking was highly ionic-strength-dependent. The peroxidases responsible were heat-labile, although relatively heat-stable peroxidases (assayed on o-dianisidine) were also present. Surprisingly, added horseradish peroxidase, even after heat-denaturation, blocked the arabinoxylan-cross-linking action of maize peroxidases, suggesting that the horseradish protein was a competing substrate for [3H]arabinoxylan coupling. In conclusion, we show for the first time that cross-linking of extracellular arabinoxylan in living maize cultures is an action of apoplastic peroxidases, some of whose unusual properties we report.

  20. Analytical characterisation of glutardialdehyde cross-linking products in gelatine-gum arabic complex coacervates

    Energy Technology Data Exchange (ETDEWEB)

    Fuguet, Elisabet [Advanced Measurement and Imaging, Unilever Food and Health Research Institute, Olivier van Noortlaan 120, 3133 AT Vlaardingen (Netherlands)], E-mail: eli.fuguet@gmail.com; Platerink, Chris van [Advanced Measurement and Imaging, Unilever Food and Health Research Institute, Olivier van Noortlaan 120, 3133 AT Vlaardingen (Netherlands); Department of Biomolecular Mass Spectrometry, Bijvoet Center for Biomolecular Research, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht (Netherlands); Janssen, Hans-Gerd [Advanced Measurement and Imaging, Unilever Food and Health Research Institute, Olivier van Noortlaan 120, 3133 AT Vlaardingen (Netherlands); van' t Hoff Institute for Molecular Sciences, University of Amsterdam, Nieuwe Achtergracht 166, 1018 WV Amsterdam (Netherlands)

    2007-11-26

    Encapsulates having shells of cross-linked mixtures of proteins and polysaccharides are widely used in the food and pharmaceutical industry for controlled release of actives and flavour compounds. In order to be able to predict the behaviour and the release characteristics of the microcapsules, a better understanding of the nature and extent of the cross-linking reaction is needed. Several analytical techniques were applied for the characterisation of glutardialdehyde (GDA) cross-linked encapsulates made of gelatine and gum arabic. To allow the use of sensitive, high-resolution methods such as chromatography and mass spectrometry, the sample first had to be hydrolysed. In this way, a mixture of amino acids, small peptides and the cross-link moieties was obtained. High-resolution liquid chromatography coupled to high-resolution mass spectrometry (HPLC-MS) was applied to detect possible cross-link markers through a comparison of HPLC-MS mass-chromatograms obtained for cross-linked and non-cross-linked coacervates. HPLC-MS/MS was used to identify the species responsible for the differences. Cross-linking occurred between GDA molecules and lysine and hydroxylysine {epsilon}-amino groups, and up to eight cross-link products of different nature could be identified. They included pyridinium ions and Schiff bases, and also unreacted GDA condensation products. Next, based on the insight gained in the possible chemical structures present in the cross-link markers, methods for selective labelling of these functionalities were employed to allow easier detection of related reaction products. Both liquid chromatography (LC) and gas chromatography (GC) were used in these experiments. Unfortunately, these approaches failed to detect new cross-link markers, most likely as a result of the low levels at which these are present.

  1. Feruloylated Arabinoxylans Are Oxidatively Cross-Linked by Extracellular Maize Peroxidase but Not by Horseradish Peroxidase

    Institute of Scientific and Technical Information of China (English)

    Sally J. Burr; Stephen C. Fry

    2009-01-01

    Covalent cross-linking of soluble extraceUular arabinoxylans in living maize cultures, which models the cross-linking of wall-bound arabinoxylans, is due to oxidation of feruloyl esters to oligoferuloyl esters and ethers. The oxidizing system responsible could be H_2O_2/peroxidase, O_2/laccase, or reactive oxygen species acting non-enzymically. To distinguish these possibilities, we studied arabinoxylan cross-linking in vivo and in vitro. In living cultures, exogenous, soluble, extra-cellular, feruloylated [pentosyl-~3H]arabinoxylans underwent cross-linking, beginning abruptly 8 d after sub-culture. Cross-linking was suppressed by iodide, an H_2O_2 scavenger, indicating dependence on endogenous H2O2. However, exogenous H_2O_2 did not cause precocious cross-linking, despite the constant presence of endogenous peroxidases, suggesting that younger cultures contained natural cross-linking inhibitors. Dialysed culture-filtrates cross-linked [~3H]arabinoxylans in vitro only if H_20_2 was also added, indicating a peroxiclase requirement. This cross-linking was highly ionic-strength-dependent. The peroxidases responsible were heat-labile, although relatively heat-stable peroxidases (assayed on o-dianisidine) were also present, Surprisingly, added horseradish peroxidase, even after heat-denaturation, blocked the arabinoxylan-cross-linking action of maize peroxidases, suggesting that the horseradish protein was a competing substrate for [~3H]arabino-xylan coupling. In conclusion, we show for the first time that cross-linking of extracellular arabinoxylan in living maize cultures is an action of apoplastic peroxidases, some of whose unusual properties we report.

  2. Absorbed Pb2+ and Cd2+ Ions in Water by Cross-Linked Starch Xanthate

    Directory of Open Access Journals (Sweden)

    Kai Feng

    2017-01-01

    Full Text Available A cross-linked starch xanthate was prepared by graft copolymerization of acrylamide and sodium acrylate onto starch xanthate using potassium persulfate and sodium hydrogen sulfite initiating system and N,N′-methylenebisacrylamide as a cross-linker. As this kind of cross-linked potato starch xanthate can effectively absorb heavy metal ions, it was dispersed in aqueous solutions of divalent heavy metal ions (Pb2+ and Cd2+ to investigate their absorbency by the polymer. Factors that can influence absorbency were investigated, such as the ratio of matrix to monomers, the amount of initiator and cross-linker, pH, and the concentration of metal ions. Results were reached and conclusion was drawn that the best synthetic conditions for the polymer adsorbing Pb2+ and Cd2+ were as follows: the quality ratio of matrix to monomers was 1 : 12 and 1 : 11, the amount of initiator was 2.4% and 3.2% of matrix, and the amount of cross-linker was 12 mg and 13 mg. When the initial concentration of ions was 10 mg/L, the highest quantities of adsorption of Pb2+ and Cd2+ were 47.11 mg/g and 36.55 mg/g. Adsorption mechanism was discussed by using Fourier transform infrared (FTIR spectroscopy, X-ray diffraction (XRD, scanning electron microscope (SEM, Energy Dispersive X-Ray Spectroscopy (EDS test, and adsorption kinetic simulation.

  3. Cross-Linking Density and Temperature Effects on the Self-Assembly of SiO2-PNIPAAm Core-Shell Particles at Interfaces

    NARCIS (Netherlands)

    Nazli, Kadriye Oezlem; Pester, Christian W.; Konradi, Artjom; Boeker, Alexander; van Rijn, Patrick

    2013-01-01

    SiO2PNIPAAm coreshell microgels (PNIPAAm=poly(N-isopropylacrylamide)) with various internal cross-linking densities and different degrees of polymerization were prepared in order to investigate the effects of stability, packing, and temperature responsiveness at polarapolar interfaces. The effects w

  4. Three methods for in situ cross-linking of polyvinyl alcohol films for application as ion-conducting membranes in potassium hydroxide electrolyte. [battery separators

    Science.gov (United States)

    Philipp, W. H.; Hsu, L. C.

    1979-01-01

    Three methods of in situ cross-linking polyvinyl alcohol films are presented. They are: (1) acetalization with a dialdehyde such as glutaraldehyde, (2) acetalization with aldehyde groups formed by selective oxidative cleaving of the few percent of 1,2 diol units present in polyvinyl alcohol, and (3) cross-linking by hydrogen abstraction by reaction with hydrogen atoms and hydroxyl radicals from irradiated water. For the third method, improvement in film conductivity in KOH solution at the expense of mechanical strength is obtained by the presence of polyacrylic acid in the polyvinyl alcohol films. Resistivities in 45 percent KOH are given for in situ cross-linked films prepared by each of the three methods.

  5. Physical Characterization Of High Amylose/Pectin Mixtures Cross-Linked With Sodium Trimetaphosphate; Caracterizacao fisica de misturas alta amilose/pectina reticuladas com trimetafosfato de sodio

    Energy Technology Data Exchange (ETDEWEB)

    Carbinatto, F.M.; Cury, B.S.F.; Evangelista, R.C., E-mail: curybsf@fcfar.unesp.b [UNESP, Araraquara, SP (Brazil). Fac. de Ciencias Farmaceuticas

    2010-07-01

    Some researches have reported that pectin and high amylose mixtures presented superior mechanical properties in relation to those of the isolated polymers. In this work, mixtures at different ratios (1:4; 1:1) of pectin and high amylose were crosslinked with sodium trimetaphosphate at different degrees by varying reaction conditions. All samples were characterized by rheological and X-ray diffraction analyses. Samples without cross-linker were prepared as control. The oscillatory dynamic tests showed that all samples exhibited predominant elastic behavior, although cross-linked samples presented higher G' values, suggesting that crosslinking by phosphorylation resulted in more strength structures. The diffractograms showed that cross-linked samples underwent structural modifications that resulted in increase of crystallinity due to cross-linking process. (author)

  6. Antimicrobial Properties of Microparticles Based on Carmellose Cross-Linked by Cu2+ Ions

    Directory of Open Access Journals (Sweden)

    Martina Kejdušová

    2015-01-01

    Full Text Available Carmellose (CMC is frequently used due to its high biocompatibility, biodegradability, and low immunogenicity for development of site-specific or controlled release drug delivery systems. In this experimental work, CMC dispersions in two different concentrations (1% and 2% cross-linked by copper (II ions (0.5, 1, 1.5, or 2.0 M CuCl2 were used to prepare microspheres with antimicrobial activity against Escherichia coli and Candida albicans, both frequently occurring pathogens which cause vaginal infections. The microparticles were prepared by an ionotropic gelation technique which offers the unique possibility to entrap divalent copper ions in a CMC structure and thus ensure their antibacterial activity. Prepared CMC microspheres exhibited sufficient sphericity. Both equivalent diameter and copper content were influenced by CMC concentration, and the molarity of copper (II solution affected only the copper content results. Selected samples exhibited stable but pH-responsive behaviour in environments which corresponded with natural (pH 4.5 and inflamed (pH 6.0 vaginal conditions. All the tested samples exhibited proven substantial antimicrobial activity against both Gram-negative bacteria Escherichia coli and yeast Candida albicans. Unexpectedly, a crucial parameter for microsphere antimicrobial activity was not found in the copper content but in the swelling capacity of the microparticles and in the degree of CMC surface shrinking.

  7. SYNTHESIS AND CATALYTIC PROPERTIES OF CROSS-LINKED HYDROPHOBICALLY ASSOCIATING POLY(ALKYLMETHYLDIALLYLAMMONIUM BROMIDES)

    NARCIS (Netherlands)

    WANG, GJ; ENGBERTS, JBFN

    1994-01-01

    Cross-linked, hydrophobically associating homo- and copolymers were synthesized by free-radical cyclo(co)polymerization of alkylmethyldiallylammonium bromide monomers with a small amount of N,N'-methylenebisacrylamide in aqueous solution using ammonium persulfate as the initiator. The cross-linked h

  8. Rheological properties of dispersions of enzymatically cross-linked apo-α-lactalbumin

    NARCIS (Netherlands)

    Saricay, Yunus; Wierenga, Peter A.; Vries, de Renko

    2016-01-01

    The enzymatic cross-linking of apo-α-lactalbumin (α-LA) with horseradish peroxidase (HRP) leads to the formation of hydrophilic protein aggregates with controlled size and architecture. We explore the rheological properties of dispersions of these HRP-cross-linked α-LA aggregates with a hydrodyna

  9. Covalently Cross-Linked Sulfone Polybenzimidazole Membranes with Poly(Vinylbenzyl Chloride) for Fuel Cell Applications

    DEFF Research Database (Denmark)

    Yang, Jingshuai; Aili, David; Li, Qingfeng;

    2013-01-01

    Covalently cross-linked polymer membranes were fabricated from poly(aryl sulfone benzimidazole) (SO(2) PBI) and poly(vinylbenzyl chloride) (PVBCl) as electrolytes for high-temperature proton-exchange-membrane fuel cells. The cross-linking imparted organo insolubility and chemical stability against...

  10. Effects of Supercritical CO 2 Conditioning on Cross-Linked Polyimide Membranes

    KAUST Repository

    Kratochvil, Adam M.

    2010-05-25

    The effects of supercritical CO2 (scCO2) conditioning on high-performance cross-linked polyimide membranes is examined through gas permeation and sorption experiments. Under supercritical conditions, the cross-linked polymers do not exhibit a structural reorganization of the polymer matrix that was observed in the non-cross-linkable, free acid polymer. Pure gas permeation isotherms and mixed gas permeabilities and selectivities show the cross-linked polymers to be much more stable to scCO2 conditioning than the free acid polymer. In fact, following scCO2 conditioning, the mixed gas CO2 permeabilities of the cross-linked polymers increased while the CO2/CH4 separation factors remained relatively unchanged. This response highlights the stability and high performance of these cross-linked membranes in aggressive environments. In addition, this response reveals the potential for the preconditioning of cross-linked polymer membranes to enhance productivity without sacrificing efficiency in practical applications which, in effect, provides another tool to \\'tune\\' membrane properties for a given separation. Finally, the dual mode model accurately describes the sorption and dilation characteristics of the cross-linked polymers. The changes in the dual mode sorption model parameters before and after the scCO2 exposure also provide insights into the alterations in the different glassy samples due to the cross-linking and scCO2 exposure. © 2010 American Chemical Society.

  11. Self-assembly made durable: water-repellent materials formed by cross-linking fullerene derivatives.

    Science.gov (United States)

    Wang, Jiaobing; Shen, Yanfei; Kessel, Stefanie; Fernandes, Paulo; Yoshida, Kaname; Yagai, Shiki; Kurth, Dirk G; Möhwald, Helmuth; Nakanishi, Takashi

    2009-01-01

    Fullerene flakes: A diacetylene-functionalized fullerene derivative self-organizes into flakelike microparticles (see picture). Both the diacetylene and C(60) moieties can be effectively cross-linked, which leads to supramolecular materials with remarkable resistivity to solvent, heat, and mechanical stress. Moreover, the surface of the cross-linked flakelike objects is highly durable and water-repellent.

  12. Quantification of carboxyl groups in carbodiimide cross-linked collagen sponges

    NARCIS (Netherlands)

    Everaerts, Frank; Torrianni, Mark; Hendriks, Marc; Feijen, Jan

    2007-01-01

    Glutaraldehyde (GA) fixation of bioprosthetic tissue is a well adapted technique, with commercial products on the market for almost 40 years. Amine groups present in tissue react with GA to form different types of cross-links. An estimation of the degree of cross-linking of the tissue can be obtaine

  13. Infrared microspectroscopic determination of collagen cross-links in articular cartilage

    Science.gov (United States)

    Rieppo, Lassi; Kokkonen, Harri T.; Kulmala, Katariina A. M.; Kovanen, Vuokko; Lammi, Mikko J.; Töyräs, Juha; Saarakkala, Simo

    2017-03-01

    Collagen forms an organized network in articular cartilage to give tensile stiffness to the tissue. Due to its long half-life, collagen is susceptible to cross-links caused by advanced glycation end-products. The current standard method for determination of cross-link concentrations in tissues is the destructive high-performance liquid chromatography (HPLC). The aim of this study was to analyze the cross-link concentrations nondestructively from standard unstained histological articular cartilage sections by using Fourier transform infrared (FTIR) microspectroscopy. Half of the bovine articular cartilage samples (n=27) were treated with threose to increase the collagen cross-linking while the other half (n=27) served as a control group. Partial least squares (PLS) regression with variable selection algorithms was used to predict the cross-link concentrations from the measured average FTIR spectra of the samples, and HPLC was used as the reference method for cross-link concentrations. The correlation coefficients between the PLS regression models and the biochemical reference values were r=0.84 (p<0.001), r=0.87 (p<0.001) and r=0.92 (p<0.001) for hydroxylysyl pyridinoline (HP), lysyl pyridinoline (LP), and pentosidine (Pent) cross-links, respectively. The study demonstrated that FTIR microspectroscopy is a feasible method for investigating cross-link concentrations in articular cartilage.

  14. Glucose-mediated cross-linking of collagen in rat tendon and skin

    NARCIS (Netherlands)

    Mentink, CJAL; Hendriks, M; Levels, AAG; Wolffenbuttel, BHR

    2002-01-01

    Back-ground: Cross-linking of macromolecules like collagen plays an important role in the development of complications in diabetes and ageing. One of the underlying mechanisms of this cross-linking is the formation of advanced glycation endproducts (AGEs). Methods: In this study, we assessed the use

  15. Peroxidase-mediated cross-linking of a tyrosine-containing peptide with ferulic acid

    NARCIS (Netherlands)

    Oudgenoeg, G.; Hilhorst, R.; Piersma, S.R.; Boeriu, C.G.; Gruppen, H.; Hessing, M.; Voragen, A.G.J.; Laane, C.

    2001-01-01

    The tyrosine-containing peptide Gly-Tyr-Gly (GYG) was oxidatively cross-linked by horseradish peroxidase in the presence of hydrogen peroxide. As products, covalently coupled di- to pentamers of the peptide were identified by LC-MS. Oxidative cross-linking of ferulic acid with horseradish peroxidase

  16. Biodegradation of differently cross-linked collagen membranes: an experimental study in the rat.

    NARCIS (Netherlands)

    Rothamel, D.; Schwarz, F.; Sager, M.; Herten, M. van; Sculean, A.; Becker, J.M.

    2005-01-01

    The aim of the present study was to compare the biodegradation of differently cross-linked collagen membranes in rats. Five commercially available and three experimental membranes (VN) were included: (1) BioGide (BG) (non-cross-linked porcine type I and III collagens), (2) BioMend (BM), (3) BioMendE

  17. Investigation of anisotropic thermal transport in cross-linked polymers

    Science.gov (United States)

    Simavilla, David Nieto

    Thermal transport in lightly cross-linked polyisoprene and polybutadine subjected to uniaxial elongation is investigated experimentally. We employ two experimental techniques to assess the effect that deformation has on this class of materials. The first technique, which is based on Forced Rayleigh Scattering (FRS), allows us to measure the two independent components of the thermal diffusivity tensor as a function of deformation. These measurements along with independent measurements of the tensile stress and birefringence are used to evaluate the stress-thermal and stress-optic rules. The stress-thermal rule is found to be valid for the entire range of elongations applied. In contrast, the stress-optic rule fails for moderate to large stretch ratios. This suggests that the degree of anisotropy in thermal conductivity depends on both orientation and tension in polymer chain segments. The second technique, which is based on infrared thermography (IRT), allows us to measure anisotropy in thermal conductivity and strain induced changes in heat capacity. We validate this method measurements of anisotropic thermal conductivity by comparing them with those obtained using FRS. We find excellent agreement between the two techniques. Uncertainty in the infrared thermography method measurements is estimated to be about 2-5 %. The accuracy of the method and its potential application to non-transparent materials makes it a good alternative to extend current research on anisotropic thermal transport in polymeric materials. A second IRT application allows us to investigate the dependence of heat capacity on deformation. We find that heat capacity increases with stretch ratio in polyisoprene specimens under uniaxial extension. The deviation from the equilibrium value of heat capacity is consistent with an independent set of experiments comparing anisotropy in thermal diffusivity and conductivity employing FRS and IRT techniques. We identify finite extensibility and strain

  18. Resin bond strength to water versus ethanol-saturated human dentin pretreated with three different cross-linking agents

    Science.gov (United States)

    Venigalla, Bhuvan Shome; Jyothi, Pinnamreddy; Kamishetty, Shekhar; Reddy, Smitha; Cherukupalli, Ravi Chandra; Reddy, Depa Arun

    2016-01-01

    Context: Resin-dentin bonds are unstable owing to hydrolytic and enzymatic degradation. Several approaches such as collagen cross-linking and ethanol-wet bonding (EWB) have been developed to overcome this problem. Collagen cross-linking improves the intrinsic properties of the collagen matrix. However, it leaves a water-rich collagen matrix with incomplete resin infiltration making it susceptible to fatigue degradation. Since EWB is expected to overcome the drawbacks of water-wet bonding (WWB), a combination of collagen cross-linking with EWB was tested. Aim: The aim of this study was to compare the effect of pretreatment with different cross-linking agents such as ultraviolet A (UVA)-activated 0.1% riboflavin, 1 M carbodiimide, and 6.5 wt% proanthocyanidin on the immediate and long-term bond strengths of an etch and rinse adhesive system to water- versus ethanol-saturated dentin within clinically relevant application time periods. Settings and Design: Long-term in vitro study evaluating the microtensile bond strength of adhesive-dentin interface after different surface pretreatments. Subjects and Methods: Eighty freshly extracted human molars were prepared to expose dentin, etched with 37% phosphoric acid for 15 s rinsed, and grouped randomly. They were blot-dried and pretreated with different cross-linkers: 0.1% riboflavin for 2 min followed by UVA activation for 2 min; 1 M carbodiimide for 2 min; 6.5 wt% proanthocyanidin for 2 min and rinsed. They were then bonded with Adper Single Bond Adhesive (3M ESPE), by either WWB or EWB, followed by resin composite build-ups (Filtek Z350, 3M ESPE). Bonded specimens in each group were then sectioned and divided into two halves. Microtensile bond strength was tested in one half after 24 h and the other after 6 months storage in artificial saliva. Statistical Analysis Used: Analysis was done using SPSS version 18 software (SPSS Inc., Chicago, IL, USA). Intergroup comparison of bond strength was done using ANOVA with post hoc

  19. Assessment of protein function following cross-linking by alpha-dicarbonyls.

    Science.gov (United States)

    Miller, Antonia G; Gerrard, Juliet A

    2005-06-01

    Protein cross-linking via the Maillard reaction with alpha-dicarbonyl compounds has been the subject of intense scrutiny in the literature. We report here a study of the impact of this cross-linking on enzyme function. Protein function following glycation was examined by treating ribonuclease A with methylglyoxal, glyoxal, and diacetyl, which cross-linked the enzyme and impaired its activity. The effects of two reported Maillard reaction inhibitors, aminoguanidine and 3,5-dimethylpyrazole-1-carboxamidine, on the cross-linking reaction were assessed, with a parallel measurement of the effect on enzyme activity. The results demonstrate that preventing protein cross-linking does not necessarily preserve enzyme activity. These results cast doubt on the likely efficacy of some purported antiaging compounds in vivo.

  20. Characteristic of hyaluronic acid derivative films cross-linked by polyethylene glycol of low water content

    Institute of Scientific and Technical Information of China (English)

    Chen Jinghua; Chen Jingtao; Xu Zheng; Gu Qisheng

    2008-01-01

    Objective: To test the characteristics of byaluronic acid (HA) derivative cross-linked by polyethylene glycol films of low water content. Methods: The cross-linked HA film with 200 μm thickness was got at atmospheric pressure at 25℃ for 5 d. After dried, cross-linked films of 10 mm×10 mm were weighed and immersed in phosphate buffered saline (PBS pH 7.45) at 37℃ for 24 h. Then the solution fraction and water content were estimated. Meanwhile, cross-linked HA derivative films were immersed in phosphate buffered saline (PBS: pH 7.45) at 37℃ for determined time and then implanted subcutaneously in the back of white rats to test in vitro or in vivo degradation characteristic. Results and Conclusion: HA hydrogel cross-linked by polyethylene glycol with water content is as low as 60% and this kind of HA derivative has a slow degradation rate.

  1. [Studies of dental methacrylic resin. (Part 8) Flexural and impact adhesive strength of self-curing methacrylic resin to cross-linked polymethyl methacrylate resins (author's transl)].

    Science.gov (United States)

    Hirasawa, T; Hirabayashi, S; Harashima, I

    1981-10-01

    Heat-curing methacylic resins cross-linked with three kinds of dimethacrylates, i.e. EDMA, tri-EDMA and nona-EDMA, were prepared, and the flexural and the impact adhesive strength of the dough moulding type and the pour type self-curing methacrylic resins to them were examined. The results obtained were as follows. (1) The flexural and the impact adhesive strength of the pour type self-curing resin were higher and more stable than those of the dough moulding type one. (2) The flexural and the impact adhesive strength of self-curing resins to cross-linked adherent resins rised in order of nona-EDMA greater than tri-EDMA greater than EDMA in the range of higher concentration of cross-linking agents. This tendency was marked for the pour type resin. (3) When the dough moulding type resin was used as adhesive resin, to adherent resin cross-linked with EDMA or tri-EDMA which had relatively short chain, the respective adhesive strength of that decreased with increasing the concentration of cross-linking agent. While, to adherent resin cross-linked with nona-EDMA, which had relatively long and more flexible chain, the respective adhesive strength of the dough moulding type resin increased with increasing the concentration of cross-linking agent. (4) When the pour type resin was used as adhesive resin, to adherent resin cross-linked with EDMA or tri-EDMA, the respective adhesive strength of that showed the maximum at the concentration near 2 to 5 mole% and decreased with increasing the concentration. While, to adherent resin cross-linked with nona-EDMA, the flexural adhesive strength of the pour type resin was approximately constant without the effect of the concentration, but the impact adhesive strength of that increased with increasing the concentration. (5) The flexural adhesive strength of the dough moulding and the pour type resin under the wet condition decreased about 30 to 60% compared with under the dry condition, but the percentage of the falling for the impact

  2. Disuccinimidyl suberate cross-linked hemoglobin as a novel red blood cell substitute

    Institute of Scientific and Technical Information of China (English)

    LU; Xiuling; ZHENG; Chunyang; XU; Yuhong; SU; Zhiguo

    2005-01-01

    Disuccinimidyl suberate (DSS) intramolecularly cross-linked hemoglobin (Hb) was developed as a novel red blood cell substitute. A multi-angle laser light scattering detector coupled with size exclusion HPLC was applied to determine the molecular weight of the modified Hb. SDS-PAGE was also used as a complement. It was proved that 83.8% of the product was intramolecularly cross-linked Hb with weight-average molecular weights (Mw) of 67.5 kD, 12% was dimeric Hb with Mw of 146.6 kD, and 4.2% was trimeric Hb with Mw of 306.4 kD. The tetramer structure of the cross-linked Hb was stable as shown in size-exclusion chromatography using a mobile phase containing 1 mol/L MgCl2. Analysis by LC-MS demonstrated that the reaction of DSS with Hb mainly took place between the twoα subunits within a Hb molecule, resulting in stabilization of the tetramer structure. However, the cross-linking was not site-specific. The P50 of the cross-linked Hb decreased from 21.8 mmHg to 14.3 mmHg, and the Hill coefficient decreased from 2.22 to 1.41. Result of isoelectric focusing showed that the pI of DSS cross-linked Hb was in the range of 4.6-5.2, similar to that of serum albumin. The safety of DSS cross-linked Hb was favored by animal tests on rats and guinea pigs. Exchange transfusion experiment with DSS cross-linked Hb using rats as a model indicated no pressor effect or other significant side effects. The characteristics and properties of DSS cross-linked Hb were also compared with that of diaspirin cross-linked Hb reported in the literature.

  3. Corneal changes following collagen cross linking and simultaneous topography guided photoablation with collagen cross linking for keratoconus

    Directory of Open Access Journals (Sweden)

    Prema Padmanabhan

    2014-01-01

    Full Text Available Purpose: To compare the outcome of Collagen cross-linking (CXL with that following topography-guided customized ablation treatment (T-CAT with simultaneous CXL in eyes with progressive keratoconus. Materials and Methods: This was a prospective, non-randomized single centre study of 66 eyes with progressive keratoconus. Of these, 40 eyes underwent CXL and 26 eyes underwent T-CAT + CXL. The refractive, topographic, tomographic and aberrometric changes measured at baseline, 1, 3 and 6 months post-operatively were compared between both groups. Results: After a mean follow-up of 7.7 ± 1.3 months, the mean retinoscopic cylinder decreased by 1.02 ± 3.16 D in the CXL group ( P = 0.1 and 2.87 ± 3.22 D in the T-CAT + CXL group ( P = 0.04. The Best corrected visual acuity increased by 2 lines or more in 10% of eyes in the CXL group and in 23.3% of eyes in the T-CAT + CXL group. The mean steepest-K reduced by 0.40 ± 3.71 D ( P = 0.77 in the CXL group and by 2.91 ± 2.01D ( P = 0.03 in the T-CAT + CXL group. The sag factor and surface asymmetry index showed no significant change in the CXL group but reduced by 3.59 ± 5.94 D ( P = 0.01 and 0.72 ± 1.18 ( P = 0.02 respectively in the T-CAT + CXL group. There was a significant increase in the highest posterior corneal elevation in both groups (9.57 ± 14.93 μ in the CXL group and 7.85 ± 9.25 μ in the T-CAT + CXL group, P ≤ 0.001 for both. There was significantly greater reduction of mean coma ( P < 0.001 and mean higher-order aberrations ( P = 0.01 following T-CAT + CXL compared to CXL. Conclusions: CAT + CXL is an effective approach to confer biomechanical stability and to improve the corneal contour in eyes with keratoconus and results in better refractive, topographic and aberrometric outcomes than CXL alone.

  4. In vitro and in vivo characteristics of core–shell type nanogel particles: Optimization of core cross-linking density and surface poly(ethylene glycol) density in PEGylated nanogels

    OpenAIRE

    Tamura, Masato; Ichinohe, Satoshi; Tamura, Atsushi; Ikeda, Yutaka; Nagasaki, Yukio

    2011-01-01

    The biocompatibility and body distribution of PEGylated polyamine nanogels composed of chemically cross-linked poly(2-N,N-(diethylamino)ethyl methacrylate) (PEAMA) gel cores surrounded by poly(ethylene glycol) (PEG) chains were investigated to evaluate their feasibility as drug nanocarriers for systemic administration. PEGylated nanogels with different cross-linking densities (1, 2, and 5 mol.%) were prepared to evaluate their biocompatibilities by in vitro cytotoxicity assay, hemolysis assay...

  5. Superamphiphobic surfaces constructed by cross-linked hollow SiO2 spheres

    Science.gov (United States)

    Cui, Weihao; Wang, Tao; Yan, Aili; Wang, Sheng

    2017-04-01

    By using stringed carbon spheres as template material, a series of hierarchical 3D cross-linked SiO2 coated carbon spheres and hollow SiO2 spheres were fabricated, and spray-coated on glass slides, followed by the fluorination treatment with per-fluorotrichlorosilane. The surface characterization and surface wettability data indicated that hollow SiO2 spheres spray-coated surfaces showed better superhydrophobicity and superoleophobcity properties than the corresponding solid C@SiO2 coated surface. This study further demonstrated that superamphiphobicity depends on two critical factors, namely a cavity- and spot-rich hierarchical structure and the size and shape of overhangs. Moreover, the optimal conditions for the preparation of hollow SiO2 coated glass slide were identified after a systematic investigation of various concentrations of the carbon precursor and tetraethylorthosilicate. It was found that when 0.10 g carbon spheres prepared from 1.0 M carbon precursor were used as the template and 20 mg/mL tetraethylorthosilicate was used as silica precursor, the hollow SiO2 coated glass slide exhibited the best superamphiphobic performance, with the highest contact angles and lowest sliding angles for various liquids, such as water, olive oil, n-hexadecane and n-dodecane.

  6. Characterization of receptor proteins using affinity cross-linking with biotinylated ligands.

    Science.gov (United States)

    Shinya, Tomonori; Osada, Tomohiko; Desaki, Yoshitake; Hatamoto, Masahiro; Yamanaka, Yuko; Hirano, Hisashi; Takai, Ryota; Che, Fang-Sik; Kaku, Hanae; Shibuya, Naoto

    2010-02-01

    The plant genome encodes a wide range of receptor-like proteins but the function of most of these proteins is unknown. We propose the use of affinity cross-linking of biotinylated ligands for a ligand-based survey of the corresponding receptor molecules. Biotinylated ligands not only enable the analysis of receptor-ligand interactions without the use of radioactive compounds but also the isolation and identification of receptor molecules by a simple affinity trapping method. We successfully applied this method for the characterization, isolation and identification of the chitin elicitor binding protein (CEBiP). A biocytin hydrazide conjugate of N-acetylchitooctaose (GN8-Bio) was synthesized and used for the detection of CEBiP in the plasma or microsomal membrane preparations from rice and carrot cells. Binding characteristics of CEBiP analyzed by inhibition studies were in good agreement with the previous results obtained with the use of a radiolabeled ligand. The biotin-tagged CEBiP could be purified by avidin affinity chromatography and identified by LC-MALDI-MS/MS after tryptic digestion. We also used this method to detect OsFLS2, a rice receptor-like kinase for the perception of the peptide elicitor flg22, in membrane preparations from rice cells overexpressing OsFLS2. This work demonstrates the applicability of this method to the purification and identification of plant receptor proteins.

  7. Chemistry and physical properties of melt-processed and solution-cross-linked corn zein.

    Science.gov (United States)

    Sessa, David J; Mohamed, Abdellatif; Byars, Jeffrey A

    2008-08-27

    Corn zein was cross-linked with glutaraldehyde (GDA) using glacial acetic acid (HAc) as catalyst. The objectives are to evaluate the swelling characteristics of GDA cross-linked zein gels in water, ethanol, and their combinations. Similar formulations, upon solvent evaporation, form films. The mechanical properties of the films are compared to compression molded tensile bars from GDA melt-processed zein as a second objective. Chemistry of the cross-linking reaction was based on the aldehyde binding characteristics defined by use of fluorescence spectroscopy; sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) to demonstrate the cross-linking reaction; FTIR to observe absorption differences of the cross-linked product; differential scanning calorimetry, dynamic mechanical analysis and thermogravimetric analysis to assess thermal properties; and the use of Instron Universal Testing Machine to evaluate mechanical properties. A reaction mechanism for acid catalyzed GDA cross-linking of zein is proposed. Thermal and mechanical properties of tensile bars cut from either film or formed by compression molding were similar, where both showed increased tensile strengths, ductility and stiffness when compared with unmodified controls. Samples that were reacted with 8% GDA by weight based on weight of zein from either process retained their integrity when tensile bars from each were subjected to boiling water for 10 min or soaking in either water or HAc for 24 h. The melt-processed, cross-linked zein is a more environmentally friendly method that would eliminate the need for HAc recovery.

  8. Understanding chemical reactivity for homo- and heterobifunctional protein cross-linking agents.

    Science.gov (United States)

    Chen, Fan; Nielsen, Simone; Zenobi, Renato

    2013-07-01

    Chemical cross-linking, combined with mass spectrometry, has been applied to map three-dimensional protein structures and protein-protein interactions. Proper choice of the cross-linking agent, including its reactive groups and spacer arm length, is of great importance. However, studies to understand the details of reactivity of the chemical cross-linkers with proteins are quite sparse. In this study, we investigated chemical cross-linking from the aspects of the protein structures and the cross-linking reagents involved, by using two structurally well-known proteins, glyceraldehyde 3-phosohate dehydrogenase and ribonuclease S. Chemical cross-linking reactivity was compared using a series of homo- and hetero-bifunctional cross-linkers, including bis(sulfosuccinimidyl) suberate, dissuccinimidyl suberate, bis(succinimidyl) penta (ethylene glycol), bis(succinimidyl) nona (ethylene glycol), m-maleimidobenzoyl-N-hydroxysulfosuccinimide ester, 2-pyridyldithiol-tetraoxaoctatriacontane-N-hydrosuccinimide and succinimidyl-[(N-maleimidopropionamido)-tetracosaethyleneglycol]ester. The protein structure itself, especially the distances between target amino acid residues, was found to be a determining factor for the cross-linking efficiency. Moreover, the reactive groups of the chemical cross-linker also play an important role; a higher cross-linking reaction efficiency was found for maleimides compared to 2-pyrimidyldithiols. The reaction between maleimides and sulfhydryl groups is more favorable than that between N-hydroxysuccinimide esters and amine groups, although cysteine residues are less abundant in proteins compared to lysine residues. Copyright © 2013 John Wiley & Sons, Ltd.

  9. Novel antimicrobial superporous cross-linked chitosan/pyromellitimide benzoyl thiourea hydrogels.

    Science.gov (United States)

    Mohamed, Nadia A; Abd El-Ghany, Nahed A; Fahmy, Mona M

    2016-01-01

    In this work, chitosan (CS) was cross-linked with different amounts of pyromellitimide benzoyl thiourea moieties. The structure of the cross-linked CS was confirmed by elemental analyses, FTIR and (1)H- NMR spectroscopy. The cross-linking process proceeds via reacting of the amino groups of CS with the isothiocyanate groups of the N,N'-bis [4-(isothiocyanate carbonyl)phenyl] pyromellitimide cross-linker. The amount of the cross-linker was varied with respect to CS to produce four new pyromellitimide benzoyl thiourea cross-linked CS (PIBTU-CS) hydrogels designated as PIBTU-CS-1, PIBTU-CS-2, PIBTU-CS-3, and PIBTU-CS-4 of increasing cross-linking degree percent of 11, 22, 44 and 88%, respectively. The scanning electron microscopy observation indicates the extremely porous structure of the hydrogels. XRD results showed that the crystallinity of CS was decreased upon cross-linking. The four hydrogels exhibit a higher antibacterial activity on Bacillus subtilis and Streptococcus pneumoniae as Gram positive bacteria and against Escherichia coli as Gram negative bacteria and higher antifungal activity on Aspergillus fumigatus, Syncephalastrum racemosum and Geotricum candidum than that of the parent CS as shown from their higher inhibition zone diameters and their lower MIC values. The swell ability of the hydrogel as well as their antimicrobial activity increased with increasing cross-linking density.

  10. Novel cross linked guar gum-g-poly(acrylate) porous superabsorbent hydrogels: Characterization and swelling behaviour in different environments.

    Science.gov (United States)

    Chandrika, Ksv Poorna; Singh, Anupama; Rathore, Abhishek; Kumar, Anil

    2016-09-20

    A new series of eco-friendly cross linked guar gum-g-poly(acrylate) porous superabsorbent hydrogels was prepared by in situ grafting polymerization and cross-linking on to a natural guar gum employing N,N-methylene bis acrylamide as cross linker. Morphological and structural characterization of the prepared hydrogels (SPHs) done by Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and solid state C(13) NMR spectroscopy confirmed formation of porous grafted and crosslinked hydrogel structure. Increase in cross linker concentration in the feed mass exhibited decrease in porosity and increase in density of the hydrogels. Swelling of an optimized hydrogel (SPH) in response to external stimuli namely, salt solutions, fertilizer solutions, temperature, and pH exhibited high swelling ratios in various environments. Swelling rate of the SPH was faster than the corresponding nonporous superabsorbent hydrogel. The prepared hydrogels can serve as excellent carriers of pesticides, fertilizers and agriculturally important microbes. Biocontrol formulations based on a representative SPH exhibited excellent shelf-life characteristics and bioefficacy against phytopathogenic fungus Pythium aphanidermatum.

  11. Grafted, cross-linked carbon black as a double-layer capacitor electrode material

    Energy Technology Data Exchange (ETDEWEB)

    Richner, R.; Mueller, S.; Wokaun, A.

    2001-03-01

    Isocyanate prepolymers readily react with oxidic functional groups on carbon black. On carbon black grafted with diisocyanates, reactive isocyanate groups are available for cross-linking to a polyurethane system. This cross-linked carbon black was considered as a new active material for electrochemical electrodes. Active material for electric double-layer capacitor electrodes was produced which had values of specific capacitance of up to 200 F/g. Cross-linking efficiencies of up to 58 % of the polymers utilised were achieved. (author)

  12. Characterization of solid UV cross-linked PEGDA for biological applications

    KAUST Repository

    Castro, David

    2013-10-20

    This paper reports on solid UV cross-linked Poly(ethylene)-glycol-diacrylate (PEGDA) as a material for microfluidic devices for biological applications. We have evaluated biocompatibility of PEGDA through two separate means: 1) by examining cell viability and attachment on cross-linked PEGDA surfaces for cell culture applications, and 2) by determining if cross-linked PEGDA inhibits the polymerase chain reaction (PCR) processes for on-chip PCR. Through these studies a correlation has been found between degree of curing and cell viability, attachment, as well as on PCR outcome.

  13. Permanent Set of Cross-Linking Networks: Comparison of Theory with Molecular Dynamics Simulations

    DEFF Research Database (Denmark)

    Rottach, Dana R.; Curro, John G.; Budzien, Joanne

    2006-01-01

    The permanent set of cross-linking networks is studied by molecular dynamics. The uniaxial stress for a bead-spring polymer network is investigated as a function of strain and cross-link density history, where cross-links are introduced in unstrained and strained networks. The permanent set...... is found from the strain of the network after it returns to the state-of-ease where the stress is zero. The permanent set simulations are compared with theory using the independent network hypothesis, together with the various theoretical rubber elasticity theories: affine, phantom, constrained junction...

  14. A genetic anomaly of oriented collagen biosynthesis and cross-linking: Keratoconus.

    Science.gov (United States)

    Bourges, J L; Robert, A M; Robert, L

    2015-02-01

    Oriented collagen biosynthesis is one of the major mechanisms involved in tissue and organ formation during development. Corneal biogenesis is one example. Defects in this process lead to anomalies in tissue structure and function. The transparency of cornea and its achievement are a good example as well as its pathological modifications. Keratoconus is one example of this type of pathologies, involving also inappropriate cross-linking of collagen fibers. Among the tentatives to correct this anomaly, the riboflavin-potentiated UV-cross-linking (CXL) of keratoconus corneas appears clinically satisfactory, although none of the experiments and clinical results published prove effective cross-linking. The published results are reviewed in this article.

  15. Permanent Set of Cross-Linking Networks: Comparison of Theory with Molecular Dynamics Simulations

    DEFF Research Database (Denmark)

    Rottach, Dana R.; Curro, John G.; Budzien, Joanne;

    2006-01-01

    is found from the strain of the network after it returns to the state-of-ease where the stress is zero. The permanent set simulations are compared with theory using the independent network hypothesis, together with the various theoretical rubber elasticity theories: affine, phantom, constrained junction......The permanent set of cross-linking networks is studied by molecular dynamics. The uniaxial stress for a bead-spring polymer network is investigated as a function of strain and cross-link density history, where cross-links are introduced in unstrained and strained networks. The permanent set...

  16. Properties of cassava cross-linked carboxymethylated starch(Ⅰ)%木薯交联羧甲基淀粉的性质研究(Ⅰ)

    Institute of Scientific and Technical Information of China (English)

    谭义秋; 黄祖强; 农克良

    2013-01-01

    采用搅拌球磨机对木薯淀粉进行机械活化,以活化60 min的木薯淀粉为原料,环氧氯丙烷为交联剂,一氯乙酸钠为醚化剂制备交联羧甲基淀粉,对交联羧甲基淀粉的溶解度,糊的透明度、冻融稳定性、抗老化、抗酸、抗剪切等性质进行研究.结果表明,相对于交联淀粉,交联羧甲基淀粉的溶解度增大、糊的透明度增大;相对于羧甲基淀粉,交联羧甲基淀粉的溶解度减小,糊的透明度降低;相对于交联淀粉和羧甲基淀粉,交联羧甲基淀粉糊的冻融稳定性、抗老化、抗酸和抗剪切能力增强.%The cross-linked carboxymethylated starch was prepared by cassava starch, mechanically activated for 60 min by a stirring-type ball mill, as a starting material, epichlorohydrin as cross-linked agent, and sodium chloroacetate as etherifying a-gent. The properties of the cross-linked carboxymethylated starch, such as solubility, transparency, freeze-thaw stability, anti-retrogradation ability, anti-acid ability and anti-shearing ability, were studied. The results showed that solubility and transparency of the cross-linked carboxymethylated starch increased compared to the cross-linked starch; solubility and transparency of the cross-linked carboxymethylated starch decreased compared to carboxymethylated starch; and the freeze-thaw stability, anti-retrogradation ability, anti-acid ability, and anti-shearing ability of the cross-linked carboxymethylated starch were enhanced compared to the cross-linked starch and carboxymethylated starch.

  17. Synthesis Technology of Octenyl Succinic Acid Cross - Link Starch Esters%辛烯基琥珀酸交联淀粉酯合成工艺研究

    Institute of Scientific and Technical Information of China (English)

    石海信; 谢新玲; 张友全; 童张法

    2009-01-01

    以木薯淀粉为原料,用环氧氯丙烷作交联剂,辛烯基琥珀酸酐作酯化剂,采用湿法工艺合成辛烯基琥珀酸交联淀粉酯.探讨了淀粉乳浓度、反应温度、反应时间、pH和沉降积对辛烯基琥珀酸交联淀粉酯取代度的影响,确定制备辛烯基琥珀酸交联淀粉酯的最佳工艺参数为:淀粉乳浓度35%,酯化pH 8.0,酯化温度35℃,酯化时间3 h.交联淀粉的沉降积对酯化取代度影响较小,在生产中可根据最终产品的用途选用合适沉降积的交联淀粉进行酯化复合变性.复合变性淀粉符合食品行业标准,可以在食品工业中应用.扫描电镜对其结构进行观察显示淀粉中受侵蚀颗粒增多,颗粒表面的小凹痕数量增加.%Octenyl succinic acid cross - link starch esters were prepared by wet process with cassava starch as raw material, epichlorohydrin as cross - link agent and octenyl succinic anhydride as esterifying agent. The effects of starch slurry concentration, reaction temperature, reaction time, pH and sediment volume on the substitution degree of octenyl succinic acid cross - link starch esters were studied. Results; The optimal conditions for preparing octenyl succinic acid cross -link starch esters are starch slurry concentration 35% , esterification pH 8.0, esterification temperature 35 ℃ and esterification time 3 h. The sediment volume of cross - link starch has little effect on the substitution degree. Thus, a proper sediment volume can be determined according to the usage of final octenyl succinic acid cross - link starch esters. The produced octenyl succinic acid cross - link starch esters are identified safe to be used in food industry. The result of scanning electron microscope observation shows that the number of dents and splits in the granule surface of the prepared starch increases.

  18. Mass spectrometric analysis of a UV-cross-linked protein-DNA complex: tryptophans 54 and 88 of E. coli SSB cross-link to DNA

    DEFF Research Database (Denmark)

    Steen, H; Petersen, J; Mann, M

    2001-01-01

    of two different peptide-DNA heteroconjugates was accomplished by matrix-assisted laser desorption/ionization mass spectrometry and allowed assignment of tryptophan-54 and tryptophan-88 as candidate cross-linked residues. Sequencing of those peptide-DNA heteroconjugates by nanoelectrospray quadrupole...

  19. Tissue-specific effects of aldose reductase inhibition on fluorescence and cross-linking of extracellular matrix in chronic galactosemia. Relationship to pentosidine cross-links.

    Science.gov (United States)

    Richard, S; Tamas, C; Sell, D R; Monnier, V M

    1991-08-01

    Chronic experimental hyperglycemia mediated by galactose has been shown to induce browning and cross-linking of rat tail tendon collagen that could be duplicated in vitro by nonenzymatic galactosylation. To investigate the nature of these changes, Sprague-Dawley rats were placed on a 33% galactose diet without and with sorbinil for 6 and 12 mo. Collagen-linked fluorescence and pentosidine cross-links increased with age and galactosemia in tail tendons (P less than 0.001) and skin but were essentially unresponsive to aldose reductase inhibition (ARI). In contrast, tendon breaking time in urea, a likely parameter of cross-linking, was markedly improved (P less than 0.001) by ARI. Fluorescence that was inhibited by sorbinil treatment was increased in pepsin and proteinase K digest of aortic tissue from galactosemic rats (P less than 0.001), but impaired enzymatic digestibility was not observed. Systolic blood pressure as potential consequence of aortic stiffening was not increased in galactosemia. These data suggest that fluorescence in skin and tendon might be in part due to advanced glycosylation and pentosidine formation because these were not decreased by ARI. However, they also suggest that nonfluorescent cross-links may also be forming because, in contrast to fluorescence, tail tendon breaking time was partly corrected by ARI. Thus, it appears that extracellular matrix changes in chronic galactosemia are complex, being partly attributable to advanced glycosylation and partly to polyol-pathway activation.

  20. Inverted bulk-heterojunction solar cell with cross-linked hole-blocking layer

    Science.gov (United States)

    Udum, Yasemin; Denk, Patrick; Adam, Getachew; Apaydin, Dogukan H.; Nevosad, Andreas; Teichert, Christian; S. White, Matthew.; S. Sariciftci, Niyazi.; Scharber, Markus C.

    2014-01-01

    We have developed a hole-blocking layer for bulk-heterojunction solar cells based on cross-linked polyethylenimine (PEI). We tested five different ether-based cross-linkers and found that all of them give comparable solar cell efficiencies. The initial idea that a cross-linked layer is more solvent resistant compared to a pristine PEI layer could not be confirmed. With and without cross-linking, the PEI layer sticks very well to the surface of the indium–tin–oxide electrode and cannot be removed by solvents used to process PEI or common organic semiconductors. The cross-linked PEI hole-blocking layer functions for multiple donor–acceptor blends. We found that using cross-linkers improves the reproducibility of the device fabrication process. PMID:24817837

  1. Stabilized sulfonated aromatic polymers by in situ solvothermal cross-linking

    Directory of Open Access Journals (Sweden)

    Maria Luisa eDi Vona

    2014-10-01

    Full Text Available The cross-link reaction via sulfone bridges of sulfonated polyetheretherketone (SPEEK by thermal treatment at 180 °C in presence of dimethylsulfoxide (DMSO is discussed. The modifications of properties subsequent to the cross-linking are presented. The mechanical strength as well as the hydrolytic stability increased with the thermal treatment time, i.e., with the degree of cross-linking. The proton conductivity was determined as function of temperature, IEC, degree of cross-linking and hydration number. The memory effect, which is the membrane ability to remember the water uptake reached at high temperature also at lower temperature, is exploited in order to achieve high values of conductivity. Membranes swelled at 110 °C can reach a conductivity of 0.14 S/cm at 80°C with a hydration number ( of 73.

  2. An Investigation on Rheology of Peroxide Cross-linking of Low Density Polyethylene

    DEFF Research Database (Denmark)

    Ghasemi, Ismaeil; Rasmussen, Henrik K.; Szabo, Peter

    2005-01-01

    One of the most important post-reactor modifications of polyethylene is cross-linking. It improves some properties of polyethylene such as environmental stress cracking resistance, chemical and abrasion resistance, and service temperature. In this study, the effect of peroxide cross-linking on th......One of the most important post-reactor modifications of polyethylene is cross-linking. It improves some properties of polyethylene such as environmental stress cracking resistance, chemical and abrasion resistance, and service temperature. In this study, the effect of peroxide cross......-linking on the rheological behaviour of low density polyethylene was investigated by using a combination of creep test and differential scanning calorimeter (DSC) in isotherm condition. The used peroxide was di-cumyl peroxide and its concentration was 2 wt%. The experiments were carried out at 150,160, and 170 degrees C...

  3. PROSPECTS OF HIGH-CURRENT ELECTRON BEAMS APPLICATION TO RADIATION POLYETHYLENE CROSS-LINKING

    Directory of Open Access Journals (Sweden)

    A.G. Gurin

    2013-09-01

    Full Text Available A possibility of applying a pulse-periodic high-current induction electron accelerators to radiation polyethylene cross-linking is considered in the article. A comparative analysis with other devices used for irradiation is made.

  4. Molecular Dynamics Simulations of Polymer Networks Undergoing Sequential Cross-Linking and Scission Reactions

    DEFF Research Database (Denmark)

    Rottach, Dana R.; Curro, John G.; Budzien, Joanne;

    2007-01-01

    The effects of sequential cross-linking and scission of polymer networks formed in two states of strain are investigated using molecular dynamics simulations. Two-stage networks are studied in which a network formed in the unstrained state (stage 1) undergoes additional cross-linking in a uniaxia......The effects of sequential cross-linking and scission of polymer networks formed in two states of strain are investigated using molecular dynamics simulations. Two-stage networks are studied in which a network formed in the unstrained state (stage 1) undergoes additional cross...... good agreement with the predictions of Flory and Fricker. It was found that the fractional stress reduction upon removal of the first-stage cross-links could be accurately calculated from the slip tube model of Rubinstein and Panyukov modified to use the theoretical transfer functions of Fricker.  ...

  5. Comparative study of PBI Cross Linked Utilizing Agents of Varying Steric Configurations

    DEFF Research Database (Denmark)

    Kirkebcek, Andreas; Aili, David; Li, Qingfeng;

    2016-01-01

    The high thermal and chemical stability of poly[2,2'-(m-phenylene)-5,5' bibenzimidazole] (PBI) accounts for its wise spread use in high temperature polymer electrolyte membrane fuel cells (HT- PEMFC). By doping the membrane with phosphoric acid (PA) ionic conductivity is obtained. Thus conductivity...... ionic or covalent cross linking. When considering such, little attention is devoted to explore the effect of the sterical configuration of the cross linking agent. In this contribution three different cross linking agents are utilized to evaluate how these affects final membrane properties....... is dependent on the amount of PA present within the membrane. However mechanical properties are reduced are significantly reduced due to the plasticizing effect shown by PA [1]. This effect is due to PBI chain displacement. This effect can be lessened by use of cross linking [2-4]. This can be obtained using...

  6. CrossWork: Software-assisted identification of cross-linked peptides

    DEFF Research Database (Denmark)

    Rasmussen, Morten; Refsgaard, Jan; Peng, Li;

    2011-01-01

    The increased interest in chemical cross-linking for probing protein structure and interaction has led to a large increase in literature describing new cross-linkers and search programs. However, this has not led to a corresponding increase in the analysis of large and complex proteins. A major...... obstacle is that the new cross-linkers are either not readily available and/or have a low reactivity. In combination with aging search programs that are slow and have low sensitivity, or new search programs that are described but not released, these efforts do little to advance the field of cross......-linking. Here we present a method pipeline for chemical cross-linking, using two standard cross-linkers, BS3 and BS2G, combined with our freely available CrossWork search program. By this approach we generate cross-link data sufficient to derive structural information for large and complex proteins. Cross...

  7. A Review of Collagen Cross-Linking in Cornea and Sclera

    Directory of Open Access Journals (Sweden)

    Xiao Zhang

    2015-01-01

    Full Text Available Riboflavin/UVA cross-linking is a technique introduced in the past decades for the treatment of keratoconus, keratectasia, and infectious keratitis. Its efficacy and safety have been investigated with clinical and laboratory studies since its first clinical application by Wollensak for the treatment of keratoconus. Although its complications are encountered during clinical practice, such as infection inducing risk, minimal invasion merits a further investigation on its future application in clinical practice. Recently, collagen cross-linking in sclera shows a promising prospect. In present study, we summarized the representative studies describing the clinical and laboratory application of collagen cross-linking published in past decades and provided our opinion on the positive and negative results of cross-linking in the treatment of ophthalmic disorders.

  8. New insights into the pros and cons of cross-linking decellularized bioartificial organs.

    Science.gov (United States)

    Hussein, Kamal H; Park, Kyung-Mee; Lee, Yun-Suk; Woo, Jae-Seok; Kang, Byung-Jae; Choi, Ki-Young; Kang, Kyung-Sun; Woo, Heung-Myong

    2017-01-25

    ABSTRACTDecellularization is an attractive method for scaffold designing in regenerative medicine. The resulting extracellular matrix (ECM) consists of structural proteins such as collagen and elastin, growth factors, and glycosaminoglycans, which can direct site-appropriate remodeling after in vivo implantation. Mainly, collagen and elastin of ECM are exposed to the enzymatic biodegradation in the host. To control the biodegradation process, treatment of decellularized tissue by a cross-linking agent is required. Cross-linking also reduces antigenicity and increases the storage properties. Cross-linkers should be nontoxic, with the ability to preserve the ECM components, especially glycosaminoglycans and associated growth factors for retention of scaffold bioactivity. In this review, we describe the different cross-linking agents and methods of evaluation of cross-linking efficiency.

  9. Plasticizer migration from cross-linked flexible PVC. 1. Effects on tribology

    Science.gov (United States)

    Pannico, M.; Persico, P.; Ambrogi, V.; Carfagna, C.

    2010-06-01

    Utilization of soft PVC is restricted by plasticizer migration that can affect material properties, as well as its toxicity. Modifying the chemical structure of PVC is one of the most effective tool to reduce the diffusion of plasticizer. In this work, a soft cross-linked PVC was obtained using a difunctional amine, namely isophoron diamine (IPDA) as the cross-linking agent. The gel content (wt %) was evaluated by weighting the insoluble portion obtained through solvent extraction technique. Thermogravimetric analysis (TGA) revealed that cross-linking reactions promote thermal degradation phenomena in the polymer matrix. Tribological properties of soft uncross-linked, cross-linked and rigid PVC were determined. Soft formulations were held in contact for 32 days with rigid PVC sheets. Plasticizer migration towards the interface causes an increase of dynamic friction compared to that of the reference rigid PVC.

  10. New techniques to improve classical corneal collagen cross-linking treatment

    Institute of Scientific and Technical Information of China (English)

    Li Na; Peng Xiujun; Fan Zhengjun; Xia Yu; Wu Tengfei

    2014-01-01

    Objective The aim of this review is to comprehensively and unbiasedly summarize the improvements in the techniques for classical corneal collagen cross-linking (CXL) by covering the reasons for this improvement,measure,and effect to approach the future direction of the CXL.Data sources All articles used in this review were mainly retrieved from the PubMed database.Study selection Original articles and reviews were selected if they were related to the improvement in the technique of classical CXL.Data were mainly extracted from 94 articles,which are listed in the reference section of this review.Results This innovative research involves every step such as instrument preparation,epithelial management,riboflavin instillation,and UVA irradiation.These clinical and experimental results seem promising.Conclusions CXL treatment is the only recent promising method for preventing the progress of keratoconus.The limitations and potential complications that accompany classical CXL such as corneal thickness limitations,ultraviolet-A (UVA) light injury,and the impact of de-epithelialization encourage people to research new improvements in techniques.While this research needs to be further investigated,we hope our review can help related researchers and patients.

  11. Single- and double-ion type cross-linked polysiloxane solid electrolytes for lithium cells

    Science.gov (United States)

    Tsutsumi, Hiromori; Yamamoto, Masahiro; Morita, Masayuki; Matsuda, Yoshiharu; Nakamura, Takashi; Asai, Hiroyuki

    Polymeric solid electrolytes, that have poly(dimethylsiloxane) (PMS) backbone and cross-linked network, were applied to a rechargeable lithium battery system. Single- (PMS-Li) and double-ion type (PMS-LiClO 4) electrolytes were prepared from the same prepolymers. Lithium electrode in the both electrolytes showed reversible stripping and deposition of lithium. Intercalation and deintercalation processes of lithium ion between lithium-manganese composite oxide (Li xMnO 2) electrode and the electrolytes were also confirmed by cyclic voltammetry, however, peak current decreased with several cycles in both cases. The model cell, Li/PMS-Li/Li xMnO 2 cell had 1.4 mA h g -1 (per 1 g of active material, current density: 3.77 μA cm -2), and the Li/PMS-LiClO 4/Li xMnO 2 cell had 1.6 mA h g -1 (current density: 75.3 μA cm -2).

  12. Single- and double-ion type cross-linked polysiloxane solid electrolytes for lithium cells

    Energy Technology Data Exchange (ETDEWEB)

    Tsutsumi, Hiromori; Yamamoto, Masahiro; Morita, Masayuki; Matsuda, Yoshiharu (Dept. of Applied Chemistry and Chemical Engineering, Faculty of Engineering, Yamaguchi Univ., Ube (Japan)); Nakamura, Takashi; Asai, Hiroyuki (Dow Corning Toray Silicone Co. Ltd., Ichihara (Japan))

    1993-01-19

    Polymeric solid electrolytes, that have poly(dimethylsiloxane) (PMS) backbone and cross-linked network, were applied to a rechargeable lithium battery system. Single- (PMS-Li) and double-ion type (PMS-LiClO[sub 4]) electrolytes were prepared from the same prepolymers. Lithium electrode in the both electrolytes showed reversible stripping and deposition of lithium. Intercalation and deintercalation processes of lithium ion between lithium-manganese composite oxide (Li[sub x]MnO[sub 2]) electrode and the electrolytes were also confirmed by cyclic voltammetry, however, peak current decreased with several cycles in both cases. The model cell, Li/PMS-Li/Li[sub x]MnO[sub 2] cell had 1.4 mA h g[sup -1] (per 1 g of active material, current density: 3.77 [mu]A cm[sup -2]), and the Li/PMS-LiClO[sub 4]/Li[sub x]MnO[sub 2] cell had 1.6 mA h g[sup -1] (current density: 75.3 [mu]A cm[sup -2]). (orig.).

  13. Synthesis, Characterization and Surface Properties of Cross-linked Polyurethane Dispersion Modified by Organosiloxane

    Institute of Scientific and Technical Information of China (English)

    高明志; 许戈文

    2006-01-01

    A series of cross-linked polyether-polyester polyurethane dispersions modified with organosiloxane were prepared based on hydroxyl-terminated polydimethylsiloxane (HTPS) as hydrophobic component and 3-aminopropyl-triethoxysilane (APTS) as cross-linker as well as a bridge between polyurethane (PU) and polysiloxane (PSIL). It was discovered that polydimethylsiloxane segments were incorporated into PU chains chemically and organosiloxane was preferentially oriented toward the surface layer of the film by making a comparison of attenuated total reflection (ATR) spectra between the copolymer and the blend of PU and PSIL, which was further confirmed by investigation of electron spectroscopy for chemical analysis (ESCA). The relationships between surface properties of the film formed from polyurethane dispersion and organosiloxane content were also studied. The results showed that water contact angle of the film increased with the increase of organosiloxane content. Interestingly, it was also found that water contact angle of PUS film increased firstly and then decreased when film-forming temperature varied from 25℃ to 55℃.

  14. Properties of collagen gels cross-linked by N-hydroxysuccinimide activated adipic acid deriviate.

    Science.gov (United States)

    Duan, Lian; Liu, Wentao; Tian, Zhenhua; Li, Conghu; Li, Guoying

    2014-08-01

    In order to improve the properties of collagen gel, N-hydroxysuccinimide activated adipic acid derivative (NHS-AA) was introduced into the formation of collagen fibrils. NHS-AA with different [NHS-AA]/[NH2] ratios (0.1-1.5, calculated by [ester group] of NHS-AA and [NH2] of lysine and hydroxylysine residues of collagen) was added after, simultaneously with or before the formation of collagen fibrils (abbreviated CAF, CSF and CBF, respectively) to obtain different collagen gels. With the same dose of NHS-AA, the cross-linking degree for CAF was lower than those for CSF and CBF. The formation of collagen fibrils was restrained by NHS-AA for CSF and CBF while that for CAF was unaffected. When the dose of NHS-AA increased from 0.1 to 1.5, the water contents of CSF and CBF increased while that of CAF had no obvious change. With lower dose of NHS-AA (0.1), CAF possessed higher value of G' (87.3Pa) and the best thermal stability (47.6°C). As the ratio of [NHS-AA]/[NH2] increased to 1.5, CSF had the maximum value of G' (288.8Pa) and CAF had the best thermal stability (52.9°C). These results showed collagen gels with different properties could be prepared by adding NHS-AA with different adding sequence and dose.

  15. Graphene oxide-reinforced biodegradable genipin-cross-linked chitosan fluorescent biocomposite film and its cytocompatibility

    Directory of Open Access Journals (Sweden)

    Li JH

    2013-09-01

    Full Text Available Jianhua Li,1 Na Ren1, Jichuan Qiu,1 Xiaoning Mou,2 Hong Liu1,21Center of Bio and Micro/Nano Functional Materials, State Key Laboratory of Crystal Materials, Shandong University, Jinan, People's Republic of China; 2Beijing Institute of Nanoenergy and Nanosystems, Chinese Academy of Sciences, Beijing, People's Republic of ChinaAbstract: A genipin-cross-linked chitosan/graphene oxide (GCS/GO composite film was prepared using a solution casting method. Fourier transform infrared (FTIR and ultraviolet-visible (UV-Vis spectroscopy of the composite films showed that the interactions between the CS and oxygen-containing groups of GO resulted in good dispersion of the GO sheets in the CS network. The addition of GO decreased the expansion ratio of the composite films in physiological conditions and increased the resistance to degradation by lysozymes in vitro. As well, the tensile strength values of the GCS/GO films were significantly increased with the increasing load of GO. Moreover, the GCS/GO composite film also maintained the intrinsic fluorescence of GCS. The in vitro cell study results revealed that the composite films were suitable for the proliferation and adhesion of mouse preosteoblast (MC3T3-E1 cells. The GCS/GO biocomposite films might have a potential use in tissue engineering, bioimaging, and drug delivery.Keywords: chitosan film degradation, fluorescence, cytocompatibility

  16. Tripolyphosphate Cross-Linked Macromolecular Composites for the Growth of Shape- and Size-Controlled Apatites

    Directory of Open Access Journals (Sweden)

    Fwu-Long Mi

    2012-12-01

    Full Text Available Bioactive composites that enable the formation of calcium phosphates have received increased attention over the last decade, in the development of osteoconductive biomaterials for orthopaedic applications. In this work, tripolyphosphate (TPP-cross-linked chitosan/gelatin composites (TPP-CG were prepared for the growth of shape- and size-controlled calcium phosphates on/in the composites. The mineralization pattern of the composites, after soaking in the Ca(OH2 aqueous solution, clearly demonstrated oriented, needle-like nanocrystallites of calcium phosphates in the matrix with especially high Ca/P molar ratio (3.98 as detected by energy dispersive X-ray spectroscopy (EDX analysis. Subsequent to mineralization in a simulated body fluid (SBF, the mineralized composites showed micro-scaled spherical aggregates deposited on the surface and granule-like nanocrystallites grew in the matrix. The Ca/P molar ratio (1.72 and X-ray diffraction pattern of the nanocrystallites grown in the composites were similar to those of hydroxyapatite (HAp. Osteoblastic differentiation of ROS cells cultured on the mineralized composites allowed an enhanced expression of the chosen osteogenic marker (alkaline phosphatase, ALPase. These results indicated that the composites mineralized with micro- and nano-scaled calcium phosphates with various structural features make them attractive for bone tissue engineering applications.

  17. Comparison of Riboflavin/Ultraviolet-A Cross-Linking in Porcine, Rabbit, and Human Sclera

    Directory of Open Access Journals (Sweden)

    Yali Zhang

    2014-01-01

    Full Text Available Purpose. To compare the biomechanical properties of porcine, rabbit, and human sclera before and after riboflavin/ultraviolet-A (UVA collagen cross-linking (CXL. Methods. Eight rabbits, 8 porcine eyeballs, and 8 human eyeballs were included. One rabbit eye and half of each bisected human and porcine eyeball were treated with riboflavin/UVA CXL. Untreated fellow rabbit eyes and eyeball halves served as controls. A 10 mm × 20 mm scleral band was harvested from each specimen. From this band, two 3.5 mm × 15.0 mm strips were prepared for biomechanical testing. The biomechanical parameters were ultimate stress, stress and Young’s modulus. Results. Values of stress, and Young’s modulus showed that human sclera was 4 times stiffer than porcine sclera and 3 times stiffer than rabbit sclera. In rabbit sclera, both the stress and Young’s modulus were significantly increased by CXL (P0.05. Conclusions. Human sclera has higher biomechanical stiffness than porcine and rabbit sclera. With the same irradiation dose, riboflavin/UVA CXL increases the biomechanical stiffness of rabbit sclera but not porcine or human sclera.

  18. Comparison of hydrazone heterobifunctional cross-linking agents for reversible conjugation of thiol-containing chemistry.

    Science.gov (United States)

    Christie, R James; Anderson, Diana J; Grainger, David W

    2010-10-20

    Reversible covalent conjugation chemistries that allow site- and condition-specific coupling and uncoupling reactions are attractive components in nanotechnologies, bioconjugation methods, imaging, and drug delivery systems. Here, we compare three heterobifunctional cross-linkers, containing both thiol- and amine-reactive chemistries, to form pH-labile hydrazones with hydrazide derivatives of the known and often published water-soluble polymer, poly[N-(2-hydroxypropyl methacrylamide)] (pHPMA), while subsequently coupling thiol-containing molecules to the cross-linker via maleimide addition. Two novel cross-linkers were prepared from the popular heterobifunctional cross-linking agent, succinimidyl-4-(N-maleimidomethyl) cyclohexane-1-carboxylate (SMCC), modified to contain either terminal aldehyde groups (i.e., 1-(N-3-propanal)-4-(N-maleimidomethyl) cyclohexane carboxamide, PMCA) or methylketone groups (i.e., 1-(N-3-butanone)-4-(N-maleimidomethyl) cyclohexane carboxamide, BMCA). A third cross-linking agent was the commercially available N-4-acetylphenyl maleimide (APM). PMCA and BMCA exhibited excellent reactivity toward hydrazide-derivatized pHPMA with essentially complete hydrazone conjugation to polymer reactive sites, while APM coupled only ∼60% of available reactive sites on the polymer despite a 3-fold molar excess relative to polymer hydrazide groups. All polymer hydrazone conjugates bearing these bifunctional agents were then further reacted with thiol-modified tetramethylrhodamine dye, confirming cross-linker maleimide reactivity after initial hydrazone polymer conjugation. Incubation of dye-labeled polymer conjugates in phosphate buffered saline at 37 °C showed that hydrazone coupling resulting from APM exhibited the greatest difference in stability between pH 7.4 and 5.0, with hydrolysis and dye release increased at pH 5.0 over a 24 h incubation period. Polymer conjugates bearing hydrazones formed from cross-linker BMCA exhibited intermediate stability

  19. The Release Behavior and Kinetic Evaluation of Tramadol HCl from Chemically Cross Linked Ter Polymeric Hydrogels

    Directory of Open Access Journals (Sweden)

    Muhammad A Malana

    2013-01-01

    Full Text Available Background and the purpose of the study: Hydrogels, being stimuli responsive are considered to be effective for targeted and sustained drug delivery. The main purpose for this work was to study the release behavior and kinetic evaluation of Tramadol HCl from chemically cross linked ter polymeric hydrogels.MethodsTer-polymers of methacrylate, vinyl acetate and acrylic acid cross linked with ethylene glycol dimethacrylate (EGDMA were prepared by free radical polymerization. The drug release rates, dynamic swelling behavior and pH sensitivity of hydrogels ranging in composition from 1-10 mol % EGDMA were studied. Tramadol HCl was used as model drug substance. The release behavior was investigated at pH 8 where all formulations exhibited non-Fickian diffusion mechanism.Results and major conclusion: Absorbency was found to be more than 99% indicating good drug loading capability of these hydrogels towards the selected drug substance. Formulations designed with increasing amounts of EGDMA had a decreased equilibrium media content as well as media penetrating velocity and thus exhibited a slower drug release rate. Fitting of release data to different kinetic models indicate that the kinetic order shifts from the first to zero order as the concentration of drug was increased in the medium, showing gradual independency of drug release towards its concentration. Formulations with low drug content showed best fitness with Higuchi model whereas those with higher concentration of drug followed Hixson-Crowell model with better correlation values indicating that the drug release from these formulations depends more on change in surface area and diameter of tablets than that on concentration of the drug. Release exponent (n derived from Korse-Meyer Peppas equation implied that the release of Tramadol HCl from these formulations was generally non-Fickian (n>0.5>1 showing swelling controlled mechanism. The mechanical strength and controlled release capability of

  20. The release behavior and kinetic evaluation of tramadol HCl from chemically cross linked Ter polymeric hydrogels

    Directory of Open Access Journals (Sweden)

    Malana Muhammad A

    2013-01-01

    Full Text Available Abstract Background and the purpose of the study Hydrogels, being stimuli responsive are considered to be effective for targeted and sustained drug delivery. The main purpose for this work was to study the release behavior and kinetic evaluation of Tramadol HCl from chemically cross linked ter polymeric hydrogels. Methods Ter-polymers of methacrylate, vinyl acetate and acrylic acid cross linked with ethylene glycol dimethacrylate (EGDMA were prepared by free radical polymerization. The drug release rates, dynamic swelling behavior and pH sensitivity of hydrogels ranging in composition from 1-10 mol% EGDMA were studied. Tramadol HCl was used as model drug substance. The release behavior was investigated at pH 8 where all formulations exhibited non-Fickian diffusion mechanism. Results and major conclusion Absorbency was found to be more than 99% indicating good drug loading capability of these hydrogels towards the selected drug substance. Formulations designed with increasing amounts of EGDMA had a decreased equilibrium media content as well as media penetrating velocity and thus exhibited a slower drug release rate. Fitting of release data to different kinetic models indicate that the kinetic order shifts from the first to zero order as the concentration of drug was increased in the medium, showing gradual independency of drug release towards its concentration. Formulations with low drug content showed best fitness with Higuchi model whereas those with higher concentration of drug followed Hixson-Crowell model with better correlation values indicating that the drug release from these formulations depends more on change in surface area and diameter of tablets than that on concentration of the drug. Release exponent (n derived from Korse-Meyer Peppas equation implied that the release of Tramadol HCl from these formulations was generally non-Fickian (n > 0.5 > 1 showing swelling controlled mechanism. The mechanical strength and controlled

  1. Long-Term Sustained Release from a Biodegradable Photo-Cross-Linked Network for Intraocular Corticosteroid Delivery.

    Science.gov (United States)

    Amsden, Brian G; Marecak, Dale

    2016-09-06

    Intravitreal sustained delivery of corticosteroids such as dexamethasone is an effective means of treating a number of ocular diseases, including diabetic retinopathy, uveitis, and age-related or diabetic macular edema. There are currently marketed devices for this purpose, yet only one, Ozurdex, is degradable. In vitro release of dexamethasone from the Ozurdex device is limited to approximately 30 days, however. It was the objective of this study to examine the potential for prolonged and sustained release of a corticosteroid in vitro from a degradable polymer prepared from terminally acrylated star co- and ter-prepolymers composed of d,l-lactide, ε-caprolactone, and trimethylene carbonate co-photo-cross-linked with poly(ethylene glycol) diacrylate. Through manipulation of the network polymer glass transition temperature and degradation rate, a sustained release of triamcinolone was achieved, with an estimated release duration greater than twice that of the Ozurdex system. Moreover, a period of nearly constant release was obtained using a network prepared from 5000 Da star-poly(trimethylene carbonate-co-d,l-lactide) triacrylate (3:1 trimethylene carbonate:d,l-lactide) co-cross-linked with 700 Da poly(ethylene glycol diacrylate). These formulations show promise as implantable, intravitreal corticosteroid delivery devices.

  2. Effects of cross-linking, capsule wall thickness, and compound hydrophobicity on aroma release from complex coacervate microcapsules.

    Science.gov (United States)

    Leclercq, Segolene; Milo, Christian; Reineccius, Gary A

    2009-02-25

    Microcapsules were produced by complex coacervation with a gelatin-gum acacia wall and medium-chain-triglyceride core. Dry capsules were partially rehydrated and then loaded with model aroma compounds covering a range of volatility, hydrophobicity, and molecular structure. An experimental design was prepared to evaluate the effects of cross-linking, wall/core ratio, and volatile load level on aroma release from capsules in a hot, aqueous environment. The real-time release on rehydration was measured by monitoring the headspace of a vessel containing the capsules to proton transfer reaction mass spectrometry (PTR-MS). Data collected showed no effects of cross-linking or wall/core ratio on volatile release in hot water for any of the volatiles studied. When comparing real-time release of the prepared coacervates to a spray-dried equivalent, there was no difference in the release from hot water but the release was slower when coacervates were added to ambient-temperature water. We found volatile release to be primarily determined by compound partition coefficients (oil/water and water/air) and temperature.

  3. Design of a stable and methanol resistant membrane with cross-linked multilayered polyelectrolyte complexes for direct methanol fuel cells

    Science.gov (United States)

    Wang, Jing; Zhao, Chengji; Lin, Haidan; Zhang, Gang; Zhang, Yang; Ni, Jing; Ma, Wenjia; Na, Hui

    Sulfonated poly (arylene ether ketone) bearing carboxyl groups (SPAEK-C) membranes have been prepared as proton exchange membranes for applications in direct methanol fuel cells (DMFCs). Multilayered polyelectrolyte complexes (PECs) which applied as methanol barrier agents are prepared by alternate deposition of the oppositely charged amino-containing poly (ether ether ketone) (Am-PEEK) and the highly sulfonated SPAEK-C via a layer-by-layer method. The cross-linked PEC (c-PEC) is derived from a simple heat-induced cross-linking reaction between Am-PEEK and SPAEK-C. Fourier transform infrared spectroscopy confirms that Am-PEEK and SPAEK-C are assembled successfully in the multilayers. The morphology of the membranes is studied by scanning electron microscopy, which shows the presence of the thin layers coated on the SPAEK-C membrane. After PEC and c-PEC modification, the methanol permeability decreases obviously when compared to that of the pristine membrane. Notably, improved proton conductivities are obtained for the PEC modified membranes in comparison with the pristine membrane. Moreover, the selectivity of these modified membranes is one order of magnitude higher than that of Nafion 117. The thermal stability, oxidative stability, water uptake and swelling of PEC and c-PEC modified membranes are also investigated.

  4. Spray-by-spray in situ cross-linking alginate hydrogels delivering a tea tree oil microemulsion.

    Science.gov (United States)

    Catanzano, O; Straccia, M C; Miro, A; Ungaro, F; Romano, I; Mazzarella, G; Santagata, G; Quaglia, F; Laurienzo, P; Malinconico, M

    2015-01-23

    In this paper we propose an in situ forming ionically cross-linked alginate (Alg) hydrogel delivering a Tea Tree Oil microemulsion (MeTTO) and potentially useful as an advanced dressing for infected wounds. Alg hydrogels were prepared by a spray-by-spray deposition method with the aim to minimize the discomforts during application. From pseudoternary phase diagrams, it was found that proper combination of TTO, water, polysorbate 80 and ethanol gave stable spherical MeTTO with good antimicrobial activity. On this basis, MeTTO at 20% TTO was selected for further inclusion in an Alg hydrogel prepared by alternating sprays of Alg/MeTTO and calcium chloride solutions. Homogeneous dispersion of MeTTO inside cross-linked Alg was assessed by different macroscopic and microscopic methods demonstrating the superior propensity of MeTTO to be integrated in the water-based hydrogel as compared to TTO. Antimicrobial effect of Alg/MeTTO hydrogels on Escherichia Coli strains was remarkable, highlighting the potential of the system as bioactive wound dressing.

  5. Synthesis, characterization and cytocompatibility of a poly(diol-tricarballylate) visible light photo-cross-linked biodegradable elastomer.

    Science.gov (United States)

    Shaker, Mohamed A; Doré, Jules J E; Younes, Husam M

    2010-01-01

    The synthesis, characterization and in vitro cytocompatibility of a new family of photo-cross-linked amorphous poly(diol-tricarballylate) (PDT) biodegradable elastomeric polyesters are reported. The synthesis was based on the polycondensation reaction between tricarballylic acid and alkylene diols, followed by acrylation. The prepared and acrylated poly(diol-tricarballylate) (APDT) was characterized by means of FT-IR, (1)H-NMR, GPC and DSC. Liquid-to-solid photo-curing was carried out by exposing the APDT to visible light in the presence of camphorquinone as a photoinitiator. The thermal properties, mechanical characteristics, sol content, long-term in vitro degradation and cytocompatibility of the prepared PDT elastomers were also reported. The mechanical and degradation properties of this new photocurable elastomer can be precisely controlled by varying the density of acrylate moieties in the matrix of the polymer, and through changes in the pre-polymer chain length. The use of visible light cross-linking, possibility of solventless drug loading, controllable mechanical properties and cytocompatibility of these new elastomers make them excellent candidates for use in controlled implantable drug-delivery systems of protein drugs and other biomedical applications.

  6. The level of cross-linking and the structure of anisotropic magnetorheological elastomers

    Energy Technology Data Exchange (ETDEWEB)

    Borin, Dmitry, E-mail: dmitry.borin@tu-dresden.de [Institute of Fluid Mechanics, Technische Universitaet Dresden, Dresden 01062 (Germany); Guenther, David [Institute of Fluid Mechanics, Technische Universitaet Dresden, Dresden 01062 (Germany); Hintze, Christian; Heinrich, Gert [Leibniz Institute of Polymer Research, Dresden 01069 (Germany); Odenbach, Stefan [Institute of Fluid Mechanics, Technische Universitaet Dresden, Dresden 01062 (Germany)

    2012-10-15

    The influence of the concentration of the magnetic powder on the level of cross-linking of magnetorheological elastomers (MREs) has been studied. Afterwards the structural characterisation of manufactured MREs has been performed by using non-destructive method, specifically the computed tomography. The correlation between internal structures of MREs and the developing of its cross-linking level during the curing was found. It was shown that changes in the concentration of the powder significantly affect morphologies of the sample.

  7. Sorption of substituted indoles on highly cross-linked polystyrene from water-acetonitrile solutions

    Science.gov (United States)

    Shafigulin, R. V.; Myakishev, A. A.; Il'Ina, E. A.; Il'in, M. M.; Davankov, V. A.; Bulanova, A. V.

    2011-07-01

    The sorption of first synthesized indole derivatives by highly cross-linked polystyrenes from water-acetonitrile solutions was studied by high-performance liquid chromatography. The retention factors and differences in the Gibbs energy of adsorption from infinite diluted solutions were calculated, and the applicability of the Snyder-Soczewinski and Scott-Kucera models for describing the chromatographic retention of sorbates on a polymer network of highly cross-linked polystyrene was shown.

  8. Analysis of glycation induced protein cross-linking inhibitory effects of some antidiabetic plants and spices

    OpenAIRE

    Perera, Handunge Kumudu Irani; Handuwalage, Charith Sandaruwan

    2015-01-01

    Background Protein cross-linking which occurs towards the latter part of protein glycation is implicated in the development of chronic diabetic complications. Glycation induced protein cross-linking inhibitory effects of nine antidiabetic plants and three spices were evaluated in this study using a novel, simple, electrophoresis based method. Methods Methanol extracts of thirteen plants including nine antidiabetic plants and three spices were used. Lysozyme and fructose were incubated at 37 °...

  9. Computational exploration of polymer nanocomposite mechanical property modification via cross-linking topology

    Energy Technology Data Exchange (ETDEWEB)

    Lacevic, N; Gee, R; Saab, A; Maxwell, R

    2008-04-24

    Molecular dynamics simulations have been performed in order to study the effects of nanoscale filler cross-linking topologies and loading levels on the mechanical properties of a model elastomeric nanocomposite. The model system considered here is constructed from octa-functional polyhedral oligomeric silsesquioxane (POSS) dispersed in a poly(dimethylsiloxane) (PDMS) matrix. Shear moduli, G, have been computed for pure and for filled and unfilled PDMS as a function of cross-linking density, POSS fill loading level, and polymer network topology. The results reported here show that G increases as the cross-linking (covalent bonds formed between the POSS and the PDMS network) density increases. Further, G is found to have a strong dependence on cross-linking topology. The increase in shear modulus, G, for POSS filled PDMS is significantly higher than that for unfilled PDMS cross-linked with standard molecular species, suggesting an enhanced reinforcement mechanism for POSS. In contrast, in blended systems (POSS/PDMS mixture with no cross-linking) G was not observed to significantly increase with POSS loading. Finally, we find intriguing differences in the structural arrangement of bond strains between the cross-linked and the blended systems. In the unfilled PDMS the distribution of highly strained bonds appears to be random, while in the POSS filled system, the strained bonds form a net-like distribution that spans the network. Such a distribution may form a structural network 'holding' the composite together and resulting in increases in G compared to an unfilled, cross-linked system. These results are of importance for engineering of new POSS-based multifunctional materials with tailor-made mechanical properties.

  10. Computational exploration of polymer nanocomposite mechanical property modification via cross-linking topology.

    Science.gov (United States)

    Lacevic, Naida; Gee, Richard H; Saab, Andrew; Maxwell, Robert

    2008-09-28

    Molecular dynamics simulations have been performed in order to study the effects of nanoscale filler cross-linking topologies and loading levels on the mechanical properties of a model elastomeric nanocomposite. The model system considered here is constructed from octafunctional polyhedral oligomeric silsesquioxane (POSS) dispersed in a poly(dimethylsiloxane) (PDMS) matrix. Shear moduli, G, have been computed for pure and for filled and unfilled PDMS as a function of cross-linking density, POSS fill loading level, and polymer network topology. The results reported here show that G increases as the cross-linking (covalent bonds formed between the POSS and the PDMS network) density increases. Further, G is found to have a strong dependence on cross-linking topology. The increase in shear modulus, G, for POSS filled PDMS is significantly higher than that for unfilled PDMS cross-linked with standard molecular species, suggesting an enhanced reinforcement mechanism for POSS. In contrast, in blended systems (POSS/PDMS mixture with no cross-linking) G was not observed to significantly increase with POSS loading. Finally, we find intriguing differences in the structural arrangement of bond strains between the cross-linked and the blended systems. In the unfilled PDMS the distribution of highly strained bonds appears to be random, while in the POSS filled system, the strained bonds form a netlike distribution that spans the network. Such a distribution may form a structural network "holding" the composite together and resulting in increases in G compared to an unfilled, cross-linked system. These results are of importance for engineering of new POSS-based multifunctional materials with tailor-made mechanical properties.

  11. Porphyrin-induced photodynamic cross-linking of hepatic heme-binding proteins.

    Science.gov (United States)

    Vincent, S H; Holeman, B; Cully, B C; Muller-Eberhard, U

    1986-01-27

    Three types of hepatic proteins, a heme-binding Z protein, a mixture of the glutathione S-transferases and a cytochrome P450 isozyme, were shown to be susceptible to photodynamic cross-linking and loss in antigenicity by naturally occurring porphyrins. At 50 microM, uroporphyrin caused the most and protoporphyrin the least photodecomposition. Hemopexin, a specific serum heme carrier, was photodecomposed but no cross-linking was detected. Heme and scavengers of singlet oxygen partially prevented protein photodecomposition.

  12. Off-resonance-robust velocity-selective magnetization preparation for non-contrast-enhanced peripheral MR angiography.

    Science.gov (United States)

    Shin, Taehoon; Hu, Bob S; Nishimura, Dwight G

    2013-11-01

    To develop a new velocity-selective (VS) excitation pulse sequence which is robust to field inhomogeneity, and demonstrate its application to non-contrast-enhanced peripheral MR angiography (MRA). The off-resonance-robust VS saturation pulse is designed by incorporating 180° refocusing pulses into the k-space-based reference design and tailoring sequence parameters in a velocity region of interest. The VS saturation pulse is used as magnetization preparation for non-contrast-enhanced peripheral MRA to suppress background tissues but not arterial blood based on their velocities. Non-contrast-enhanced peripheral MRA using the proposed VS preparation was tested in healthy volunteers and a patient with arterial stenosis. Calf angiograms obtained using the new VS preparation show more uniform background suppression than the reference VS preparation, as demonstrated by larger mean values and smaller standard deviations of artery-to-vein and artery-to-muscle contrast-to-noise ratios (71.0 ± 11.4 and 75.3 ± 12.1 versus 61.7 ± 22.7 and 58.5 ± 27.8). Two-station peripheral MRA using the new VS preparation identifies stenosis of the femoral and popliteal arteries in the patient, as validated by digital subtraction angiography. Non-contrast-enhanced MRA using the new VS magnetization preparation can reliably provide high angiographic contrast in the lower extremities with significantly improved immunity to field inhomogeneity. Copyright © 2012 Wiley Periodicals, Inc.

  13. Characterization of the receptor for endothelial cell growth factor (ECGF) by affinity cross-linking

    Energy Technology Data Exchange (ETDEWEB)

    Friesel, R.; Burgess, W.H.; Mehlman, T.; Maciag, T.

    1986-05-01

    The authors have demonstrated high affinity receptors for ECGF on endothelial cells by covalent cross-linking of (/sup 125/I)-ECGF with disuccinimidyl suberate and observe a single chain cross-linked polypeptide species with an apparent M/sub r/ of 170K. The M/sub r/ 170K species represents (/sup 125/I)-ECGF bound to its receptor since (i) excess unlabeled ECGF inhibits the cross-linking of (/sup 125/I)-ECGF, (ii) labeling of the M/sub r/170K species does not take place in the absence of cross-linker, (iii) cells previously shown to be refractory to ECGF and lack ECGF receptors do not yield a cross-linked species, (iv) the cross-linked species can be immunoprecipitated with anti-ECGF antibodies, and (v) preincubation of cells with ECGF at 37/sup 0/C significantly reduces cross-linking while incubation at 4/sup 0/C does not. These data demonstrate that ECGF induced cell proliferation occurs through the occupancy of a specific cell surface polypeptide receptor with an apparent M/sub r/ of 150K, and suggests that internalization of the receptor-ligand complex may be relevant to ECGF-induced signal transduction.

  14. Directing the oligomer size distribution of peroxidase-mediated cross-linked bovine alpha-lactalbumin.

    Science.gov (United States)

    Heijnis, Walter H; Wierenga, Peter A; van Berkel, Willem J H; Gruppen, Harry

    2010-05-12

    Enzymatic protein cross-linking is a powerful tool to change protein functionality. For optimal functionality in gel formation, the size of the cross-linked proteins needs to be controlled, prior to heating. In the current study, we addressed the optimization of the horseradish peroxidase-mediated cross-linking of calcium-depleted bovine alpha-lactalbumin. To characterize the formed products, the molecular weight distribution of the cross-linked protein was determined by size exclusion chromatography. At low ionic strength, more dimers of alpha-lactalbumin are formed than at high ionic strength, while the same conversion of monomers is observed. Similarly, at pH 5.9 more higher oligomers are formed than at pH 6.8. This is proposed to be caused by local changes in apo alpha-lactalbumin conformation as indicated by circular dichroism spectroscopy. A gradual supply of hydrogen peroxide improves the yield of cross-linked products and increases the proportion of higher oligomers. In conclusion, this study shows that the size distribution of peroxidase-mediated cross-linked alpha-lactalbumin can be directed toward the protein oligomers desired.

  15. Cross-linking proteins by laccase-catalyzed oxidation: importance relative to other modifications.

    Science.gov (United States)

    Steffensen, Charlotte L; Andersen, Mogens L; Degn, Peter E; Nielsen, Jacob H

    2008-12-24

    Laccase-catalyzed oxidation was able to induce intermolecular cross-links in beta-lactoglobulin, and ferulic acid-mediated laccase-catalyzed oxidation was able to induce intermolecular cross-links in alpha-casein, whereas transglutaminase cross-linked only alpha-casein. In addition, different patterns of laccase-induced oxidative modifications were detected, including dityrosine formation, formation of fluorescent tryptophan oxidation products, and carbonyls derived from histidine, tryptophan, and methionine. Laccase-catalyzed oxidation as well as transglutaminase induced only minor changes in surface tension of the proteins, and the changes could not be correlated to protein cross-linking. The presence of ferulic acid was found to influence the effect of laccase, allowing laccase to form irreducible intermolecular cross-links in beta-lactoglobulin and resulting in proteins exercising higher surface tensions due to cross-linking as well as other oxidative modifications. The outcome of using ferulic acid-mediated laccase-catalyzed oxidation to modify the functional properties of proteinaceous food components or other biosystems is expected to be highly dependent on the protein composition, resulting in different changes of the functional properties.

  16. Smooth muscle cell phenotype modulation and contraction on native and cross-linked polyelectrolyte multilayers.

    Science.gov (United States)

    Moussallem, Maroun D; Olenych, Scott G; Scott, Shannon L; Keller, Thomas C S; Schlenoff, Joseph B

    2009-11-09

    Smooth muscle cells convert between a motile, proliferative "synthetic" phenotype and a sessile, "contractile" phenotype. The ability to manipulate the phenotype of aortic smooth muscle cells with thin biocompatible polyelectrolyte multilayers (PEMUs) with common surface chemical characteristics but varying stiffness was investigated. The stiffness of (PAH/PAA) PEMUs was varied by heating to form covalent amide bond cross-links between the layers. Atomic force microscopy (AFM) showed that cross-linked PEMUs were thinner than those that were not cross-linked. AFM nanoindentation demonstrated that the Young's modulus ranged from 6 MPa for hydrated native PEMUs to more than 8 GPa for maximally cross-linked PEMUs. Rat aortic A7r5 smooth muscle cells cultured on native PEMUs exhibited morphology and motility of synthetic cells and expression of the synthetic phenotype markers vimentin, tropomyosin 4, and nonmuscle myosin heavy chain IIB (nmMHCIIB). In comparison, cells cultured on maximally cross-linked PEMUs exhibited the phenotype markers calponin, smooth muscle myosin heavy chain (smMHC), myocardin, transgelin, and smooth muscle alpha-actin (smActin) that are characteristic of the smooth muscle "contractile" phenotype. Consistent with those cells being "contractile", A7r5 cells grown on cross-linked PEMUs produced contractile force when stimulated with a Ca(2+) ionophore.

  17. Cross-linked survey analysis is an approach for separating cause and effect in survey research.

    Science.gov (United States)

    Redelmeier, Donald A; Thiruchelvam, Deva; Lustig, Andrew J

    2015-01-01

    We developed a new research approach, called cross-linked survey analysis, to explore how an acute exposure might lead to changes in survey responses. The goal was to identify associations between exposures and outcomes while reducing some ambiguities related to interpreting cause and effect in survey responses from a population-based community questionnaire. Cross-linked survey analysis differs from a cross-sectional, longitudinal, and panel survey analysis by individualizing the timeline to the unique history of each respondent. Cross-linked survey analysis, unlike a repeated-measures self-matching design, does not track changes in a repeated survey question given to the same respondent at multiple time points. Pilot data from three analyses (n = 1,177 respondents) illustrate how a cross-linked survey analysis can control for population shifts, temporal trends, and reverse causality. Accompanying graphs provide an intuitive display to readers, summarize results, and show differences in response distributions. Population-based individual-level linkages also reduce selection bias and increase statistical power compared with a single-center cross-sectional survey. Cross-linked survey analysis has limitations related to unmeasured confounding, pragmatics, survivor bias, statistical models, and the underlying artifacts in survey responses. We suggest that a cross-linked survey analysis may help in epidemiology science using survey data. Copyright © 2015 Elsevier Inc. All rights reserved.

  18. Digestibility of β-lactoglobulin following cross-linking by Trametes versicolor laccase and apple polyphenols

    Directory of Open Access Journals (Sweden)

    DRAGANA STANIĆ-VUČINIĆ

    2011-06-01

    Full Text Available β-Lactoglobulin (BLG is an important nutrient of dairy products and an important allergen in cow’s milk allergy. The aim of this study was to investigate the potential of laccase to cross-link BLG in the presence of an apple phenolic extract (APE and to characterize the obtained products for their digestibility by pepsin and pancreatin. The composition of the apple phenolics used for cross-linking was determined by liquid chromatography–electrospray ionization-mass spectrometry (LC–ESI-MS. The apple phenolic extract contained significant amounts of quercetin glycosides, catechins and chlorogenic acid. The laccase cross-linked BLG in the presence of apple phenolics. The polymerization rendered the protein insoluble in the reaction mixture. Sodium dodecyl sulfate–polyacrylamide gel electrophoresis (SDS-PAGE analysis of the cross-linking reaction mixture revealed a heterogeneous mixture of high molecular masses (cross-linked BLG, with a fraction of the BLG remaining monomeric. Enzymatic processing of BLG by laccase and apple polyphenols as mediators can decrease the biphasal pepsin–pancreatin digestibility of the monomeric and cross-linked protein, thus decreasing its nutritional value. In addition, reduced BLG digestibility can decrease its allergenic potential. Apple polyphenols can find usage in the creation of new, more functional food products, designed to prevent obesity and hypersensitivity-related disorders.

  19. Exogenous collagen cross-linking recovers tendon functional integrity in an experimental model of partial tear.

    Science.gov (United States)

    Fessel, Gion; Wernli, Jeremy; Li, Yufei; Gerber, Christian; Snedeker, Jess G

    2012-06-01

    We investigated the hypothesis that exogenous collagen cross-linking can augment intact regions of tendon to mitigate mechanical propagation of partial tears. We first screened the low toxicity collagen cross-linkers genipin, methylglyoxal and ultra-violet (UV) light for their ability to augment tendon stiffness and failure load in rat tail tendon fascicles (RTTF). We then investigated cross-linking effects in load bearing equine superficial digital flexor tendons (SDFT). Data indicated that all three cross-linking agents augmented RTTF mechanical properties but reduced native viscoelasticity. In contrast to effects observed in fascicles, methylglyoxal treatment of SDFT detrimentally affected tendon mechanical integrity, and in the case of UV did not alter tendon mechanics. As in the RTTF experiments, genipin cross-linking of SDFT resulted in increased stiffness, higher failure loads and reduced viscoelasticity. Based on this result we assessed the efficacy of genipin in arresting tendon tear propagation in cyclic loading to failure. Genipin cross-linking secondary to a mid-substance biopsy-punch significantly reduced tissue strains, increased elastic modulus and increased resistance to fatigue failure. We conclude that genipin cross-linking of injured tendons holds potential for arresting tendon tear progression, and that implications of the treatment on matrix remodeling in living tendons should now be investigated.

  20. A Comparative Study of the Characteristics of Cross-Linked, Oxidized and Dual-Modified Rice Starches

    Directory of Open Access Journals (Sweden)

    Feng-Xiang Yu

    2012-09-01

    Full Text Available Rice starch was cross-linked with epichlorohydrin (0.3%, w/w, on a dry starch basis and oxidized with sodium hypochlorite (2.5% w/w, respectively. Two dual-modified rice starch samples (oxidized cross-linked rice starch and cross-linked oxidized rice starch were obtained by the oxidation of cross-linked rice starch and the cross-linking of oxidized rice starch at the same level of reagents. The physicochemical properties of native rice starch, cross-linked rice starch and oxidized rice starch were also studied parallel with those of the two dual-modified rice starch samples using rapid visco analysis (RVA, differential scanning calorimetry (DSC, dynamic rheometry and scanning electron microscopy (SEM. It was found that the levels of cross-linking and oxidation used in this study did not cause any significant changes in the morphology of rice starch granules. Cross-linked oxidized starch showed lower swelling power (SP and solubility, and higher paste clarity in comparison with native starch. Cross-linked oxidized rice starch also had the lowest tendency of retrogradation and highest ability to resistant to shear compared with native, cross-linked, oxidized and oxidized cross-linked rice starches. These results suggest that the undesirable properties in native, cross-linked and oxidized rice starch samples could be overcome through dual-modification.

  1. Study on Synthesis of Cross Linking Starch Adhesives%交联淀粉胶粘剂的合成研究

    Institute of Scientific and Technical Information of China (English)

    章昌华; 管猛

    2012-01-01

    以乙二醛为交联剂与土豆淀粉制备了交联淀粉胶粘剂。考察了土豆淀粉浓度、乙二醛浓度、反应温度和反应时间对胶粘剂性能的影响,并采用红外光谱对树脂结构进行了表征。研究结果表明:当土豆淀粉浓度为3%、乙二醛浓度为1.2%、反应时间3h、反应温度70℃时,所制备的交联淀粉胶粘剂综合性能最佳。%Cross linking starch adhesives were prepared with potato starch and glyoxal as cross linking agent. The effects of concentration of potato starch, concentration of glyoxal, reaction temperature and reaction time on properties of the cross linking starch adhesives were investigated. In addition, the structure of cross linking starch adhesive was characterized by FTIR. The results showed that the overall performance of the synthetic adhesive was excellent under the conditions of 3% potato starch, 1.2% glyoxal, and reacted for 3h at 70℃,

  2. Cross-linked Composite Gel Polymer Electrolyte using Mesoporous Methacrylate-Functionalized SiO2 Nanoparticles for Lithium-Ion Polymer Batteries

    Science.gov (United States)

    Shin, Won-Kyung; Cho, Jinhyun; Kannan, Aravindaraj G.; Lee, Yoon-Sung; Kim, Dong-Won

    2016-05-01

    Liquid electrolytes composed of lithium salt in a mixture of organic solvents have been widely used for lithium-ion batteries. However, the high flammability of the organic solvents can lead to thermal runaway and explosions if the system is accidentally subjected to a short circuit or experiences local overheating. In this work, a cross-linked composite gel polymer electrolyte was prepared and applied to lithium-ion polymer cells as a safer and more reliable electrolyte. Mesoporous SiO2 nanoparticles containing reactive methacrylate groups as cross-linking sites were synthesized and dispersed into the fibrous polyacrylonitrile membrane. They directly reacted with gel electrolyte precursors containing tri(ethylene glycol) diacrylate, resulting in the formation of a cross-linked composite gel polymer electrolyte with high ionic conductivity and favorable interfacial characteristics. The mesoporous SiO2 particles also served as HF scavengers to reduce the HF content in the electrolyte at high temperature. As a result, the cycling performance of the lithium-ion polymer cells with cross-linked composite gel polymer electrolytes employing methacrylate-functionalized mesoporous SiO2 nanoparticles was remarkably improved at elevated temperatures.

  3. Cross-linked Composite Gel Polymer Electrolyte using Mesoporous Methacrylate-Functionalized SiO2 Nanoparticles for Lithium-Ion Polymer Batteries.

    Science.gov (United States)

    Shin, Won-Kyung; Cho, Jinhyun; Kannan, Aravindaraj G; Lee, Yoon-Sung; Kim, Dong-Won

    2016-05-18

    Liquid electrolytes composed of lithium salt in a mixture of organic solvents have been widely used for lithium-ion batteries. However, the high flammability of the organic solvents can lead to thermal runaway and explosions if the system is accidentally subjected to a short circuit or experiences local overheating. In this work, a cross-linked composite gel polymer electrolyte was prepared and applied to lithium-ion polymer cells as a safer and more reliable electrolyte. Mesoporous SiO2 nanoparticles containing reactive methacrylate groups as cross-linking sites were synthesized and dispersed into the fibrous polyacrylonitrile membrane. They directly reacted with gel electrolyte precursors containing tri(ethylene glycol) diacrylate, resulting in the formation of a cross-linked composite gel polymer electrolyte with high ionic conductivity and favorable interfacial characteristics. The mesoporous SiO2 particles also served as HF scavengers to reduce the HF content in the electrolyte at high temperature. As a result, the cycling performance of the lithium-ion polymer cells with cross-linked composite gel polymer electrolytes employing methacrylate-functionalized mesoporous SiO2 nanoparticles was remarkably improved at elevated temperatures.

  4. Cross-linked Composite Gel Polymer Electrolyte using Mesoporous Methacrylate-Functionalized SiO2 Nanoparticles for Lithium-Ion Polymer Batteries

    Science.gov (United States)

    Shin, Won-Kyung; Cho, Jinhyun; Kannan, Aravindaraj G.; Lee, Yoon-Sung; Kim, Dong-Won

    2016-01-01

    Liquid electrolytes composed of lithium salt in a mixture of organic solvents have been widely used for lithium-ion batteries. However, the high flammability of the organic solvents can lead to thermal runaway and explosions if the system is accidentally subjected to a short circuit or experiences local overheating. In this work, a cross-linked composite gel polymer electrolyte was prepared and applied to lithium-ion polymer cells as a safer and more reliable electrolyte. Mesoporous SiO2 nanoparticles containing reactive methacrylate groups as cross-linking sites were synthesized and dispersed into the fibrous polyacrylonitrile membrane. They directly reacted with gel electrolyte precursors containing tri(ethylene glycol) diacrylate, resulting in the formation of a cross-linked composite gel polymer electrolyte with high ionic conductivity and favorable interfacial characteristics. The mesoporous SiO2 particles also served as HF scavengers to reduce the HF content in the electrolyte at high temperature. As a result, the cycling performance of the lithium-ion polymer cells with cross-linked composite gel polymer electrolytes employing methacrylate-functionalized mesoporous SiO2 nanoparticles was remarkably improved at elevated temperatures. PMID:27189842

  5. Characterization and in vitro and in vivo evaluation of cross-linked chitosan films as implant for controlled release of citalopram

    Indian Academy of Sciences (India)

    Patit P Kundu; Santosh Kumar Jindal; Manish Goswami

    2013-02-01

    The aim of the present study is to develop cross-linked chitosan (CH) films that can release drug over an extended period of time and that too in a controlled manner. A solution of different percentages of CH, is prepared in 1% lactic acid, followed by addition of citalopram (CTP) and then reacted with increasing amounts of glutaraldehyde (GL) to obtain films with different cross-linking densities. Prepared films are characterized for their physical and mechanical properties. The films are then subjected to in vitro drug release studies using pH 7.4 phosphate buffer saline (PBS) as dissolution medium and cumulative amount of drug released is calculated. Kinetic analysis of drug release is performed using Power law model and Higuchi’s model.With increase in concentration of CH, water absorption capacity and mechanical strength are increased; whereas, water vapour permeability and elasticity of the films are decreased. The effect of cross-linking agent, GL, is such that with an increase in the amount of GL, water vapour permeability, water absorption capacity and elasticity of the films are decreased; whereas, mechanical strength increased to some extent and then decreased. In vitro release studies indicate that films containing 3% CH, cross-linked with 2–3% GL and films containing 4%CH, cross-linked 1%GL are able to sustain the drug release for a prolonged time along with releasing almost complete drug in a desired period. Out of these batches, films containing 3% CH, cross-linked with 2–3% GL are having sufficient strength, water vapour permeation, water absorption capacity and elongation at break for implantation purpose. The in vitro degradation studies and histopathological studies were carried out with a sample film (batch C3 as in table 1) in rabbit model. In vitro degradation study indicates that the films maintained their integrity for desired implantation. The histopathological studies under optical microscope indicates that on implanting, there is no

  6. Oxidative Cross-linking of Skimmed Milk and Its Effects on the Rheology of the Prepared Set-yoghurt%脱脂乳的氧化交联处理以及对凝固型酸奶流变学的影响

    Institute of Scientific and Technical Information of China (English)

    温研; 张英华; 赵新淮

    2011-01-01

    利用辣根过氧化物酶处理脱脂乳并制备凝固型酸奶,采用流变仪对脱脂乳和所制备的酸奶样品进行流变特性对比研究。研究结果表明:辣根过氧化物酶处理、阿魏酸的添加影响脱脂乳和酸奶样品的流变特性;脱脂乳的表观黏度和黏弹性均增加,同时,所得到的凝固型酸奶的表观黏度、触变性和黏弹性也都增加。研究结果显示,脱脂乳的辣根过氧化物酶处理可以作为一个改善凝固性酸奶流变学品质的技术手段。%Skimmed milk was treated with horseradish peroxidase or/and ferulic acid, and used to prepare setyoghurt. The rheological properties of the skimmed milk and the set-yoghurt prepared were measured with a Rheometer. The analysis results showed that treatment of skimmed milk with horseradish peroxidase or/and ferulic acid had clear influence on the rheological properties of the skimmed milk and the set-yoghurt prepared. The apparent viscosity and viscoelastic behavior of the skimmed milk were increased, meanwhile, the apparent viscosity, thixotropy and viscoelastic behavior of the prepared yoghurt samples were also enhanced. The present work indicates that horseradish peroxidase plus ferulic acid treatment of skimmed milk might be a new approach to improve the rheological properties of the set-yoghurt.

  7. Optimized RNA gel-shift and UV cross-linking assays for characterization of cytoplasmic RNA-protein interactions.

    Science.gov (United States)

    Thomson, A M; Rogers, J T; Walker, C E; Staton, J M; Leedman, P J

    1999-11-01

    Considerable interest has recently focused on defining the mechanisms involved in the regulation of gene expression at the level of mRNA stability and translational efficiency. However, the assays used to directly investigate interactions between RNA and cytoplasmic proteins have been difficult to establish, and methods are not widely available. Here, we describe a robust method for RNA electrophoretic mobility shift and UV cross-linking assays that allows rapid detection of cytoplasmic RNA-protein interactions. For added convenience to new investigators, these assays use mini-gels with an electrophoresis time of 15-20 min, enabling a high throughput of samples. The method works successfully with many different probes and cytoplasmic extracts from a variety of cell lines. Furthermore, we provide a system to optimize characterization of the RNA-protein complex and troubleshoot most assay difficulties.

  8. A dication cross-linked composite anion-exchange membrane for all-vanadium flow battery applications.

    Science.gov (United States)

    Zhang, Fengxiang; Zhang, Huamin; Qu, Chao

    2013-12-01

    We report the fabrication and properties of a high-performance, inexpensive, composite, anion-exchange membrane (AEM) for an all-vanadium flow battery (VFB) application. The AEM was fabricated by dication cross-linking without the involvement of trimethylamine, and shows well-balanced anion conductivity and robustness due to imidazolium and imidazolium-ammonium functionalities, as well as a concomitantly achieved semi-interpenetrating network structure. The VFB single cell yielded a Coulombic efficiency of 99 % and an energy efficiency of 84 % at 80 mA cm(-2) , and operated for over 900 charge/discharge cycles. This work demonstrates the combined use of several favorable AEM design rationales, such as incorporating abundant and efficient anion-exchange groups, constructing a swelling- and oxidation-resistant structure, and facile fabrication; it provides an effective way of developing high-performance, low-cost AEMs for VFB applications.

  9. Immunoadjuvant potential of cross-linked dextran microspheres mixed with chitosan nanospheres encapsulated with tetanus toxoid.

    Science.gov (United States)

    Pirouzmand, Haniyeh; Khameneh, Bahman; Tafaghodi, Mohsen

    2017-12-01

    Nasal mucosa is a desirable route for mucosal vaccine delivery. Mucosal co-administration of chitosan nanoparticles with absorption enhancers such as cross-linked dextran microspheres (CDM, Sephadex(®)) is a promising antigen delivery system. In the current study, the chitosan nanospheres loaded with tetanus toxoid (CHT:TT NPs) was prepared and characterized. The immune responses against tetanus toxoid after nasal administration of CHT:TT NPs alone or mixed with CDM were also determined. Chitosan nanospheres were prepared by ionic gelation method. Particle size, releasing profile and antigen stability were evaluated by dynamic light scattering, diffusion chamber and SDS-PAGE methods, respectively. Rabbits were nasally immunized with different formulations loaded with 40 Lf TT. After three times immunizations with 2 weeks intervals, sera IgG titres and nasal lavage sIgA titres were determined. Mean size of CHT NPs and CHT:TT NPs were 205 ± 42 nm and 432 ± 85 nm, respectively. The release profile showed that 42.4 ± 10.5% of TT was released after 30 min and reached to a steady state after 1.5 h. Stability of encapsulated TT in nanospheres was confirmed by SDS-PAGE. The antibody titres showed that CHT:TT NPs-induced antibody titres were higher than TT solution. CHT NPs mixed with CDM induced the systemic IgG and nasal lavage sIgA titres higher than intranasal administration of TT solution (p < 0.001). As the results indicated, these CHT:TT NPs when co-administered with CDM were able to induce more immune responses and have the potential to be used in mucosal immunization.

  10. Polymeric molecular sieve membranes via in situ cross-linking of non-porous polymer membrane templates

    Science.gov (United States)

    Qiao, Zhen-An; Chai, Song-Hai; Nelson, Kimberly; Bi, Zhonghe; Chen, Jihua; Mahurin, Shannon M.; Zhu, Xiang; Dai, Sheng

    2014-04-01

    High-performance polymeric membranes for gas separation are attractive for molecular-level separations in industrial-scale chemical, energyand environmental processes. Molecular sieving materials are widely regarded as the next-generation membranes to simultaneously achieve high permeability and selectivity. However, most polymeric molecular sieve membranes are based on a few solution-processable polymers such as polymers of intrinsic microporosity. Here we report an in situ cross-linking strategy for the preparation of polymeric molecular sieve membranes with hierarchical and tailorable porosity. These membranes demonstrate exceptional performance as molecular sieves with high gas permeabilities and selectivities for smaller gas molecules, such as carbon dioxide and oxygen, over larger molecules such as nitrogen. Hence, these membranes have potential for large-scale gas separations of commercial and environmental relevance. Moreover, this strategy could provide a possible alternative to ‘classical’ methods for the preparation of porous membranes and, in some cases, the only viable synthetic route towards certain membranes.

  11. Click Cross-Linking-Improved Waterborne Polymers for Environment-Friendly Coatings and Adhesives.

    Science.gov (United States)

    Hu, Jianqing; Peng, Kaimei; Guo, Jinshan; Shan, Dingying; Kim, Gloria B; Li, Qiyao; Gerhard, Ethan; Zhu, Liang; Tu, Weiping; Lv, Weizhong; Hickner, Michael A; Yang, Jian

    2016-07-13

    Waterborne polymers, including waterborne polyurethanes (WPU), polyester dispersions (PED), and polyacrylate emulsions (PAE), are employed as environmentally friendly water-based coatings and adhesives. An efficient, fast, stable, and safe cross-linking strategy is always desirable to impart waterborne polymers with improved mechanical properties and water/solvent/thermal and abrasion resistance. For the first time, click chemistry was introduced into waterborne polymer systems as a cross-linking strategy. Click cross-linking rendered waterborne polymer films with significantly improved tensile strength, hardness, adhesion strength, and water/solvent resistance compared to traditional waterborne polymer films. For example, click cross-linked WPU (WPU-click) has dramatically improved the mechanical strength (tensile strength increased from 0.43 to 6.47 MPa, and Young's modulus increased from 3 to 40 MPa), hardness (increased from 59 to 73.1 MPa), and water resistance (water absorption percentage dropped from 200% to less than 20%); click cross-linked PED (PED-click) film also possessed more than 3 times higher tensile strength (∼28 MPa) than that of normal PED (∼8 MPa). The adhesion strength of click cross-linked PAE (PAE-click) to polypropylene (PP) was also improved (from 3 to 5.5 MPa). In addition, extra click groups can be preserved after click cross-linking for further functionalization of the waterborne polymeric coatings/adhesives. In this work, we have demonstrated that click modification could serve as a convenient and powerful approach to significantly improve the performance of a variety of traditional coatings and adhesives.

  12. Cross-linked chitosan/sepiolite composite for the adsorption of methylene blue and reactive orange 16.

    Science.gov (United States)

    Marrakchi, F; Khanday, W A; Asif, M; Hameed, B H

    2016-12-01

    Cross-linked chitosan/sepiolite composite was prepared from sepiolite clay and chitosan, and was cross-linked using epichlorohydrin. Among the various weight ratio percentage of chitosan and sepiolite clay composites, CS50SP50 was selected as the best adsorbent for both methylene blue (MB) and reactive orange 16 (RO 16). At an optimum adsorbent dosage of 0.2g/100mL, the effects of initial dye concentration (25-400mg/L) and pH (3-11) on MB and RO 16 adsorption onto CS50SP50 composite were studied. Monolayer adsorption capacities of CS50SP50 composite for MB and RO 16 were 40.986mg/g and 190.965mg/g, respectively at 30°C. Freundlich, Langmuir and Temkin isotherms applied on the adsorption data for both the dyes reveal that data fitted best for Freundlich model. For both the dyes pseudo-second-order kinetics were found to describe the adsorption process better than pseudo-first-order kinetics. The adsorption capacity of CS50SP50 composite for both the dyes was found better compared to previous studies thus making it potentially low-cost adsorbent for removal of both cationic and reactive dyes. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Core Cross-Linked Multiarm Star Polymers with Aggregation-Induced Emission and Temperature Responsive Fluorescence Characteristics

    KAUST Repository

    Zhang, Zhen

    2017-05-19

    Aggregation-induced emission (AIE) active core cross-linked multiarm star polymers, carrying polystyrene (PS), polyethylene (PE), or polyethylene-b-polycaprolactone (PE-b-PCL) arms, have been synthesized through an “arm-first” strategy, by atom transfer radical copolymerization (ATRP) of a double styrene-functionalized tetraphenylethene (TPE-2St) used as a cross-linker with linear arm precursors possessing terminal ATRP initiating moieties. Polyethylene macroinitiator (PE–Br) was prepared via the polyhomologation of dimethylsulfoxonium methylide with triethylborane followed by oxidation/hydrolysis and esterification of the produced PE–OH with 2-bromoisobutyryl bromide; polyethylene-block-poly(ε-caprolactone) diblock macroinitiator was derived by combining polyhomologation with ring-opening polymerization (ROP). All synthesized star polymers showed AIE-behavior either in solution or in bulk. At high concentration in good solvents (e.g., THF, or toluene) they exhibited low photoluminescence (PL) intensity due to the inner filter effect. In sharp contrast to the small molecule TPE-2St, the star polymers were highly emissive in dilute THF solutions. This can be attributed to the cross-linked structure of poly(TPE-2St) core which restricts the intramolecular rotation and thus induces emission. In addition, the PL intensity of PE star polymers in THF(solvent)/n-hexane(nonsolvent) mixtures, due to their nearly spherical shape, increased when the temperature decreased from 55 to 5 °C with a linear response in the range 40–5 °C.

  14. An Injectable, Click-Cross-Linked Small Intestinal Submucosa Drug Depot for the Treatment of Rheumatoid Arthritis.

    Science.gov (United States)

    Kim, Kyungsook; Park, Ji Hoon; Park, Seung Hun; Lee, Hye Yun; Kim, Jae Ho; Kim, Moon Suk

    2016-12-01

    Here, a click-cross-linked small intestine submucosa (SIS) drug depot is described for the treatment of rheumatoid arthritis (RA). To the best of the knowledge, there have been no studies related to the intra-articular injection of methotrexate (Met)-loaded click-cross-linkable SIS (Met-loaded Cx-SIS) for RA treatment. As the key objective of this work, injectable formulations of tetrazine-modified SIS (TE-SIS) and transcyclooctene-modified SIS (TC-SIS) are employed as drug depots. Within a few seconds, the simple mixing of equal amounts of TE-SIS and TC-SIS suspensions forms a gelatinous click-cross-linked SIS (Cx-SIS) drug depot in vitro and in vivo. The formed Cx-SIS depot is maintained in the articular joint over an extended period, while SIS alone rapidly disappears. Injectable formulations of Met-loaded Cx-SIS and Met-loaded SIS are prepared and then injected into articular joints to form drug depots. Compared to animals treated with Met-loaded SIS, RA animals treated with Met-loaded Cx-SIS show effective RA repair, as well as extensive regeneration of chondrocytes and glycosaminoglycan deposits. Collectively, these results indicate that the Met-loaded Cx-SIS depot is successfully formed after intra-articular injection of click-cross-linkable SIS, and that this formulation induces long-lasting Met release and allows Met to act effectively in the articular joint, resulting in RA repair.

  15. Effects of Molecular Weight upon Irradiation-Cross-Linked Poly(vinyl alcohol)/Clay Aerogel Properties.

    Science.gov (United States)

    Chen, Hong-Bing; Zhao, Yan; Shen, Peng; Wang, Jun-Sheng; Huang, Wei; Schiraldi, David A

    2015-09-16

    Facile fabrication of mechanically strong poly(vinyl alcohol) (PVOH)/clay aerogel composites through a combination of increasing polymer molecular weights and gamma irradiation-cross-linking is reported herein. The aerogels produced from high polymer molecular weights exhibit significantly increased compressive moduli, similar to the effect of irradiation-induced cross-linking. The required irradiation dose for fabricating strong PVOH composite aerogels with dense microstructure decreased with increasing polymer molecular weight. Neither thermal stability nor flammability was significantly changed by altering the polymer molecular weight or by modest gamma irradiation, but they were highly dependent upon the polymer/clay ratio in the aerogel. Optimization of the mechanical, thermal, and flammability properties of these composite aerogels could therefore be obtained by using relatively low levels of polymer, with very high polymer molecular weight, or lower molecular weight coupled with moderate gamma irradiation. The facile preparation of strong, low flammability aerogels is an alternative to traditional polymer foams in applications where fire safety is important.

  16. Optimisation of the reaction conditions for the production of cross-linked starch with high resistant starch content.

    Science.gov (United States)

    Kahraman, Kevser; Koksel, Hamit; Ng, Perry K W

    2015-05-01

    The optimum reaction conditions (temperature and pH) for the preparation of cross-linked (CL) corn and wheat starches with maximum resistant starch (RS) content were investigated by using response surface methodology (RSM). According to the preliminary results, five levels were selected for reaction temperature (38-70 °C) and pH (10-12) in the main study. RS contents of the CL corn and wheat starch samples increased with increasing temperature and pH, and pH had a greater influence on RS content than had temperature. The maximum RS content (with a maximum p value of 0.4%) was obtained in wheat starch cross-linked at 38 °C and pH 12. In the case of CL corn starch, the optimum condition was 70 °C and pH 12. CL corn and wheat starch samples were also produced separately under the optimum conditions and their RS contents were 80.4% and 83.9%, respectively. These results were also in agreement with the values predicted by RSM.

  17. A STUDY OF SILICA-SUPPORTED CROSS-LINKED POLY(MALEIC ACID-CO-STYRENE)-PLATINUM COMPLEX IN THE HYDROGENATION OF p-CRESOL

    Institute of Scientific and Technical Information of China (English)

    CHEN Chunwei; WANG Xin; HUANG Meiyu; JIANG Yingyan

    1996-01-01

    A silica-supported cross-linked poly(maleic acid -co- styrene)-platinum complex (PMSPt) has been prepared and found to be active in the hydrogenation of p-cresol under mild conditions (303-323K, 1.01 × 105Pa). In this hydrogenation system water serves as a solvent and p-cresol can be converted to 4-methylcyclohexanol quantitatively via 4-methylcyclohexanone as intermediate.

  18. Effects of UV-Light and Silane Cross-Linking on the Properties of Polyethylene Cable Materials%紫外光与硅烷交联对聚乙烯电缆材料性能的影响

    Institute of Scientific and Technical Information of China (English)

    马宝红; 鲍文波; 姜国发; 高广刚

    2013-01-01

    In this paper,the cross-linking insulation cable materials based on linear low density polyethylene (LLDPE) resin was prepared by UV-light and silane cross-linking methods respectively.The effects of two kinds of cross-linking methods on properties were investigated.The experimental results demonstrated that the UV-light cross-linking method was more effective than the silane cross-linking method.The UV-light cross-linking polyethylene materials showed better properties,such as gel content,thermal contraction,ageing resistance and electric properties.%以线型低密度聚乙烯(LLDPE)为基体树脂,分别制备出紫外光交联与硅烷交联电缆用绝缘料.讨论了两种交联方法对聚乙烯绝缘材料性能的影响.结果表明:对于无色母填充的聚乙烯材料,紫外光交联后的样品在凝胶含量、热收缩、耐老化及电性能等方面均明显优于硅烷交联聚乙烯材料.

  19. Vitamin E-diffused highly cross-linked UHMWPE particles induce less osteolysis compared to highly cross-linked virgin UHMWPE particles in vivo.

    Science.gov (United States)

    Bichara, David A; Malchau, Erik; Sillesen, Nanna H; Cakmak, Selami; Nielsen, G Petur; Muratoglu, Orhun K

    2014-09-01

    Recent in vitro findings suggest that UHMWPE wear particles containing vitamin E (VE) may have reduced biologic activity and decreased osteolytic potential. We hypothesized that particles from VE-stabilized, radiation cross-linked UHMWPE would cause less osteolysis in a murine calvarial bone model when compared to virgin gamma irradiated cross-linked UHMWPE. Groups received equal amount of particulate debris overlaying the calvarium for 10 days. Calvarial bone was examined using high resolution micro-CT and histomorphometric analyses. There was a statistically significant difference between virgin (12.2%±8%) and VE-UHMWPE (3%±1.4%) groups in regards to bone resorption (P=0.005) and inflammatory fibrous tissue overlaying the calvaria (0.48 vs. 0.20, PUHMWPE particles have reduced osteolytic potential in vivo when compared to virgin UHMWPE.

  20. Protein structure prediction guided by cross-linking restraints - A systematic evaluation of the impact of the cross-linking spacer length

    CERN Document Server

    Hofmann, Tommy; Meiler, Jens; Kalkhof, Stefan

    2015-01-01

    Recent development of high-resolution mass spectrometry (MS) instruments enables chemical cross-linking (XL) to become a high-throughput method for obtaining structural information about proteins. Restraints derived from XL-MS experiments have been used successfully for structure refinement and protein-protein docking. However, one formidable question is under which circumstances XL-MS data might be sufficient to determine a protein's tertiary structure de novo? Answering this question will not only include understanding the impact of XL-MS data on sampling and scoring within a de novo protein structure prediction algorithm, it must also determine an optimal cross-linker type and length for protein structure determination. While a longer cross-linker will yield more restraints, the value of each restraint for protein structure prediction decreases as the restraint is consistent with a larger conformational space. In this study, the number of cross-links and their discriminative power was systematically analyz...

  1. Adsorption of Amido Black 10B from aqueous solutions onto Zr (IV) surface-immobilized cross-linked chitosan/bentonite composite

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lujie; Hu, Pan; Wang, Jing; Huang, Ruihua, E-mail: hrh20022002@163.com

    2016-04-30

    Graphical abstract: - Highlights: • Zr-CCB was prepared and characterized. • The adsorption of AB10B followed the Langmuir isotherm model. • The pseudo-second-order model described the kinetic behavior. - Abstract: Zr(IV) surface-immobilized cross-linked chitosan/bentonite composite was synthesized by immersing cross-linked chitosan/bentonite composite in zirconium oxychloride solution, and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, Scanning electron microscopy techniques. The adsorption of an anionic dye, Amido Black 10B, from aqueous solution by Zr(IV) loaded cross-linked chitosan/bentonite composite was investigated as a function of loading amount of Zr(IV), adsorbent dosage, pH value of initial dye solution, and ionic strength. The removal of Amido Black 10B increased with an increase in loading amount of Zr(IV) and adsorbent dosage, but decreased with an increase in pH or ionic strength. The adsorption of AB10B onto Zr(IV) loaded cross-linked chitosan/bentonite composite was favored at lower pH values and higher temperatures. The Langmuir isotherm model fitted well with the equilibrium adsorption isotherm data and the maximum monolayer adsorption capacity was 418.4 mg/g at natural pH value and 298 K. The pseudo-second-order kinetic model well described the adsorption process of Amido Black 10B onto Zr(IV) loaded cross-linked chitosan/bentonite composite. The possible mechanisms controlling Amido Black 10B adsorption included hydrogen bonding and electrostatic interactions.

  2. Enhancement of mechanical properties, microstructure, and antimicrobial activities of zein films cross-linked using succinic anhydride, eugenol, and citric Acid.

    Science.gov (United States)

    Khalil, Ashraf A; Deraz, Sahar F; Elrahman, Somia Abd; El-Fawal, Gomaa

    2015-08-18

    Zein constitutes about half of the endosperm proteins in corn. Recently, attempts have been made to utilize zein for food coatings and biodegradable materials, which require better physical properties, using chemical modification of zein. In this study, zein proteins were modified using citric acid, succinic anhydride, and eugenol as natural cross-linking agents in the wet state. The cross-linkers were added either separately or combined in increment concentrations (0.1, 0.2, 0.3, and 0.4%). The effects of those agents on the mechanical properties, microstructure, optical properties, infrared (IR) spectroscopy, and antibacterial activities of zein were investigated. The addition of cross-linking agents promoted changes in the arrangement of groups in zein film-forming particles. Regarding the film properties, incorporation of cross-linking agents into zein films prepared in ethanol resulted in two- to three-fold increases in tensile strength (TS) values. According to the Fourier-transform infrared (FTIR) spectra and Hunter parameters there were no remarkable changes in the structure and color of zein films. Transparency of zein films was decreased differentially according to the type and cross-linker concentration. The mechanical and optical properties of zein films were closely related to their microstructure. All cross-linked films showed remarkable antibacterial activities against Bacillus cereus ATCC 49064 and Salmonella enterica ATCC 25566. Food spoilage and pathogenic bacteria were affected in a film-dependent manner. Our experimental results show that even with partial cross-linking the mechanical properties and antipathogen activities of zein films were significantly improved, which would be useful for various industrial applications.

  3. Vitamin E-diffused highly cross-linked UHMWPE particles induce less osteolysis compared to highly cross-linked virgin UHMWPE particles in vivo

    DEFF Research Database (Denmark)

    Bichara, David A; Malchau, Erik; Sillesen, Nanna H

    2014-01-01

    when compared to virgin gamma irradiated cross-linked UHMWPE. Groups received equal amount of particulate debris overlaying the calvarium for 10 days. Calvarial bone was examined using high resolution micro-CT and histomorphometric analyses. There was a statistically significant difference between...... virgin (12.2%±8%) and VE-UHMWPE (3%±1.4%) groups in regards to bone resorption (P=0.005) and inflammatory fibrous tissue overlaying the calvaria (0.48 vs. 0.20, P

  4. Supercritical CO2 Foaming of Radiation Cross-Linked Isotactic Polypropylene in the Presence of TAIC

    Directory of Open Access Journals (Sweden)

    Chen-Guang Yang

    2016-12-01

    Full Text Available Since the maximum foaming temperature window is only about 4 °C for supercritical CO2 (scCO2 foaming of pristine polypropylene, it is important to raise the melt strength of polypropylene in order to more easily achieve scCO2 foaming. In this work, radiation cross-linked isotactic polypropylene, assisted by the addition of a polyfunctional monomer (triallylisocyanurate, TAIC, was employed in the scCO2 foaming process in order to understand the benefits of radiation cross-linking. Due to significantly enhanced melt strength and the decreased degree of crystallinity caused by cross-linking, the scCO2 foaming behavior of polypropylene was dramatically changed. The cell size distribution, cell diameter, cell density, volume expansion ratio, and foaming rate of radiation-cross-linked polypropylene under different foaming conditions were analyzed and compared. It was found that radiation cross-linking favors the foamability and formation of well-defined cell structures. The optimal absorbed dose with the addition of 2 wt % TAIC was 30 kGy. Additionally, the foaming temperature window was expanded to about 8 °C, making the handling of scCO2 foaming of isotactic polypropylene much easier.

  5. Incorporation of Decanethiol-Passivated Gold Nanoparticles into Cross-Linked Poly(Dimethylsiloxane Films

    Directory of Open Access Journals (Sweden)

    Motohiro Tagaya

    2011-01-01

    Full Text Available Cross-linking degree of a poly(dimethylsiloxane (PDMS film was controlled, and the incorporation of hydrophobic decanethiol-passivated gold (Au nanoparticles into the film was investigated. FT-IR spectra indicated that the hydrosilylation reaction between a vinyl group and a hydrosilyl group occurred with the cross-linking. The swelling degree of the film in toluene changed with a cross-linker concentration, indicating the control of the cross-linking degree of PDMS film. By EDX analysis, the amount of incorporated Au nanoparticles increased with decreasing a cross-linker concentration, indicating the enlarged free volume of the film. The Au nanoparticle-PDMS composite film containing a cross-linker at 6 wt% showed brown color attributed to plasmon resonance of Au nanoparticles, suggesting the Au nanoparticles in the film at monodispersion state. The UV-visible absorbance of the composite film decreased without spectralshift by swelling with toluene, and the changes were reversible. The aggregation among Au nanoparticles in the composite film after calcination also depended on the cross-linking degree. Thus, the control of cross-linking degree of PDMS film successfully leaded to a simple way of fabricating the Au nanoparticle-PDMS composite film at the mono-dispersion state.

  6. Mapping of the dimer interface of the Escherichia coli mannitol permease by cysteine cross-linking.

    Science.gov (United States)

    van Montfort, Bart A; Schuurman-Wolters, Gea K; Wind, Joyce; Broos, Jaap; Robillard, George T; Poolman, Bert

    2002-04-26

    A cysteine cross-linking approach was used to identify residues at the dimer interface of the Escherichia coli mannitol permease. This transport protein comprises two cytoplasmic domains and one membrane-embedded C domain per monomer, of which the latter provides the dimer contacts. A series of single-cysteine His-tagged C domains present in the native membrane were subjected to Cu(II)-(1,10-phenanthroline)(3)-catalyzed disulfide formation or cysteine cross-linking with dimaleimides of different length. The engineered cysteines were at the borders of the predicted membrane-spanning alpha-helices. Two residues were found to be located in close proximity of each other and capable of forming a disulfide, while four other locations formed cross-links with the longer dimaleimides. Solubilization of the membranes did only influence the cross-linking behavior at one position (Cys(73)). Mannitol binding only effected the cross-linking of a cysteine at the border of the third transmembrane helix (Cys(134)), indicating that substrate binding does not lead to large rearrangements in the helix packing or to dissociation of the dimer. Upon mannitol binding, the Cys(134) becomes more exposed but the residue is no longer capable of forming a stable disulfide in the dimeric IIC domain. In combination with the recently obtained projection structure of the IIC domain in two-dimensional crystals, a first proposal is made for alpha-helix packing in the mannitol permease.

  7. Effects of partial hydrolysis and subsequent cross-linking on wheat gluten physicochemical properties and structure.

    Science.gov (United States)

    Wang, Kaiqiang; Luo, Shuizhong; Cai, Jing; Sun, Qiaoqiao; Zhao, Yanyan; Zhong, Xiyang; Jiang, Shaotong; Zheng, Zhi

    2016-04-15

    The rheological behavior and thermal properties of wheat gluten following partial hydrolysis using Alcalase and subsequent microbial transglutaminase (MTGase) cross-linking were investigated. The wheat gluten storage modulus (G') and thermal denaturation temperature (Tg) were significantly increased from 2.26 kPa and 54.43°C to 7.76 kPa and 57.69°C, respectively, by the combined action of partial hydrolysis (DH 0.187%) and cross-linking. The free SH content, surface hydrophobicity, and secondary structure analysis suggested that an appropriate degree of Alcalase-based hydrolysis allowed the compact wheat gluten structure to unfold, increasing the β-sheet content and surface hydrophobicity. This improved its molecular flexibility and exposed additional glutamine sites for MTGase cross-linking. SEM images showed that a compact 3D network formed, while SDS-PAGE profiles revealed that excessive hydrolysis resulted in high-molecular-weight subunits degrading to smaller peptides, unsuitable for cross-linking. It was also demonstrated that the combination of Alcalase-based partial hydrolysis with MTGase cross-linking might be an effective method for modifying wheat gluten rheological behavior and thermal properties.

  8. Site specificity of psoralen-DNA interstrand cross-linking determined by nuclease Bal31 digestion

    DEFF Research Database (Denmark)

    Zhen, W P; Buchardt, O; Nielsen, Henrik

    1986-01-01

    A novel method for determination of psoralen photo-cross-linking sites in double-stranded DNA is described, which is based on a pronounced inhibition of Bal31 exonuclease activity by psoralen-DNA interstrand cross-links. The results using a 51 base pair fragment of plasmid pUC19 and a 346 base pair...... fragment of pBR322 show that 5'-TA sequences are preferred cross-linking sites compared to 3'-TA sequences. They also indicate that sequences flanking the 5'-TA site influence the cross-linking efficiency at the site. The DNA photo-cross-linking by 4,5',8-trimethylpsoralen and 8-methoxypsoralen...... was analyzed, and these two psoralens showed identical site specificity. The 5'-TA preference is rationalized on the basis of the local DNA structure in terms of the pi-pi electronic interaction between the thymines and the intercalated psoralens, as well as on the base tilt angles of the DNA....

  9. Effects of alginate hydrogel cross-linking density on mechanical and biological behaviors for tissue engineering.

    Science.gov (United States)

    Jang, Jinah; Seol, Young-Joon; Kim, Hyeon Ji; Kundu, Joydip; Kim, Sung Won; Cho, Dong-Woo

    2014-09-01

    An effective cross-linking of alginate gel was made through reaction with calcium carbonate (CaCO3). We used human chondrocytes as a model cell to study the effects of cross-linking density. Three different pore size ranges of cross-linked alginate hydrogels were fabricated. The morphological, mechanical, and rheological properties of various alginate hydrogels were characterized and responses of biosynthesis of cells encapsulated in each gel to the variation in cross-linking density were investigated. Desired outer shape of structure was maintained when the alginate solution was cross-linked with the applied method. The properties of alginate hydrogel could be tailored through applying various concentrations of CaCO3. The rate of synthesized GAGs and collagens was significantly higher in human chondrocytes encapsulated in the smaller pore structure than that in the larger pore structure. The expression of chondrogenic markers, including collagen type II and aggrecan, was enhanced in the smaller pore structure. It was found that proper structural morphology is a critical factor to enhance the performance and tissue regeneration.

  10. Synthesis, Characterization, and Antibacterial Activity of Cross-Linked Chitosan-Glutaraldehyde

    Directory of Open Access Journals (Sweden)

    Long-Biao Guo

    2013-05-01

    Full Text Available This present study deals with synthesis, characterization and antibacterial activity of cross-linked chitosan-glutaraldehyde. Results from this study indicated that cross-linked chitosan-glutaraldehyde markedly inhibited the growth of antibiotic-resistant Burkholderia cepacia complex regardless of bacterial species and incubation time while bacterial growth was unaffected by solid chitosan. Furthermore, high temperature treated cross-linked chitosan-glutaraldehyde showed strong antibacterial activity against the selected strain 0901 although the inhibitory effects varied with different temperatures. In addition, physical-chemical and structural characterization revealed that the cross-linking of chitosan with glutaraldehyde resulted in a rougher surface morphology, a characteristic Fourier transform infrared (FTIR band at 1559 cm−1, a specific X-ray diffraction peak centered at 2θ = 15°, a lower contents of carbon, hydrogen and nitrogen, and a higher stability of glucose units compared to chitosan based on scanning electron microscopic observation, FTIR spectra, X-ray diffraction pattern, as well as elemental and thermo gravimetric analysis. Overall, this study indicated that cross-linked chitosan-glutaraldehyde is promising to be developed as a new antibacterial drug.

  11. Cross-Linking Poly(lactic acid) Film Surface by Neutral Hyperthermal Hydrogen Molecule Bombardment.

    Science.gov (United States)

    Du, Wangli; Shao, Hong; He, Zhoukun; Tang, Changyu; Liu, Yu; Shen, Tao; Zhu, Yan; Lau, Woon-ming; Hui, David

    2015-12-16

    Constructing a dense cross-linking layer on a polymer film surface is a good way to improve the water resistance of poly(lactic acid) (PLA). However, conventional plasma treatments have failed to achieve the aim as a result of the unavoidable surface damage arising from the charged species caused by the uncontrolled high energy coming from colliding ions and electrons. In this work, we report a modified plasma method called hyperthermal hydrogen-induced cross-linking (HHIC) technology to construct a dense cross-linking layer on PLA film surfaces. This method produces energy-controlled neutral hyperthermal hydrogen, which selectively cleaves C-H bonds by molecule collision from the PLA film without breaking other bonds (e.g., C-C bonds in the polymer backbone), and results in subsequent cross-linking of the carbon radicals generated from the organic molecules. The formation of a dense cross-linking layer can serve as a barrier layer to significantly improve both the hydrophobicity and water vapor barrier property of the PLA film. Because of the advantage of selective cleavage of C-H bonds by HHIC treatment, the original physical properties (e.g., mechanical strength and light transmittance) of the PLA films are well-preserved.

  12. Mechanical and biocompatible characterization of a cross-linked collagen-hyaluronic acid wound dressing.

    Science.gov (United States)

    Kirk, James F; Ritter, Gregg; Finger, Isaac; Sankar, Dhyana; Reddy, Joseph D; Talton, James D; Nataraj, Chandra; Narisawa, Sonoko; Millán, José Luis; Cobb, Ronald R

    2013-01-01

    Collagen scaffolds have been widely employed as a dermal equivalent to induce fibroblast infiltrations and dermal regeneration in the treatment of chronic wounds and diabetic foot ulcers. Cross-linking methods have been developed to address the disadvantages of the rapid degradation associated with collagen-based scaffolds. To eliminate the potential drawbacks associated with glutaraldehyde cross-linking, methods using a water soluble carbodiimide have been developed. In the present study, the glycosaminoglycan (GAG) hyaluronic acid (HA), was covalently attached to an equine tendon derived collagen scaffold using 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC) to create ntSPONGE The HA was shown to be homogeneously distributed throughout the collagen matrix. In vitro analyses of the scaffold indicated that the cross-linking enhanced the biological stability by decreasing the enzymatic degradation and increasing the thermal denaturation temperature. The material was shown to support the attachment and proliferation of mouse L929 fibroblast cells. In addition, the cross-linking decreased the resorption rate of the collagen as measured in an intramuscular implant model in rabbits. The material was also shown to be biocompatible in a variety of in vitro and in vivo assays. These results indicate that this cross-linked collagen-HA scaffold, ntSPONGE has the potential for use in chronic wound healing.

  13. Novel Technique of Transepithelial Corneal Cross-Linking Using Iontophoresis in Progressive Keratoconus

    Science.gov (United States)

    Raffa, Paolo; Rosati, Marianna

    2016-01-01

    In this work, the authors presented the techniques and the preliminary results at 6 months of a randomized controlled trial (NCT02117999) comparing a novel transepithelial corneal cross-linking protocol using iontophoresis with the Dresden protocol for the treatment of progressive keratoconus. At 6 months, there was a significant average improvement with an average flattening of the maximum simulated keratometry reading of 0.72 ± 1.20 D (P = 0.01); in addition, corrected distance visual acuity improved significantly (P = 0.08) and spherical equivalent refraction was significantly less myopic (P = 0.02) 6 months after transepithelial corneal cross-linking with iontophoresis. The novel protocol using iontophoresis showed comparable results with standard corneal cross-linking to halt progression of keratoconus during 6-month follow-up. Investigation of the long-term RCT outcomes are ongoing to verify the efficacy of this transepithelial corneal cross-linking protocol and to determine if it may be comparable with standard corneal cross-linking in the management of progressive keratoconus. PMID:27597895

  14. Novel Technique of Transepithelial Corneal Cross-Linking Using Iontophoresis in Progressive Keratoconus

    Directory of Open Access Journals (Sweden)

    Marco Lombardo

    2016-01-01

    Full Text Available In this work, the authors presented the techniques and the preliminary results at 6 months of a randomized controlled trial (NCT02117999 comparing a novel transepithelial corneal cross-linking protocol using iontophoresis with the Dresden protocol for the treatment of progressive keratoconus. At 6 months, there was a significant average improvement with an average flattening of the maximum simulated keratometry reading of 0.72±1.20 D (P=0.01; in addition, corrected distance visual acuity improved significantly (P=0.08 and spherical equivalent refraction was significantly less myopic (P=0.02 6 months after transepithelial corneal cross-linking with iontophoresis. The novel protocol using iontophoresis showed comparable results with standard corneal cross-linking to halt progression of keratoconus during 6-month follow-up. Investigation of the long-term RCT outcomes are ongoing to verify the efficacy of this transepithelial corneal cross-linking protocol and to determine if it may be comparable with standard corneal cross-linking in the management of progressive keratoconus.

  15. Cross-linking study on skeletal muscle actin: properties of suberimidate-treated actin.

    Science.gov (United States)

    Ohara, O; Takahashi, S; Ooi, T; Fujiyoshi, Y

    1982-06-01

    Cross-linking experiments were performed on muscle skeletal actin, using imidoesters of various chain lengths. Chemical analyses on all products except one (derived from succinimidate) show evidence of the presence of intramolecular cross-links in the molecule. The detailed properties of suberimidate-treated actin (SA) are as follows: SA contains nearly 1 mol of intramolecular cross-link per mol of actin and less than 15% of intermolecularly cross-linked products. Even at a low salt concentration, SA is polymeric, exchanges slowly its bound nucleotide with free nucleotides in solution, and shows an F-actin-type CD spectrum. Electron micrographs of SA reveal that SA exists actually as fibrous polymers in solutions of low ionic strength, although the fibers seem to be less rigid than those at high salt concentration. The F-form of SA at a high salt concentration is indistinguishable from intact F-actin. SA can bind heavy meromyosin and activate the ATPase of heavy meromyosin as observed for intact F-actin. Tropomyosin binds SA only at a high salt concentration. These results show that SA possesses the properties of F-actin even in media of low salt concentration, which are favorable for depolymerization of F-actin. Thus, we may infer that the conformation of SA is frozen in the F-state of actin by the introduction of intramolecular cross-links in the protein.

  16. DNA interstrand cross-link induced by estrogens as well as their complete and synergic carcinogenesis

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The estrogens show negative activity in Ames test, but estrodiol and diethylstilbestrol in estrogens both are carcinogens based upon animal experiments and epidemiological investigation. It is concluded from the di-region theory, a mechanism conception put forward by one of the present authors, that the carcinogenesis of estrogens is switched on by the covalent cross-link between complementary DNA bases induced by them. We verified for the first time by the DNA alkaline elution method that both estrodiol and diethylstilbestrol cause covalent cross-link between DNA-protein and DNA interstrands after metabolic activation with dosage correlation, but neither the non-carcinogens cholesterol nor pyrene can lead to these sorts of cross-link in the same condition. It has been known that there is a synergetic effect between estrogen and pollution of polycyclic aromatic hydrocarbons. Although non-carcinogenic pyrene alone cannot induce cross-link, its addition with equal molar quantity to estrodiol culture causes synergically the total and DNA interstrand cross-link ratios to be respectively four and three times more than the ones in the cultivation with estrodiol only. It is shown that not only the estrodiol set off the formation of pyrene bi-radicals, but also the pyrene radicals arouse conversely the production of estrodiol bi-radicals.

  17. Transesterification using the cross-linked enzyme aggregate of Photobacterium lipolyticum lipase M37.

    Science.gov (United States)

    Han, Jin Yee; Kim, Hyung Kwoun

    2011-11-01

    Biodiesel is methyl and ethyl esters of long-chain fatty acids produced from vegetable oils or animal fats. Lipase enzymes have occasionally been used for the production of this biofuel. Recently, biodiesel production using immobilized lipase has received increased attention. Through enhanced stability and reusability, immobilized lipase can contribute to the reduction of the costs inherent to biodiesel production. In this study, methanol-tolerant lipase M37 from Photobacterium lipolyticum was immobilized using the cross-linked enzyme aggregate (CLEA) method. Lipase M37 has a high lysine content (9.7%) in its protein sequence. Most lysine residues are located evenly over the surface of the protein, except for the lid structure region, which makes the CLEA preparation yield quite high (~93%). CLEA M37 evidences an optimal temperature of 30oC, and an optimal pH of 9-10. It was stable up to 50°C and in a pH range of 4.0-11.0. Both soluble M37 and CLEA M37 were stable in the presence of high concentrations of methanol, ethanol, 1-propanol, and nbutanol. That is, their activities were maintained at solvent concentrations above 10% (v/v). CLEA M37 could produce biodiesel from olive oil and alcohols such as methanol and ethanol. Additionally, CLEA M37 generated biodiesel via both 2-step methanol feeding procedures. Considering its physical stability and reusability, CLEA M37 may potentially be used as a catalyst in organic synthesis, including the biodiesel production reaction.

  18. Polymer composition and substrate influences on the adhesive bonding of a biomimetic, cross-linking polymer.

    Science.gov (United States)

    Matos-Pérez, Cristina R; White, James D; Wilker, Jonathan J

    2012-06-06

    Hierarchical biological materials such as bone, sea shells, and marine bioadhesives are providing inspiration for the assembly of synthetic molecules into complex structures. The adhesive system of marine mussels has been the focus of much attention in recent years. Several catechol-containing polymers are being developed to mimic the cross-linking of proteins containing 3,4-dihydroxyphenylalanine (DOPA) used by shellfish for sticking to rocks. Many of these biomimetic polymer systems have been shown to form surface coatings or hydrogels; however, bulk adhesion is demonstrated less often. Developing adhesives requires addressing design issues including finding a good balance between cohesive and adhesive bonding interactions. Despite the growing number of mussel-mimicking polymers, there has been little effort to generate structure-property relations and gain insights on what chemical traits give rise to the best glues. In this report, we examine the simplest of these biomimetic polymers, poly[(3,4-dihydroxystyrene)-co-styrene]. Pendant catechol groups (i.e., 3,4-dihydroxystyrene) are distributed throughout a polystyrene backbone. Several polymer derivatives were prepared, each with a different 3,4-dihyroxystyrene content. Bulk adhesion testing showed where the optimal middle ground of cohesive and adhesive bonding resides. Adhesive performance was benchmarked against commercial glues as well as the genuine material produced by live mussels. In the best case, bonding was similar to that obtained with cyanoacrylate "Krazy Glue". Performance was also examined using low- (e.g., plastics) and high-energy (e.g., metals, wood) surfaces. The adhesive bonding of poly[(3,4-dihydroxystyrene)-co-styrene] may be the strongest of reported mussel protein mimics. These insights should help us to design future biomimetic systems, thereby bringing us closer to development of bone cements, dental composites, and surgical glues.

  19. Photochromic cross-link polymer for color changing and sensing surface

    Science.gov (United States)

    Fu, Richard; Shi, Jianmin; Forsythe, Eric; Srour, Merric

    2016-12-01

    Photochromic cross-link polymers were developed using patented ultraviolet (UV) photoinitiator and commercial photochromic dyes. The photochromic dyes have been characterized by measuring absorbance before and after UV activation using UV-visible (Vis) spectrometry with varying activation intensities and wavelengths. Photochromic cross-link polymers were characterized by a dynamic xenon and UV light activation and fading system. The curing processes on cloth were established and tested to obtain effective photochromic responses. Both PulseForge photonic curing and PulseForge plus heat surface curing processes had much better photochromic responses (18% to 19%, 16% to 25%, respectively) than the xenon lamp treatment (8%). The newly developed photochromic cross-link polymer showed remarkable coloration contrasts and fast and comparable coloration and fading rates. Those intelligent, controlled color changing and sensing capabilities will be used on flexible and "drapeable" surfaces, which will incorporate ultra-low power sensors, sensor indicators, and identifiers.

  20. Optimizing end-group cross-linking polymer electrolytes for fuel cell applications

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Yu Seung [Los Alamos National Laboratory; Lee, Kwan Soo [Los Alamos National Laboratory; Jeong, Myung - Hwan [GIST, KOREA; Lee, Jae - Suk [GIST, KOREA

    2009-01-01

    This paper demonstrates the optimization of proton conductivity and water uptake for cross-linkable polymer electrolytes through synthesis and characterization of end-group cross-linkable sulfonated poly(arylene ether) copolymers (ESF-BPs). The extent of reaction of cross-linking was controlled by reaction time resulting in a series of polymers with two, independent tunable parameters, degree of sulfonation (DS) and degree of cross-linking (DC). For the polymers presented, cross-linking improved proton conductivity while reducing water uptake, an uncommon trend in polymer electrolytes where water is critical for proton conduction. Other trends relating to changes are reported and the results yield insight into the role of DS and DC and how to optimize electrochemical properties and performance of polymer electrolytes through these tunable parameters. Select polymer electrolytes were tested in fuel cells where performance and durability with accelerated relative humidity cycling were compared with Nafion{reg_sign}.

  1. Cross-linked PAN-based thin-film composite membranes for non-aqueous nanofiltration

    KAUST Repository

    Pérez-Manríquez, Liliana

    2015-01-01

    A new approach on the development of cross-linked PAN based thin film composite (TFC) membranes for non-aqueous application is presented in this work. Polypropylene backed neat PAN membranes fabricated by phase inversion process were cross-linked with hydrazine to get excellent solvent stability toward dimethylformamide (DMF). By interfacial polymerization a selective polyamide active layer was coated over the cross-linked PAN using N,N′-diamino piperazine (DAP) and trimesoyl chloride (TMC) as monomers. Permeation and molecular weight cut off (MWCO) experiments using various dyes were done to evaluate the performance of the membranes. Membranes developed by such method show excellent solvent stability toward DMF with a permeance of 1.7 L/m2 h bar and a molecular weight cut-off of less than 600 Da.

  2. Light-triggered cross-linking of alginates with caged Ca2+.

    Science.gov (United States)

    Cui, Jiaxi; Wang, Miao; Zheng, Yijun; Rodríguez Muñiz, Gemma Maria; del Campo, Aránzazu

    2013-05-13

    A strategy to light-trigger ionic cross-linking of alginates by incorporating a photosensitive Ca2+ cage (nitr-T) is presented. Upon irradiation, free Ca2+ was released, and this caused gelation of the alginate solution. Addition of Ca2+ "on-demand" allowed us to obtain homogeneous alginate (ALG) gels using concentrated initial ALG solutions (10%), not possible with other ionic gelation approaches. The cross-linking degree and derived mechanical properties of the hydrogel were modulated by the exposure dose. The light-mediated cross-linked alginate hydrogel displayed a significant improvement in the mechanical properties and homogeneity when compared to mixtures of alginate and soluble Ca2+ at comparable concentrations.

  3. Synthesis of acrylic and allylic bifunctional cross-linking monomers derived from PET waste

    Science.gov (United States)

    Cruz-Aguilar, A.; Herrera-González, A. M.; Vázquez-García, R. A.; Navarro-Rodríguez, D.; Coreño, J.

    2013-06-01

    An acrylic and two novel allylic monomers synthesized from bis (hydroxyethyl) terephthalate, BHET, are reported. This was obtained by glycolysis of post-consumer PET with boiling ethylene glycol. The bifunctional monomer bis(2-(acryloyloxy)ethyl) terephthalate was obtained from acryloyl chloride, while the allylic monomers 2-(((allyloxi)carbonyl)oxy) ethyl (2-hydroxyethyl) terephthalate and bis(2-(((allyloxi)carbonyl)oxy)ethyl) terephthalate, from allyl chloroformate. Cross-linking was studied in bulk polymerization using two different thermal initiators. Monomers were analyzed by means of 1H NMR and the cross-linked polymers by infrared spectroscopy. Gel content higher than 90% was obtained for the acrylic monomer. In the case of the mixture of the allylic monomers, the cross-linked polymer was 80 % using BPO initiator, being this mixture 24 times less reactive than the acrylic monomer.

  4. Cheese whey protein recovery by ultrafiltration through transglutaminase (TG) catalysis whey protein cross-linking.

    Science.gov (United States)

    Wen-Qiong, Wang; Lan-Wei, Zhang; Xue, Han; Yi, Lu

    2017-01-15

    In whey ultrafiltration (UF) production, two main problems are whey protein recovery and membrane fouling. In this study, membrane coupling protein transglutaminase (TG) catalysis protein cross-linking was investigated under different conditions to find out the best treatment. We found that the optimal conditions for protein recovery involved catalyzing whey protein cross-linking with TG (40U/g whey proteins) at 40°C for 60min at pH 5.0. Under these conditions, the recovery rate was increased 15-20%, lactose rejection rate was decreased by 10%, and relative permeate flux was increase 30-40% compared to the sample without enzyme treatment (control). It was noticeable that the total resistance and cake resistance were decreased after enzyme catalysis. This was mainly due to the increased particle size and decreased zeta potential. Therefore, membrane coupling enzyme catalysis protein cross-linking is a potential means for further use.

  5. Solution processed organic light-emitting diodes using the plasma cross-linking technology

    Science.gov (United States)

    He, Kongduo; Liu, Yang; Gong, Junyi; Zeng, Pan; Kong, Xun; Yang, Xilu; Yang, Cheng; Yu, Yan; Liang, Rongqing; Ou, Qiongrong

    2016-09-01

    Solution processed multilayer organic light-emitting diodes (OLEDs) present challenges, especially regarding dissolution of the first layer during deposition of a second layer. In this work, we first demonstrated a plasma cross-linking technology to produce a solution processed OLED. The surfaces of organic films can be cross-linked after mixed acetylene and Ar plasma treatment for several tens of seconds and resist corrosion of organic solvent. The film thickness and surface morphology of emissive layers (EMLs) with plasma treatment and subsequently spin-rinsed with chlorobenzene are nearly unchanged. The solution processed triple-layer OLED is successfully fabricated and the current efficiency increases 50% than that of the double-layer OLED. Fluorescent characteristics of EMLs are also observed to investigate factors influencing the efficiency of the triple-layer OLED. Plasma cross-linking technology may open up a new pathway towards fabrication of all-solution processed multilayer OLEDs and other soft electronic devices.

  6. Improvement on Physical Properties of Pullulan Films by Novel Cross-Linking Strategy.

    Science.gov (United States)

    Chen, Chieh-Ting; Chen, Kuan-I; Chiang, Hsin-Han; Chen, Yu-Kuo; Cheng, Kuan-Chen

    2017-01-01

    Pullulan based films possess several advantages, including high transparency, low toxicity, good biodegradability, good mechanical properties, and low oxygen permeability, are preferable for food packaging. The application of pullulan films on food packaging, however, has inherent disadvantage of high water solubility. In this study, glutaraldehyde and glycerol were used as the cross-linking reagent and the plasticizer respectively to improve water resistance and physical properties of the pullulan films. Effects of cross-linking degree on physical properties, including water absorptions, swelling behaviors, water vapor permeability and tensile strengths of films were evaluated. FTIR results demonstrated that the pullulan films were successfully cross-linked by glutaraldehyde. The tensile strength of pullulan films could be enhanced significantly (P glycerol as a plasticizer enhanced the extensibility of films as well as the hydrophilicity, resulting in higher water vapor permeability.

  7. Comparison of Wear and Oxidation in Retrieved Conventional and Highly Cross-Linked UHMWPE Tibial Inserts.

    Science.gov (United States)

    Currier, Barbara H; Currier, John H; Franklin, Katherine J; Mayor, Michael B; Reinitz, Steven D; Van Citters, Douglas W

    2015-12-01

    Two groups of retrieved tibial inserts from one manufacturer's knee system were analyzed to evaluate the effect of a highly cross-linked bearing surface on wear and in vivo oxidation. The two groups ((1) conventional gamma-inert sterilized and (2) highly cross-linked, coupled with the same rough (Ra=0.25) Ti-6Al-4V tray) were matched with statistically similar in vivo duration and patient variables. The retrieved inserts were analyzed for ketone oxidation and wear in the form of dimensional change. The difference in oxidation rate between highly cross-linked and conventional gamma-inert sterilized inserts did not reach statistical significance. Observations suggest that the majority of wear can be accounted for by the backside interface with the rough Ti-6Al-4V tray; however, wear measured by thickness-change rate was statistically indistinguishable between the two bearing materials.

  8. Biomimetic acellular detoxified glutaraldehyde cross-linked bovine pericardium for tissue engineering

    Energy Technology Data Exchange (ETDEWEB)

    Mathapati, Santosh; Bishi, Dillip Kumar [Stem Cell and Molecular Biology Laboratory, Department of Biotechnology, Indian Institute of Technology Madras, Chennai (India); Frontier Lifeline Pvt Ltd. and Dr. K. M. Cherian Heart Foundation, Mogappair, Chennai (India); Healthcare and Energy Materials Laboratory, NUSNNI, Faculty of Engineering, National University of Singapore (Singapore); Guhathakurta, Soma [Departmet of Engineering Design, Indian Institute of Technology Madras, Chennai (India); Cherian, Kotturathu Mammen [Frontier Lifeline Pvt Ltd. and Dr. K. M. Cherian Heart Foundation, Mogappair, Chennai (India); Venugopal, Jayarama Reddy; Ramakrishna, Seeram [Healthcare and Energy Materials Laboratory, NUSNNI, Faculty of Engineering, National University of Singapore (Singapore); Verma, Rama Shanker, E-mail: vermars@iitm.ac.in [Stem Cell and Molecular Biology Laboratory, Department of Biotechnology, Indian Institute of Technology Madras, Chennai (India)

    2013-04-01

    Glutaraldehyde (GLUT) processing, cellular antigens, calcium ions in circulation, and phospholipids present in the native tissue are predominantly responsible for calcification, degeneration, and lack of natural microenvironment for host progenitor cell migration in tissue implants. The study presents an improved methodology for adhesion and proliferation of endothelial progenitor cells (EPCs) without significant changes in biomechanical and biodegradation properties of the processed acellular bovine pericardium. The anti-calcification potential of the processed tissue was enhanced by detoxification of GLUT-cross-linked bovine pericardium by decellularization, pretreating it with ethanol or removing the free aldehydes by citric acid treatment and lyophilization. The treated tissues were assessed for biomechanical properties, GLUT ligand quantification, adhesion, proliferation of EPCs, and biodegradability. The results indicate that there was no significant change in biomechanical properties and biodegradability when enzymatic hydrolysis (p > 0.05) is employed in detoxified acellular GLUT cross-linked tissue (DBP–G–CA–ET), compared with the native detoxified GLUT cross-linked bovine pericardium (NBP–G–CA–ET). DBP–G–CA–ET exhibited a significant (p > 0.05) increase in the viability of EPCs and cell adhesion as compared to acellular GLUT cross-linked bovine pericardium (p < 0.05). Lyophilized acellular detoxified GLUT cross-linked bovine pericardium, employed in our study as an alternative to conventional GLUT cross-linked bovine pericardium, might provide longer durability and better biocompatibility, and reduce calcification. The developed bovine pericardium patches could be used in cardiac reconstruction and repair, arteriotomy, soft tissue repair, and general surgical procedures with tissue regeneration dimensions. - Highlights: ► We improved the quality of patch biomaterial for cardiovascular surgical procedures. ► Bovine pericardium was

  9. Cross-linking and rheological changes of whey proteins treated with microbial transglutaminase.

    Science.gov (United States)

    Truong, Van-Den; Clare, Debra A; Catignani, George L; Swaisgood, Harold E

    2004-03-10

    Modification of the functionality of whey proteins using microbial transglutaminase (TGase) has been the subject of recent studies. However, changes in rheological properties of whey proteins as affected by extensive cross-linking with TGase are not well studied. The factors affecting cross-linking of whey protein isolate (WPI) using both soluble and immobilized TGase were examined, and the rheological properties of the modified proteins were characterized. The enzyme was immobilized on aminopropyl glass beads (CPG-3000) by selective adsorption of the biotinylated enzyme on avidin that had been previously immobilized. WPI (4 and 8% w/w) in deionized water, pH 7.5, containing 10 mM dithiothreitol was cross-linked using enzyme/substrate ratios of 0.12-10 units of activity/g WPI. The reaction was carried out in a jacketed bioreactor for 8 h at 40 degrees C with continuous circulation. The gel point temperature of WPI solutions treated with 0.12 unit of immobilized TGase/g was slightly decreased, but the gel strength was unaffected. However, increasing the enzyme/substrate ratio resulted in extensive cross-linking of WPI that was manifested by increases in apparent viscosity and changes in the gelation properties. For example, using 10 units of soluble TGase/g resulted in extensive cross-linking of alpha-lactalbumin and beta-lactoglobulin in WPI, as evidenced by SDS-PAGE and Western blotting results. Interestingly, the gelling point of WPI solutions increased from 68 to 94 degrees C after a 4-h reaction, and the gel strength was drastically decreased (lower storage modulus, G'). Thus, extensive intra- and interchain cross-linking probably caused formation of polymers that were too large for effective network development. These results suggest that a process could be developed to produce heat-stable whey proteins for various food applications.

  10. Collagen telopeptides (cross-linking sites) play a role in collagen gel lattice contraction

    Science.gov (United States)

    Woodley, D. T.; Yamauchi, M.; Wynn, K. C.; Mechanic, G.; Briggaman, R. A.

    1991-01-01

    Solubilized interstitial collagens will form a fibrillar, gel-like lattice when brought to physiologic conditions. In the presence of human dermal fibroblasts the collagen lattice will contract. The rate of contraction can be determined by computer-assisted planemetry. The mechanisms involved in contraction are as yet unknown. Using this system it was found that the rate of contraction was markedly decreased when collagen lacking telopeptides was substituted for native collagen. Histidinohydroxylysinonorleucine (HHL) is a major stable trifunctional collagen cross-link in mature skin that involves a carboxyl terminal, telopeptide site 16c, the sixteenth amino acid residue from the carboxy terminal of the telopeptide region of alpha 1 (I) in type I collagen. Little, if any, HHL was present in native, purified, reconstituted, soluble collagen fibrils from 1% acetic acid-extracted 2-year-old bovine skin. In contrast, HHL cross-links were present (0.22 moles of cross-link per mole of collagen) in lattices of the same collagen contracted by fibroblasts. However, rat tail tendon does not contain HHL cross-links, and collagen lattices made of rat tail tendon collagen are capable of contraction. This suggests that telopeptide sites, and not mature HHL cross-links per se, are essential for fibroblasts to contract collagen lattices. Beta-aminopropionitrile fumarate (BAPN), a potent lathyrogen that perturbs collagen cross-linking by inhibition of lysyl oxidase, also inhibited the rate of lattice cell contraction in lattices composed of native collagen. However, the concentrations of BAPN that were necessary to inhibit the contraction of collagen lattices also inhibited fibroblast growth suggestive of cellular toxicity. In accordance with other studies, we found no inhibition of the rate of lattice contraction when fibronectin-depleted serum was used. Electron microscopy of contracted gels revealed typical collagen fibers with a characteristic axial periodicity. The data

  11. Increasing Thermal Stability of Gelatin by UV-Induced Cross-Linking with Glucose

    Directory of Open Access Journals (Sweden)

    Evan M. Masutani

    2014-01-01

    Full Text Available The effects of ultraviolet (254 nm radiation on a hydrated gelatin-glucose matrix were investigated for the development of a physiologically thermostable substrate for potential use in cell scaffold production. Experiments conducted with a differential scanning calorimeter indicate that ultraviolet irradiation of gelatin-glucose hydrogels dramatically increases thermal stability such that no melting is observed at temperatures of at least 90°C. The addition of glucose significantly increases the yield of cross-linked product, suggesting that glucose has a role in cross-link formation. Comparisons of lyophilized samples using scanning electron microscopy show that irradiated materials have visibly different densities.

  12. A novel DTPA cross-linking of hyaluronic acid and metal complexation thereof.

    Science.gov (United States)

    Buffa, Radovan; Běťák, Jiří; Kettou, Sofiane; Hermannová, Martina; Pospíšilová, Lucie; Velebný, Vladimír

    2011-09-27

    Macromolecular conjugates of a natural polysaccharide, hyaluronic acid, with diethylenetriaminepentaacetic acid (DTPA)-metal complexes were synthesized and characterized by FTIR, NMR, SEC-MALLS and ICP analysis. Several parameters of the cross-linking reaction as molecular weight of starting HA, temperature, equivalent of DTPA bis-anhydride, concentration of HA, presence of transacylation catalyst DMAP and reaction time were studied. The mechanism for the reaction was suggested and relationship between the molecular weight assigned by SEC-MALLS, reaction parameters and rheological properties of the final cross-linked products were investigated. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Reinforced films based on cross-linked water-soluble sulfonated carbon nanotubes with sulfonated polystyrene.

    Science.gov (United States)

    Dai, Ying; Haiping, Hong; Guiver, Michael; Welsh, Jeffry S

    2009-09-01

    Reinforced films based on sulfonated polystyrene cross-linked with water-soluble sulfonated carbon nanotubes were fabricated using a free-standing film-making method. Transmission and scanning electron microscopy (TEM and SEM), and X-ray photoelectron spectroscopy (XPS) were used to verify the cross-linking reaction. The mechanical properties of these films demonstrated that the tensile strength increases with an increase in the sulfonated nanotube concentration. At 5 wt% nanotube loading, the tensile strength increased 84% compared with polymer containing no nanotube loading. The relationships between structure and mechanical properties are discussed and a possible direction for making ultra thin and ultra lightweight film is proposed.

  14. Kinetics of enzyme-catalyzed cross-linking of feruloylated arabinan from sugar beet

    DEFF Research Database (Denmark)

    Abang Zaidel, Dayang Norulfairuz; Arnous, Anis; Holck, Jesper

    2011-01-01

    the kinetics of HRP catalyzed cross-linking of FA esterified to α-(1,5)-linked arabinans are affected by the length of the arabinan chains carrying the feruloyl substitutions. The kinetics of the HRP-catalyzed cross-linking of four sets of arabinan samples from sugar beet pulp, having different molecular...... weights and hence different degrees of polymerization, were monitored by the disappearance of FA absorbance at 316 nm. MALDI-TOF/TOF-MS analysis confirmed that the sugar beet arabinans were feruloyl-substituted, and HPLC analysis verified that the amounts of diFAs increased when FA levels decreased...

  15. In Situ Cross-Linking of Stimuli-Responsive Hemicellulose Microgels during Spray Drying

    OpenAIRE

    Zhao, Weifeng; Nugroho, Robertus Wahyu N.; Odelius, Karin; Edlund, Ulrica; Zhao, Changsheng; Albertsson, Ann-Christine

    2015-01-01

    Chemical cross-linking during spray drying offers the potential for green fabrication of microgels with a rapid stimuli response and good blood compatibility and provides a platform for stimuli-responsive hemicellulose microgels (SRHMGs). The cross-linking reaction occurs rapidly in situ at elevated temperature during spray drying, enabling the production of microgels in a large scale within a few minutes. The SRHMGs with an average size range of ∼1–4 μm contain O-acetyl-galactoglucomannan as...

  16. Mutational Analysis of a Conserved Glutamic Acid Required for Self-Catalyzed Cross-Linking of Bacteriophage HK97 Capsids▿

    Science.gov (United States)

    Dierkes, Lindsay E.; Peebles, Craig L.; Firek, Brian A.; Hendrix, Roger W.; Duda, Robert L.

    2009-01-01

    The capsid of bacteriophage HK97 is stabilized by ∼400 covalent cross-links between subunits which form without any action by external enzymes or cofactors. Cross-linking only occurs in fully assembled particles after large-scale structural changes bring together side chains from three subunits at each cross-linking site. Isopeptide cross-links form between asparagine and lysine side chains on two subunits. The carboxylate of glutamic acid 363 (E363) from a third subunit is found ∼2.4 Å from the isopeptide bond in the partly hydrophobic pocket that contains the cross-link. It was previously reported without supporting data that changing E363 to alanine abolishes cross-linking, suggesting that E363 plays a role in cross-linking. This alanine mutant and six additional substitutions for E363 were fully characterized and the proheads produced by the mutants were tested for their ability to cross-link under a variety of conditions. Aspartic acid and histidine substitutions supported cross-linking to a significant extent, while alanine, asparagine, glutamine, and tyrosine did not, suggesting that residue 363 acts as a proton acceptor during cross-linking. These results support a chemical mechanism, not yet fully tested, that incorporates this suggestion, as well as features of the structure at the cross-link site. The chemically identical isopeptide bonds recently documented in bacterial pili have a strikingly similar chemical geometry at their cross-linking sites, suggesting a common chemical mechanism with the phage protein, but the completely different structures and folds of the two proteins argues that the phage capsid and bacterial pilus proteins have achieved shared cross-linking chemistry by convergent evolution. PMID:19091865

  17. Cross-linked carbon network with hierarchical porous structure for high performance solid-state electrochemical capacitor

    Science.gov (United States)

    Cheng, Yongliang; Huang, Liang; Xiao, Xu; Yao, Bin; Hu, Zhimi; Li, Tianqi; Liu, Kang; Zhou, Jun

    2016-09-01

    The development of portable electronics strongly requires flexible, lightweight, and inexpensive energy-storage devices with high power density, long cycling stability, and high reliability. In this work, we prepare a flexible solid-state electrochemical capacitor using cross-linked hierarchical porous carbon network as electrode material via electrospinning and carbonization process. This device can reversibly deliver a maximum energy density of 10.18 W h/kg with excellent cycling stability which achieves 95% capacitance retention after 20000 charge/discharge cycles. Moreover, it also demonstrates outstanding mechanical flexibility and excellent capacitance retention even when the device is repeatedly bended 10000 cycles under 90°. All of these results suggest its promising perspective in flexible energy storage device.

  18. Effect of Addition of Soybean Oil and Gamma-Ray Cross-linking on the Nanoporous HDPE Membrane

    Directory of Open Access Journals (Sweden)

    Jong-Seok Park

    2012-01-01

    Full Text Available A nanoporous high-density polyethylene (HDPE membrane was prepared by a wet process. Soybean oil and dibutyl phthalate (DBP were premixed as codiluents, and gamma-rays were used for the cross-linking of HDPE. The pore volume of the nanoporous HDPE membranes with soybean oil was affected by the extracted amount of oil. The tensile strength of the membrane improved with an increasing absorbed dose up to 60 kGy, but decreased at 80 kGy due to severe degradation. The ionic conductivity of the nanoporous HDPE membrane did not really change with an increasing absorbed dose because the pores had already been formed before the gamma-ray radiation. Finally, the electrochemical stability of the HDPE membrane increased when the absorbed dose increased up to 60 kGy.

  19. A Hyper-cross-linked Polynaphthalene Semiconductor with Excellent Visible-Light Photocatalytic Performance in the Degradation of Organic Dyes.

    Science.gov (United States)

    Zhang, Lei; Huang, Xin-Hua; Hu, Jin-Song; Song, Jian; Kim, Il

    2017-02-28

    Hyper-cross-linked polynaphthalene nanoparticles (PNNs) capable of catalyzing the degradation of organic pollutants upon exposure to visible light have been developed. The nascent and metal-free PNNs with a porous structure, high specific surface area, and narrow bandgap are chemically and thermally stable in the catalytic system, which make it promising as a kind of excellent photocatalytic material compared to conventional photocatalysts. The photocatalytic activity of the as-obtained PNNs exhibits remarkable photocatalytic performance for the degradation of rhodamine B (RhB) and methyl blue (MB) under the irradiation of visible light. The easy preparation, high catalytic activity, and recyclability of the PNNs open new opportunities in the visible-light-promoted degradation of organic pollutants.

  20. Aliphatic polycarbonates based on carbon dioxide, furfuryl glycidyl ether, and glycidyl methyl ether: reversible functionalization and cross-linking.

    Science.gov (United States)

    Hilf, Jeannette; Scharfenberg, Markus; Poon, Jeffrey; Moers, Christian; Frey, Holger

    2015-01-01

    Well-defined poly((furfuryl glycidyl ether)-co-(glycidyl methyl ether) carbonate) (P((FGE-co-GME)C)) copolymers with varying furfuryl glycidyl ether (FGE) content in the range of 26% to 100% are prepared directly from CO2 and the respective epoxides in a solvent-free synthesis. All materials are characterized by size-exclusion chromatography (SEC), (1)H NMR spectroscopy, and differential scanning calorimetry (DSC). The furfuryl-functional samples exhibit monomodal molecular weight distributions with Mw/Mn in the range of 1.16 to 1.43 and molecular weights (Mn) between 2300 and 4300 g mol(-1). Thermal properties reflect the amorphous structure of the polymers. Both post-functionalization and cross-linking are performed via Diels-Alder chemistry using maleimide derivatives, leading to reversible network formation. This transformation is shown to be thermally reversible at 110 °C.

  1. Synthesis,characterization and swelling properties of a chemically cross-linked poly(vinyl alcohol) hydrogel

    Institute of Scientific and Technical Information of China (English)

    LI Wenbo; XUE Feng; CHENG Rongshi

    2007-01-01

    A poly(vinyl alcohol) hydrogel was prepared by coupling poly(vinyl alcohol) with epichlorohydrin as the cross-linking agent.The structure of the hydrogel was characterized by FTIR and GPC techniques.Various amounts of water were added into the dry gel to swell it,and the quantity of water in various states in the partially swollen hydrogel was determined by DSC technique.The analytical results indicate that the water introduced into the dry gel first combines with the hydrophilic groups of the network chains through hydrogen bond forming non-freezable water.The weight ratio of the non-freezable water to dry gel in the hydrogels is about 0.20.After the non-freezable water is saturated,the additional water penetrates the network space and exists simultaneously both in the freezable and free water states until reaching equilibrium swelling.

  2. Tuning heterogeneous poly(dopamine) structures and mechanics: in silico covalent cross-linking and thin film nanoindentation.

    Science.gov (United States)

    Lin, Shangchao; Chen, Chun-Teh; Bdikin, Igor; Ball, Vincent; Grácio, José; Buehler, Markus J

    2014-01-21

    Mussel-inspired synthetic poly(dopamine) thin films from dihydroxyphenylalanine (DOPA) and lysine, structurally similar to natural melanin, have drawn extensive interest as a versatile surface functionalization and coating material for use in a broad range of applications. In order to gain a better understanding of its complex and heterogeneous polymeric structure and mechanical properties, we report a computational model of poly(dopamine) by mimicking the polymerization process of the intermediate oxidized product of dopamine, 5,6-dihydroxyindole (DHI), via controlled in silico covalent cross-linking under the two most possible reaction schemes proposed in experiments. To validate our results using experiment, we synthesize poly(dopamine) thin films and perform experimental nanoindentations on the film. We observe an overall linear behavior for Young's modulus as a function of the degree of cross-linking, demonstrating the possibility of enhancing the mechanical robustness of poly(dopamine) materials by increasing the extent of polymerization. At the highest degree of polymerization considered (70%), the model mimics the linear tetrameric model for poly(dopamine) and melanin. At this degree of polymerization, we find a Young's modulus of 4.1-4.4 GPa, in agreement with our nanoindentation results of 4.3-10.5 GPa, previous experiments for natural melanin, as well as simulation results for the cyclic tetrameric melanin model (Chen et al., ACS Nano, 2013). Our results suggest that the non-covalent DHI aggregate model might not be appropriate to represent the structure of poly(dopamine) and melanin-like materials, since it gives a much smaller Young's modulus than the experimental lower bound. Our model not only nicely complements the previous computational work, but also provides new computational tools to study the heterogeneous structural and physicochemical properties of poly(dopamine) and melanin, as well as their formation pathways.

  3. Use of proteinase K nonspecific digestion for selective and comprehensive identification of interpeptide cross-links: application to prion proteins.

    Science.gov (United States)

    Petrotchenko, Evgeniy V; Serpa, Jason J; Hardie, Darryl B; Berjanskii, Mark; Suriyamongkol, Bow P; Wishart, David S; Borchers, Christoph H

    2012-07-01

    Chemical cross-linking combined with mass spectrometry is a rapidly developing technique for structural proteomics. Cross-linked proteins are usually digested with trypsin to generate cross-linked peptides, which are then analyzed by mass spectrometry. The most informative cross-links, the interpeptide cross-links, are often large in size, because they consist of two peptides that are connected by a cross-linker. In addition, trypsin targets the same residues as amino-reactive cross-linkers, and cleavage will not occur at these cross-linker-modified residues. This produces high molecular weight cross-linked peptides, which complicates their mass spectrometric analysis and identification. In this paper, we examine a nonspecific protease, proteinase K, as an alternative to trypsin for cross-linking studies. Initial tests on a model peptide that was digested by proteinase K resulted in a "family" of related cross-linked peptides, all of which contained the same cross-linking sites, thus providing additional verification of the cross-linking results, as was previously noted for other post-translational modification studies. The procedure was next applied to the native (PrP(C)) and oligomeric form of prion protein (PrPβ). Using proteinase K, the affinity-purifiable CID-cleavable and isotopically coded cross-linker cyanurbiotindipropionylsuccinimide and MALDI-MS cross-links were found for all of the possible cross-linking sites. After digestion with proteinase K, we obtained a mass distribution of the cross-linked peptides that is very suitable for MALDI-MS analysis. Using this new method, we were able to detect over 60 interpeptide cross-links in the native PrP(C) and PrPβ prion protein. The set of cross-links for the native form was used as distance constraints in developing a model of the native prion protein structure, which includes the 90-124-amino acid N-terminal portion of the protein. Several cross-links were unique to each form of the prion protein, including

  4. Testing of the Effect of Reaction Parameters on the Enzyme Immobilization by Adsorption and Cross-Linking Processes with Kinetic Desorption Method

    Directory of Open Access Journals (Sweden)

    Dániel Radva

    2011-01-01

    Full Text Available The activity of enzymes after the immobilization by weak interactions such as adsorption or adsorption followed by a cross-linking reaction can change easily not only during further application but during the activity measured via desorption and/or inactivation of enzymes. The changes in activity could be a consequence of the interactions between the enzyme and support. In this work a quick and efficient method is developed that permits studying of the strength and properties of the forces between the enzymes and support by examining the kinetics of desorption and/or inactivation. Applying this new cyclic kinetic desorption method, the effect of reaction parameters on immobilization could also be studied. The efficiency of this method was tested for optimizing the parameters for immobilization of β-glucosidase on Amberlite IRA 900 anion exchange resin by an adsorption followed by a cross-linking with glutaraldehyde to form potential preparation for food industry. The following parameters were chosen: concentration (0.10 M of the buffer (sodium acetate, pH=5.5 and the ratio of carrier to enzyme (10:1 for the adsorption step, then the time of treatment (1 min and concentration (0.25, by mass per volume of glutaraldehyde for the cross-linking by using the kinetic desorption method. The activity of this preparation was 57 μmol/(min·g in respect of dry resin. It was established that the effect of different parameters on this enzyme immobilization could be characterized by the new cyclic kinetic desorption method in a quick and efficient way; furthermore, it permitted separate testing of the effect of parameters on the adsorption and cross-linking processes.

  5. The Effect of Glutaraldehyde Cross-Linking on the Enzyme Activity of Immobilized &beta-Galactosidase on Chitosan Bead

    Directory of Open Access Journals (Sweden)

    He Chen

    2013-07-01

    Full Text Available The effect of glutaraldehyde solution concentration, cross-linking time, cross-linking pH and cross-linking temperature on the enzyme activity of the immobilized &beta-galactosidase on Chitosan beads were studied. The enzyme activity was measured after immobilized by detecting the absorbance value at 420 nm.The results were as follows: the immobilized enzyme activity reached the maximum when the concentration of glutaraldehyde solution was 0.3%.The immobilized enzyme had optimal cross-linking time of 3h, optimal cross-linking pH of 6.5, optimal cross-linking temperature of 25°C, under these conditions, the immobilized enzyme activity reached 101, 96, 90 U/g, respectively.

  6. Physicochemical properties and micro-structural characteristics in starch from kudzu root as affected by cross-linking.

    Science.gov (United States)

    Chen, Boru; Dang, Leping; Zhang, Xiao; Fang, Wenzhi; Hou, Mengna; Liu, Tiankuo; Wang, Zhanzhong

    2017-03-15

    Kudzu starch was cross-linked with sodium trimetaphosphate (STMP) at different temperatures, time and of STMP concentrations in this work. The cross-linked starches (CLSs) were fractionated further into cross-linked amylose and amylopectin in order to compare the effect of cross-linking on the microstructure. According to scanning electron microscope (SEM), CLSs displayed the resemble appearance of spherical and polygonal shapes like NS. X-ray diffraction (XRD) revealed that amylose of native starch (A), NS and CLS displayed a combination of A-type and B-type structure, while that was not found in amylose of cross-linked starch (CLA). The deconvoluted fourier transform infrared (FT-IR) indicated that crystal structure of kudzu starch was losing with the proceeding of cross-linking reaction. The CLSs exhibited a higher retrogradation and freeze-thaw stability than NS. This was accompanied by a significant decrease in sedimentation, transparency, swelling power and solubility.

  7. Elevated carboxy terminal cross linked telopeptide of type I collagen in alcoholic cirrhosis

    DEFF Research Database (Denmark)

    Møller, S; Hansen, M; Hillingsø, Jens

    1999-01-01

    BACKGROUND: The carboxy terminal cross linked telopeptide of type I collagen (ICTP) has been put forward as a marker of bone resorption. Patients with alcoholic liver disease may have osteodystrophy. AIMS: To assess circulating and regional concentrations of ICTP in relation to liver dysfunction...

  8. TGFβ affects collagen cross-linking independent of chondrocyte phenotype but strongly depending on physical environment

    NARCIS (Netherlands)

    Bastiaansen-Jenniskens, Y.M.; Koevoet, W.; Bart, A.C.W. de; Zuurmond, A.-M.; Bank, R.A.; Verhaar, J.A.N.; Groot, J. de; Osch, G.J.V.M. van

    2008-01-01

    Transforming growth factor beta (TGFβ) is often used in cartilage tissue engineering to increase matrix formation by cells with various phenotypes. However, adverse effects of TGFβ, such as extensive cross-linking in cultured fibroblasts, have also been reported. Our goal was to study effects of

  9. Ionically cross-linked hyaluronic acid: wetting, lubrication, and viscoelasticity of a modified adhesion barrier gel

    Directory of Open Access Journals (Sweden)

    Katherine Vorvolakos

    2010-12-01

    Full Text Available Katherine Vorvolakos1, Irada S Isayeva1, Hoan-My Do Luu1, Dinesh V Patwardhan1, Steven K Pollack21Division of Chemistry and Material Science, 2Office of Science and Engineering Laboratories, Center for Devices and Radiological Health, Food and Drug Administration, Silver Spring, MD, USAAbstract: Hyaluronic acid (HA, in linear or cross-linked form, is a common component of cosmetics, personal care products, combination medical products, and medical devices. In all cases, the ability of the HA solution or gel to wet surfaces and/or disrupt and lubricate interfaces is a limiting feature of its mechanism of action. We synthesized ferric ion–cross-linked networks of HA based on an adhesion barrier, varied the degree of cross-linking, and performed wetting goniometry, viscometry, and dynamic mechanical analysis. As cross-linking increases, so do contact angle, viscosity, storage modulus, and loss modulus; thus, wetting and lubrication are compromised. These findings have implications in medical device materials, such as adhesion barriers and mucosal drug delivery vehicles.Keywords: hyaluron, adhesion barrier, wetting, contact angle, viscosity, lubrication, elasticity, viscoelastic, hydrogel, ferric

  10. ROMP-based thermosetting polymers from modified castor oil with various cross-linking agents

    Science.gov (United States)

    Ding, Rui

    Polymers derived from bio-renewable resources are finding an increase in global demand. In addition, polymers with distinctive functionalities are required in certain advanced fields, such as aerospace and civil engineering. In an attempt to meet both these needs, the goal of this work aims to develop a range of bio-based thermosetting matrix polymers for potential applications in multifunctional composites. Ring-opening metathesis polymerization (ROMP), which recently has been explored as a powerful method in polymer chemistry, was employed as a unique pathway to polymerize agricultural oil-based reactants. Specifically, a novel norbornyl-functionalized castor oil alcohol (NCA) was investigated to polymerize different cross-linking agents using ROMP. The effects of incorporating dicyclopentadiene (DCPD) and a norbornene-based crosslinker (CL) were systematically evaluated with respect to curing behavior and thermal mechanical properties of the polymers. Isothermal differential scanning calorimetry (DSC) was used to investigate the conversion during cure. Dynamic DSC scans at multiple heating rates revealed conversion-dependent activation energy by Ozawa-Flynn-Wall analysis. The glass transition temperature, storage modulus, and loss modulus for NCA/DCPD and NCA/CL copolymers with different cross-linking agent loading were compared using dynamic mechanical analysis. Cross-link density was examined to explain the very different dynamic mechanical behavior. Mechanical stress-strain curves were developed through tensile test, and thermal stability of the cross-linked polymers was evaluated by thermogravimetric analysis to further investigate the structure-property relationships in these systems.

  11. Temperature dependence of creep compliance of highly cross-linked epoxy: A molecular simulation study

    Energy Technology Data Exchange (ETDEWEB)

    Khabaz, Fardin, E-mail: rajesh.khare@ttu.edu; Khare, Ketan S., E-mail: rajesh.khare@ttu.edu; Khare, Rajesh, E-mail: rajesh.khare@ttu.edu [Department of Chemical Engineering, Texas Tech University, Lubbock, TX 79409 (United States)

    2014-05-15

    We have used molecular dynamics (MD) simulations to study the effect of temperature on the creep compliance of neat cross-linked epoxy. Experimental studies of mechanical behavior of cross-linked epoxy in literature commonly report creep compliance values, whereas molecular simulations of these systems have primarily focused on the Young’s modulus. In this work, in order to obtain a more direct comparison between experiments and simulations, atomistically detailed models of the cross-linked epoxy are used to study their creep compliance as a function of temperature using MD simulations. The creep tests are performed by applying a constant tensile stress and monitoring the resulting strain in the system. Our results show that simulated values of creep compliance increase with an increase in both time and temperature. We believe that such calculations of the creep compliance, along with the use of time temperature superposition, hold great promise in connecting the molecular insight obtained from molecular simulation at small length- and time-scales with the experimental behavior of such materials. To the best of our knowledge, this work is the first reported effort that investigates the creep compliance behavior of cross-linked epoxy using MD simulations.

  12. Grafted Cross-Linked Polyolefin Substrates for Peptide Synthesis and Assays

    DEFF Research Database (Denmark)

    1999-01-01

    suited for use in solid-phase biosystems, notably bioassays, such as immunoassays, DNA hybridization assays or PCR amplification. The grafted chains may bear substituents which are such that the polymer-grafted cross-linked polyolefin substrate is swellable by water or aqueous media, in other words...

  13. Mocaf cross-linking with gluten to improve the quality of mocaf dough

    Science.gov (United States)

    Raharja, Sapta; Udin, Faqih; Suparno, Ono; Febrianti, Faricha Helfi; Nuraisyah, Ani

    2017-03-01

    Crosslink between mocaf and gluten is conducted to increase the using of mocaf which has very big potential in Indonesia. The effort of cross-linking between mocaf and gluten is to get mocaf flour with better dough quality. This study aims to produce a cross-linked mocaf-gluten flour and to evaluate the influence of heating temperature (X1) and the addition of gluten concentration (X2) using completely randomized design factorial (RAFL). The cross-linking is carried out in alkaline solution with 10%, 20%, and 30% gluten addition and heating temperature at 50, 55, and 60 °C. The result showed that mocaf - gluten flour with the treatment of 30% gluten addition at 55 °C had the largest amount of protein and baking expansion (i.e 19.77% and 2.78 mL/g). Swelling power of the flour was increasing along with the increasing of water absorbing capacity of the mocaf - gluten flour. Birefringence properties of mocaf - gluten flour tended to be reduced as the increasing heating temperature. FTIR analysis of mocaf - gluten flour showed that there was peak strengthening of the infrared spectrum of the C - N bond at 1167-1159 cm-1 which was presumably resulted from the gluten addition and the cross-linking properties.

  14. A minimal model for stabilization of biomolecules by hydrocarbon cross-linking

    Science.gov (United States)

    Hamacher, K.; Hübsch, A.; McCammon, J. A.

    2006-04-01

    Programmed cell death regulating protein motifs play an essential role in the development of an organism, its immune response, and disease-related cellular mechanisms. Among those motifs the BH3 domain of the BCL-2 family is found to be of crucial importance. Recent experiments showed how the isolated, otherwise unstructured BH3 peptide can be modified by a hydrocarbon linkage to regain function. We parametrized a reduced, dynamic model for the stability effects of such covalent cross-linking and confirmed that the model reproduces the reinforcement of the structural stability of the BH3 motif by cross-linking. We show that an analytically solvable model for thermostability around the native state is not capable of reproducing the stabilization effect. This points to the crucial importance of the peptide dynamics and the fluctuations neglected in the analytic model for the cross-linking system to function properly. This conclusion is supported by a thorough analysis of a simulated Gō model. The resulting model is suitable for rational design of generic cross-linking systems in silicio.

  15. Sensitizing potential of enzymatically cross-linked peanut proteins in a mouse model of peanut allergy.

    NARCIS (Netherlands)

    Smit, Joost|info:eu-repo/dai/nl/250600706

    2014-01-01

    SCOPE: The cross-linking of proteins by enzymes to form high-molecular-weight protein, aggregates can be used to tailor the technological or physiological functionality of food products. Aggregation of dietary proteins by food processing may promote allergic sensitization, but the effects of enzymat

  16. Polymers and Cross-Linking: A CORE Experiment to Help Students Think on the Submicroscopic Level

    Science.gov (United States)

    Bruce, Mitchell R. M.; Bruce, Alice E.; Avargil, Shirly; Amar, Francois G.; Wemyss, Thomas M.; Flood, Virginia J.

    2016-01-01

    The Polymers and Cross-Linking experiment is presented via a new three phase learning cycle: CORE (Chemical Observations, Representations, Experimentation), which is designed to model productive chemical inquiry and to promote a deeper understanding about the chemistry operating at the submicroscopic level. The experiment is built on two familiar…

  17. Substituent distribution within cross-linked and hydroxypropylated sweet potato starch and potato starch

    NARCIS (Netherlands)

    Zhao, J.; Schols, H.A.; Chen Zenghong,; Jin Zhengyu,; Buwalda, P.L.; Gruppen, H.

    2012-01-01

    Revealing the substituents distribution within starch can help to understand the changes of starch properties after modification. The distribution of substituents over cross-linked and hydroxypropylated sweet potato starch was investigated and compared with modified potato starch. The starches were

  18. EVA交联机理的研究%The Research of EVA Cross-linking Mechanism

    Institute of Scientific and Technical Information of China (English)

    王川艳; 苑会林

    2011-01-01

    研究了过氧化二异丙苯(DCP)对乙烯-醋酸乙烯共聚物(EVA)交联的影响,分析交联过程的反应机理.对交联的EVA样品进行紫外光辐照,分析在该过程中所发生的反应,并研究加入紫外线吸收剂2-羟基-4-正辛氧基-二苯甲酮(UV-531)后,对交联EVA样品在紫外光辐照下交联的影响.%The effect of peroxide (DCP) on Ethylene-Vinyl Acetate (EVA) cross-linking were studied, the reaction mechanism of EVA cross-linking were analyzed. Upon the exposure of cross-linked EVA samples to ultraviolet light, the reaction during this process were analyzed, and also, after adding the ultraviolet absorber (UV-531) , the influences to cross-linked EVA samples during the ultraviolet radiation process were researched.

  19. Dynamic Heterogeneity in Highly Cross-linked Epoxy in the Vicinity of Glass Transition

    Science.gov (United States)

    Lin, Po-Han; Khare, Rajesh

    2010-03-01

    Cross-linked epoxy has been widely used in aerospace and electronics industries. The highly cross-linked nature of these systems leads to different chain dynamics as compared to the linear polymeric systems. In this work, we have used molecular dynamics (MD) simulations to study the dynamic heterogeneity in cross-linked epoxy near the glass transition temperature. Well-relaxed atomistic models of cross-linked epoxy were first created by employing the simulated annealing polymerization approach. The specific epoxy system studied consisted of diglycidyl ether of bisphenol-A (DGEBA) as the epoxy monomer and trimethylene glycol di-p-aminobenzoate (TMAB) as the cross-linker. The glass transition temperature of these model structures was determined from MD simulation by monitoring their volume-temperature behaviour in a stepwise cooling run. The chain dynamics of these systems were characterized by their local translational and orientational mobility. Furthermore, dynamic heterogeneity was studied by analyzing the spatial distribution of the mobile and immobile atoms in the system near the glass transition temperature.

  20. Laccase-Based CLEAs: Chitosan as a Novel Cross-Linking Agent

    Directory of Open Access Journals (Sweden)

    Alexandre Arsenault

    2011-01-01

    Full Text Available Laccase from Coriolopsis Polyzona was insolubilized as cross-linked enzyme aggregates (CLEAs for the first time with chitosan as the cross-linking agent. Concentrations between 0.01 and 1.867 g/L of chitosan were used and between 0.05 and 600 mM of 1-ethyl-3-(3-dimethylaminopropylcarbodiimide hydrochloride. The laccase was precipitated using ammonium sulphate and cross-linked simultaneously. Specific activity and thermal stability of these biocatalysts were measured. Activities of up to 737 U/g were obtained when 2,2-azino-bis-(3-ethylbenzthiazoline-6-sulfonic acid (ABTS was used as a substrate. Moreover, the stability of these biocatalysts was improved with regards to thermal degradation compared to free laccase when exposed to denaturing conditions of high temperature and low pH. The CLEAs stability against chemical denaturants was also tested but no significant improvement was detected. The total amount of ABTS to be oxidized during thermal degradation by CLEAs and free laccase was calculated and the insolubilized enzymes were reported to oxidize more substrate than free laccase. The formation conditions were analyzed by response surface methodology in order to determine an optimal environment for the production of efficient laccase-based CLEAs using chitosan as the cross-linking agent. After 24 hours of formation at pH 3 and at 4°C without agitation, the CLEAs exhibit the best specific activity.

  1. Standard and hypoosmolar corneal cross-linking in various pachymetry groups

    NARCIS (Netherlands)

    Soeters, Nienke; Tahzib, Nayyirih G

    2015-01-01

    PURPOSE: To investigate the influence of corneal thickness on the outcome of corneal cross-linking (CXL) for progressive keratoconus. METHODS: In this cohort study, 72 unilateral eyes were treated by CXL and divided into three groups according to central corneal thickness (CCT) measured by ultrasoun

  2. The peptidoglycan of Mycobacterium abscessus is predominantly cross-linked by L,D-transpeptidases.

    Science.gov (United States)

    Lavollay, Marie; Fourgeaud, Martine; Herrmann, Jean-Louis; Dubost, Lionel; Marie, Arul; Gutmann, Laurent; Arthur, Michel; Mainardi, Jean-Luc

    2011-02-01

    Few therapeutic alternatives remain for the treatment of infections due to multiresistant Mycobacterium abscessus. Here we show that the peptidoglycans of the "rough" and "smooth" morphotypes contain predominantly 3→3 cross-links generated by l,d-transpeptidases, indicating that these enzymes are attractive targets for the development of efficient drugs.

  3. Cross-linking Electrospun Polydioxanone-Soluble Elastin Blends: Material Characterization

    Directory of Open Access Journals (Sweden)

    Michael J. McClure

    2008-03-01

    Full Text Available The purpose of this study was to establish whether material properties of elastin co-electrospun with polydioxanone (PDO would change over time in both the uncross-linked state and the cross-linked state. First, uncross-linked scaffolds were placed in phosphate buffered saline (PBS for three separate time periods: 15 minutes, 1 hour, and 24 hours, and subsequently tested using uniaxial materials testing. Several cross-linking reagents were then investigated to verify their ability to crosslink elastin: 1-ethyl-3-(dimethylaminopropyl-carbodiimide (EDC, ethylene glycol diglycidyl ether (EGDE, and genipin. Uniaxial tensile testing was performed on scaffolds cross-linked with EDC and genipin, yielding results that warranted further investigation for PDO-elastin blends. Material properties of the cross-linked scaffolds were then found within range of both pig femoral artery and human femoral artery. These results demonstrate PDO-elastin blends could potentially be favorable as vascular grafts, thus warranting future in vitro and in vivo studies.

  4. Is dialdehyde starch a valuable cross-linking agent for collagen/elastin based materials?

    Science.gov (United States)

    Skopinska-Wisniewska, J; Wegrzynowska-Drzymalska, K; Bajek, A; Maj, M; Sionkowska, A

    2016-04-01

    Collagen and elastin are the main structural proteins in mammal bodies. They provide mechanical support, strength, and elasticity to various organs and tissues, e.g. skin, tendons, arteries, and bones. They are readily available, biodegradable, biocompatible and they stimulate cell growth. The physicochemical properties of collagen and elastin-based materials can be modified by cross-linking. Glutaraldehyde is one of the most efficient cross-linking agents. However, the unreacted molecules can be released from the material and cause cytotoxic reactions. Thus, the aim of our work was to investigate the influence of a safer, macromolecular cross-linking agent--dialdehyde starch (DAS). The properties of hydrogels based on collagen/elastin mixtures (95/5, 90/10) containing 5 and 10% of DAS and neutralized via dialysis against deionized water were tested. The homogenous, transparent, stiff hydrogels were obtained. The DAS addition causes the formation of intermolecular cross-linking bonds but does not affect the secondary structure of the proteins. As a result, the thermal stability, mechanical strength, and, surprisingly, swelling ability increased. At the same time, the surface properties test and in vitro study show that the materials are attractive for 3T3 cells. Moreover, the materials containing 10% of DAS are more resistant to enzymatic degradation.

  5. Corneal Cross-Linking for Pediatric Keratoconus : Long-Term Results

    NARCIS (Netherlands)

    Godefrooij, Daniel A; Soeters, Nienke; Imhof, Saskia M; Wisse, Robert P L

    2016-01-01

    PURPOSE: To assess the efficacy and safety of cross-linking in pediatric patients with keratoconus and to provide a systematic literature overview regarding this subject. METHODS: In this prospective cohort, 54 eyes of 36 pediatric patients with keratoconus underwent standard epithelium-off cross-li

  6. Detection of DNA cross-links in tumor cells with the ethidium bromide fluorescence assay

    NARCIS (Netherlands)

    de Jong, Steven; Zijlstra, J G; Timmer-Bosscha, H; Mulder, N H; de Vries, Liesbeth

    1986-01-01

    Until now the fluorescence assay with ethidium bromide has only been used on pure DNA. This assay depends on the difference in fluorescence between single- and double-stranded DNA (dsDNA). Cross-links in DNA are measured by the return of fluorescence of dsDNA after heat denaturation at pH 12. Under

  7. Cross-linking methods of electrospun fibrinogen scaffolds for tissue engineering applications

    Energy Technology Data Exchange (ETDEWEB)

    Sell, Scott A; Garg, Koyal; McClure, Michael J; Bowlin, Gary L [Department of Biomedical Engineering, Virginia Commonwealth University, Richmond, VA 23284-3067 (United States); Francis, Michael P [Department of Pathology, Virginia Commonwealth University, Richmond, VA 23298-0709 (United States); Simpson, David G [Department of Anatomy and Neurobiology, Virginia Commonwealth University, Richmond, VA 23298-0709 (United States)], E-mail: glbowlin@vcu.edu

    2008-12-15

    The purpose of this study was to enhance the mechanical properties and slow the degradation of an electrospun fibrinogen scaffold, while maintaining the scaffold's high level of bioactivity. Three different cross-linkers were used to achieve this goal: glutaraldehyde vapour, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) in ethanol and genipin in ethanol. Scaffolds with a fibrinogen concentration of 120 mg ml{sup -1} were electrospun and cross-linked with one of the aforementioned cross-linkers. Mechanical properties were determined through uniaxial tensile testing performed on scaffolds incubated under standard culture conditions for 1 day, 7 days and 14 days. Cross-linked scaffolds were seeded with human foreskin fibroblasts (BJ-GFP-hTERT) and cultured for 7, 14 and 21 days, with histology and scanning electron microscopy performed upon completion of the time course. Mechanical testing revealed significantly increased peak stress and modulus values for the EDC and genipin cross-linked scaffolds, with significantly slowed degradation. However, cross-linking with EDC and genipin was shown to have some negative effect on the bioactivity of the scaffolds as cell migration throughout the thickness of the scaffold was slowed.

  8. Mature enzymatic collagen cross-links, hydroxylysylpyridinoline and lysylpyridinoline, in the aging human vitreous

    NARCIS (Netherlands)

    Ponsioen, T.L.; van Deemter, M.; Bank, R.A.; Snabel, J.M.; Zijlstra, G.S.; van der Worp, R.J.; Hooymans, J.M.M.; Los, L.I.

    2009-01-01

    Purpose. The vitreous body of the human eye undergoes progressive morphologic changes with aging. Since the enzymatic collagen cross-links hydroxylysylpyridinoline (HP) and lysylpyridinoline (LP) are known to be important for the integrity of the collagen matrix, the presence in the vitreous on agin

  9. Mature Enzymatic Collagen Cross-Links, Hydroxylysylpyridinoline and Lysylpyridinoline, in the Aging Human Vitreous

    NARCIS (Netherlands)

    Ponsioen, Theodorus L.; van Deemter, Marielle; Bank, Rudolf A.; Snabel, Johanna M.; Zijlstra, Gerrit S.; van der Worp, Roelofje J.; Hooymans, Johanna M. M.; Los, Leonoor I.

    2009-01-01

    PURPOSE. The vitreous body of the human eye undergoes progressive morphologic changes with aging. Since the enzymatic collagen cross-links hydroxylysylpyridinoline (HP) and lysylpyridinoline (LP) are known to be important for the integrity of the collagen matrix, the presence in the vitreous on agin

  10. Formation and Distribution of Space-Charge in Cross-Linked Polyethylene

    Science.gov (United States)

    Zhang, Ye-Wen; Li, Ji-Xiao; Zheng, Fei-Hu; Peng, Zong-Ren; Wu, Chang-Shun; Xia, Zhong-Fu

    2002-08-01

    The formation and distribution of space-charge in a cross-linked polyethylene (XLPE) sample are investigated by means of pressure wave propagation, infrared spectroscopy and electrostatic force microscopy (EFM). The related mechanism of space-charge distribution and the structure of XLPE are discussed. The EFM images show that quite large quantitative space-charges locate at the surface of spherulites.

  11. Crown ether activation of cross-linked subtilisin Carlsberg crystals in organic solvents

    NARCIS (Netherlands)

    Unen, van Dirk-Jan; Sakodinskaya, Inna K.; Engbersen, Johan F.J.; Reinhoudt, David N.

    1998-01-01

    The activity of cross-linked subtilisin Carlsberg crystals in the catalysis of peptide bond formation can be significantly enhanced by pretreatment of the enzyme crystals with crown ethers. Soaking of the enzyme crystals in a solution of crown ether in acetonitrile followed by evaporation of the sol

  12. Phosphoric acid doped polysulfone membranes with aminopyridine pendant groups and imidazole cross-links

    DEFF Research Database (Denmark)

    Hink, Steffen; Elsøe, Katrine; Cleemann, Lars Nilausen;

    2015-01-01

    Udel polysulfone based membranes with 4-aminopyridine pendant groups and cross-linking imidazole units are synthesized in a simple two step reaction. The ratio of 4-aminopyridine and imidazole is varied and the materials are extensively characterized. The average phosphoric acid uptake (in 85 wt...

  13. Effect of dual modification with hydroxypropylation and cross-linking on physicochemical properties of taro starch.

    Science.gov (United States)

    Hazarika, Bidyut Jyoti; Sit, Nandan

    2016-04-20

    Dual modification of taro starch by hydroxypropylation and cross-linking was carried out and the properties of the modified starches were investigated. Two different levels of hydroxypropylation (5 and 10%) and cross-linking (0.05 and 0.10%) were used in different sequences. The amylose contents of the starch decreased due to single and dual modification. For the dual-modified starches, the swelling, solubility and clarity was found to increase with level of hydroxypropylation and decrease with level of cross-linking. The freeze-thaw stability of the dual-modified starches was also affected by the sequence of modification. The viscosities of the cross-linked and dual-modified starches were more than native and hydroxypropylated starches. The firmness of the dual-modified starches was also higher than native and single modified starches. The dual-modified starches have benefits of both type of modifications and could be used for specific purposes e.g. food products requiring high viscosity as well as freeze-thaw stability.

  14. Vitamin E diffused highly cross-linked polyethylene in total hip arthroplasty at five years

    DEFF Research Database (Denmark)

    Nebergall, Audrey K; Greene, M. E.; Laursen, M B

    2017-01-01

    AIMS: The objective of this five-year prospective, blinded, randomised controlled trial (RCT) was to compare femoral head penetration into a vitamin E diffused highly cross-linked polyethylene (HXLPE) liner with penetration into a medium cross-linked polyethylene control liner using radiostereome......AIMS: The objective of this five-year prospective, blinded, randomised controlled trial (RCT) was to compare femoral head penetration into a vitamin E diffused highly cross-linked polyethylene (HXLPE) liner with penetration into a medium cross-linked polyethylene control liner using...... radiostereometric analysis. PATIENTS AND METHODS: Patients scheduled for total hip arthroplasty (THA) were randomised to receive either the study E1 (32 patients) or the control ArComXL polyethylene (35 patients). The median age (range) of the overall cohort was 66 years (40 to 76). RESULTS: The five-year median...... (interquartile range) proximal femoral head penetration into the E1 was -0.05 mm (-0.13 to -0.02) and 0.07 mm (-0.03 to 0.16) for ArComXL. At three and five years, the penetration was significantly greater in the ArComXL group compared with the E1 group (p = 0.029 and p = 0.019, respectively). All patient...

  15. Biomimetic acellular detoxified glutaraldehyde cross-linked bovine pericardium for tissue engineering.

    Science.gov (United States)

    Mathapati, Santosh; Bishi, Dillip Kumar; Guhathakurta, Soma; Cherian, Kotturathu Mammen; Venugopal, Jayarama Reddy; Ramakrishna, Seeram; Verma, Rama Shanker

    2013-04-01

    Glutaraldehyde (GLUT) processing, cellular antigens, calcium ions in circulation, and phospholipids present in the native tissue are predominantly responsible for calcification, degeneration, and lack of natural microenvironment for host progenitor cell migration in tissue implants. The study presents an improved methodology for adhesion and proliferation of endothelial progenitor cells (EPCs) without significant changes in biomechanical and biodegradation properties of the processed acellular bovine pericardium. The anti-calcification potential of the processed tissue was enhanced by detoxification of GLUT-cross-linked bovine pericardium by decellularization, pretreating it with ethanol or removing the free aldehydes by citric acid treatment and lyophilization. The treated tissues were assessed for biomechanical properties, GLUT ligand quantification, adhesion, proliferation of EPCs, and biodegradability. The results indicate that there was no significant change in biomechanical properties and biodegradability when enzymatic hydrolysis (p>0.05) is employed in detoxified acellular GLUT cross-linked tissue (DBP-G-CA-ET), compared with the native detoxified GLUT cross-linked bovine pericardium (NBP-G-CA-ET). DBP-G-CA-ET exhibited a significant (p>0.05) increase in the viability of EPCs and cell adhesion as compared to acellular GLUT cross-linked bovine pericardium (ppericardium, employed in our study as an alternative to conventional GLUT cross-linked bovine pericardium, might provide longer durability and better biocompatibility, and reduce calcification. The developed bovine pericardium patches could be used in cardiac reconstruction and repair, arteriotomy, soft tissue repair, and general surgical procedures with tissue regeneration dimensions. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Wear measurement of highly cross-linked UHMWPE using a 7Be tracer implantation technique.

    Science.gov (United States)

    Wimmer, Markus A; Laurent, Michel P; Dwiwedi, Yasha; Gallardo, Luis A; Chipps, Kelly A; Blackmon, Jeffery C; Kozub, Raymond L; Bardayan, Daniel W; Gross, Carl J; Stracener, Daniel W; Smith, Michael S; Nesaraja, Caroline D; Erikson, Luke; Patel, Nidhi; Rehm, Karl E; Ahmad, Irshad; Greene, John P; Greife, Uwe

    2013-04-01

    The very low wear rates achieved with the current highly cross-linked ultrahigh molecular weight polyethylenes (UHMWPE) used in joint prostheses have proven to be difficult to measure accurately by gravimetry. Tracer methods are therefore being explored. The purpose of this study was to perform a proof-of-concept experiment on the use of the radioactive tracer beryllium-7 ((7)Be) for the determination of in vitro wear in a highly cross-linked orthopedic UHMWPE. Three cross-linked and four conventional UHMWPE pins made from compression-molded GUR 1050, were activated with 10(9) to 10(10) (7)Be nuclei using a new implantation setup that produced a homogenous distribution of implanted nuclei up to 8.5 μm below the surface. The pins were tested for wear in a six-station pin-on-flat apparatus for up to 7.1 million cycles (178 km). A Germanium gamma detector was employed to determine activity loss of the UHMWPE pins at preset intervals during the wear test. The wear of the cross-linked UHMWPE pins was readily detected and estimated to be 17 ± 3 μg per million cycles. The conventional-to-cross-linked ratio of the wear rates was 13.1 ± 0.8, in the expected range for these materials. Oxidative degradation damage from implantation was negligible; however, a weak dependence of wear on implantation dose was observed limiting the number of radioactive tracer atoms that can be introduced. Future applications of this tracer technology may include the analysis of location-specific wear, such as loss of material in the post or backside of a tibial insert.

  17. Cyclodextrin/dextran based hydrogels prepared by cross-linking with sodium trimetaphosphate.

    Science.gov (United States)

    Wintgens, Véronique; Lorthioir, Cédric; Dubot, Pierre; Sébille, Bernard; Amiel, Catherine

    2015-11-01

    Novel βCD-based hydrogels have been synthesized using sodium trimetaphosphate (STMP) as non-toxic reagent. Straightforward mixing of βCD with dextran and STMP in basic aqueous media led to hydrogels incorporating dextran chains, phosphate groups and βCD units. The hydrogels have been characterized by swelling measurements, XPS and (31)P NMR. The swelling ratio was correlated to the content in phosphated groups, which give a polyelectrolyte character to these hydrogels. The significant rise of the swelling ratio with the βCD content increase has been attributed to a decrease of the number of phosphate-based crosslinks, the βCD units playing the role of dangling ends in the tridimensional network. Their loading capacity and their release properties have been investigated for methylene blue and benzophenone in order to demonstrate their potentiality for drug delivery. Through different interaction mechanisms, electrostatic and inclusion complex interactions, these compounds are loaded with different efficiencies. The release involves deswelling, diffusion mechanisms and partition equilibrium.

  18. A robust way to prepare blood-compatible and anti-fouling polyethersulfone membrane.

    Science.gov (United States)

    Xie, Yi; Wang, Rui; Li, Shuangsi; Xiang, Tao; Zhao, Chang-Sheng

    2016-10-01

    Functional copolymers were successfully grafted onto polyethersulfone (PES) membrane surfaces by free radical mechanism using ammonium persulfate (APS) as an initiator. The anti-coagulant and anti-fouling properties of the membranes were well controlled by changing the functional copolymer compositions. Attenuated total reflection-Fourier transforminfrared (ATR-FTIR), X-ray photoelectron spectrometer spectrum (XPS), water contact angles (WCAs), and scanning electron microscopy (SEM) images were used to characterize the membranes. The results of protein adsorption, clotting times, platelet adhesion and bacteria attachment indicated that the membranes had good blood-compatibility and/or anti-fouling ability. Meanwhile, the modification didn't cause an adverse effect on the membrane permeability. This new method provides a general, robust and flexible way to adjust membrane surface performance and potentially has wide applications.

  19. Microencapsulation of Lactobacillus rhamnosus GG by Transglutaminase Cross-Linked Soy Protein Isolate to Improve Survival in Simulated Gastrointestinal Conditions and Yoghurt.

    Science.gov (United States)

    Li, Chun; Wang, Chun-Ling; Sun, Yu; Li, Ai-Li; Liu, Fei; Meng, Xiang-Chen

    2016-07-01

    Microencapsulation is an effective way to improve the survival of probiotics in simulated gastrointestinal (GI) conditions and yoghurt. In this study, microencapsulation of Lactobacillus rhamnosus GG (LGG) was prepared by first cross-linking of soy protein isolate (SPI) using transglutaminase (TGase), followed by embedding the bacteria in cross-linked SPI, and then freeze-drying. The survival of microencapsulated LGG was evaluated in simulated GI conditions and yoghurt. The results showed that a high microencapsulation yield of 67.4% was obtained. The diameter of the microencapsulated LGG was in the range of 52.83 to 275.16 μm. Water activity did not differ between free and microencapsulated LGG after freeze-drying. The survival of microencapsulated LGG under simulated gastric juice (pH 2.5 and 3.6), intestinal juice (0.3% and 2% bile salt) and storage at 4 °C were significantly higher than that of free cells. The survival of LGG in TGase cross-linked SPI microcapsules was also improved to 14.5 ± 0.5% during storage in yoghurt. The microencapsulation of probiotics by TGase-treated SPI can be a suitable alternative to polysaccharide gelation technologies. © 2016 Institute of Food Technologists®

  20. Synthesis and Characterization of Chemically Cross-Linked Acrylic Acid/Gelatin Hydrogels: Effect of pH and Composition on Swelling and Drug Release

    Directory of Open Access Journals (Sweden)

    Syed Majid Hanif Bukhari

    2015-01-01

    Full Text Available This present work was aimed at synthesizing pH-sensitive cross-linked AA/Gelatin hydrogels by free radical polymerization. Ammonium persulfate and ethylene glycol dimethacrylate (EGDMA were used as initiator and as cross-linking agent, respectively. Different feed ratios of acrylic acid, gelatin, and EGDMA were used to investigate the effect of monomer, polymer, and degree of cross-linking on swelling and release pattern of the model drug. The swelling behavior of the hydrogel samples was studied in 0.05 M USP phosphate buffer solutions of various pH values pH 1.2, pH 5.5, pH 6.5, and pH 7.5. The prepared samples were evaluated for porosity and sol-gel fraction analysis. Pheniramine maleate used for allergy treatment was loaded as model drug in selected samples. The release study of the drug was investigated in 0.05 M USP phosphate buffer of varying pH values (1.2, 5.5, and 7.5 for 12 hrs. The release data was fitted to various kinetic models to study the release mechanism. Hydrogels were characterized by Fourier transformed infrared (FTIR spectroscopy which confirmed formation of structure. Surface morphology of unloaded and loaded samples was studied by surface electron microscopy (SEM, which confirmed the distribution of model drug in the gel network.