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Sample records for n-methylene phosphonic chitosan

  1. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  2. Preparation of Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) Material and its Application to Electrochemical Degradation of Methylene Blue in Sodium Chloride Solution

    Science.gov (United States)

    Riyanto; Prawidha, A. D.

    2018-01-01

    Electrochemical degradation of methylene blue using Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) electrode in sodium chloride have been done. The aim of this work was to degradation of methylene blue using Carbon-Chitosan-Polyvinyl Chloride (CC-PVC). Carbon chitosan composite electrode was preparing by Carbon and Chitosan powder and PVC in 4 mL tetrahydrofuran (THF) solvent and swirled flatly to homogeneous followed by drying in an oven at 100 °C for 3 h. The mixture was placed in stainless steel mould and pressed at 10 ton/cm2. Sodium chloride was used electrolyte solution. The effects of the current and electrolysis time were investigated using spectrophotometer UV-Visible. The experimental results showed that the carbon-chitosan composite electrode have higher effect in the electrochemical degradation of methylene blue in sodium chloride. Based on UV-visible spectra analysis shows current and electrolysis time has high effect to degradation of methylene blue in sodium chloride. Chitosan and polyvinyl chloride can strengthen the bond between the carbons so that the material has the high stability and conductivity. As conclusions is Carbon-Chitosan-Polyvinyl Chloride (CC-PVC) electrode have a high electrochemical activity for degradation of methylene blue in sodium chloride.

  3. The use of chemical modified chitosan with succinic anhydride in the methylene blue adsorption

    International Nuclear Information System (INIS)

    Lima, Ilauro S.; Ribeiro, Emerson S.; Airoldi, Claudio

    2006-01-01

    The adsorption capacity of a-chitosan and its modified form with succinic anhydride was compared with the traditional adsorbent active carbon by using the dye methylene blue, employed in the textile industry. The isotherms for both biopolymers were classified as SSA systems in the Giles model, more specifically in L class and subgroup 3. The dye concentration in the supernatant in the adsorption assay was determined through electronic spectroscopy. By calorimetric titration thermodynamic data of the interaction between methylene blue and the chemically modified chitosan at the solid/liquid interface were obtained. The enthalpy of the dye/chitosan interaction gave 2.47 ± 0.02 kJ mol-1 with an equilibrium constant of 7350 ± 10 and for the carbon/dye interaction this constant gave 5951 ± 8. The spontaneity of these adsorptions are reflected by the free Gibbs energies of -22.1 ± 0.4 and -21.5 ± 0.2 kJ mol-1, respectively, found for these systems. This new adsorbent derived from a natural polysaccharide is as efficient as activated carbon. However 97% of the bonded dye can be eluted by sodium chloride solution, while this same operation elutes only 42% from carbon. Chitosan is efficient in dye removal with the additional advantage of being cheap, non-toxic, biocompatible and biodegradable. (author)

  4. Size-controllable polypyrrole nanospheres synthesized in the presence of phosphorylated chitosan and their size effect in different applications

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jing; Cao, Yi; Lu, Yun, E-mail: yunlu@nju.edu.cn [Nanjing University, Department of Polymer Science and Engineering, State Key Laboratory of Coordination Chemistry, Key Laboratory of High Performance Polymer Materials and Technology of Ministry of Education, School of Chemistry and Chemical Engineering (China)

    2015-05-15

    The size-controllable polypyrrole (PPy) nanospheres are successfully synthesized by oxidative polymerization of pyrrole using N-methylene phosphonic chitosan (NMPC) as a structure-directing agent. By simply changing the amount of NMPC, the size of the PPy nanospheres can be adjusted from 190 to 50 nm in diameter. The spectrometric results suggest that the electrostatic interactions of phosphate groups in NMPC molecule with pyrrole ring might be a driving force for formation of the uniform and size-controllable PPy nanospheres. The PPy nanospheres with the diameter of 100 nm exhibit the largest capacity and a good cycling stability as electrode materials of supercapacitors. The as-prepared PPy nanospheres also can be combined with carbon dots to form composite nanospheres presenting enhanced fluorescence intensity, which show potential application in fluorescence detection.

  5. The inhibition of crystal growth of mirabilite in aqueous solutions in the presence of phosphonates

    Science.gov (United States)

    Vavouraki, A. I.; Koutsoukos, P. G.

    2016-02-01

    The formation of sodium sulfate decahydrate (Mirabilite) has been known to cause serious damages to structural materials both of modern and of historical buildings. Methods which can retard or completely suppress the development of mirabilte crystals are urgently needed especially as remedies or preventive measures for the preservation of the built cultural heritage. In the present work we present results on the effect of the presence of phosphonate compounds on the kinetics of crystal growth from aqueous supersaturated solutions at 18 °C using the seeded growth technique. The phosphonate compounds tested differed with respect to the number of ionizable phosphonate groups and with respect to the number of amino groups in the respective molecules. The crystal growth process was monitored by the temperature changes during the exothermic crystallization of mirabilite in the stirred supersaturated solutions. The crystal growth of mirabilite in the presence of: (1-hydroxyethylidene)-1, 1-diphosphonic acid (HEDP), amino tri (methylene phosphonic acid) (ATMP), hexamethylenediaminetetra (methylene)phosphonic acid (HTDMP), and diethylene triamine penta(methylene phosphonic acid)(DETPMP) over a range of concentrations between 0.1-5% w/w resulted in significant decrease of the rates of mirabilite crystal growth. All phosphonic compounds tested reduced the crystallization rates up to 60% in comparison with additive-free solutions. The presence of the test compounds did not cause changes of the mechanism of crystal growth which was surface diffusion controlled, as shown by the second order dependence of the rates of mirabilite crystal growth on the relative supersaturation. The excellent fit of the measured rates to a kinetic Langmuir-type model suggested that the activity of the tested inhibitors could be attributed to the adsorption and subsequent reduction of the active crystal growth sites of the seed crystals. In all cases, the inhibitory activity was reduced with

  6. Synthesis of Ethylene diamine tetra methylene phosphonic acid EDTMP

    International Nuclear Information System (INIS)

    Assaad, Th.

    2009-06-01

    Ethylenediamine tetramethylene phosphonic acid (EDTMP) is one of the most widely used ligands which forms stable complexes with various radionuclides all of which have shown high bone affinity and other favorable pharmacological characteristics in biodistribution studies. The EDTMP is very important precursor in the preparation of radiopharmaceutical kits which is used in the applications for bone diagnosis and therapy was synthesized in one step with Mannich type reaction. The obtained product was fully characterized by its multi-nuclear NMR and IR spectroscopy. The purity of the product was confirmed by HPLC. (author)

  7. The use of chemical modified chitosan with succinic anhydride in the methylene blue adsorption; O emprego de quitosana quimicamente modificada com anidrido succinico na adsorcao de azul de metileno

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Ilauro S.; Ribeiro, Emerson S.; Airoldi, Claudio [Universidade Estadual de Campinas, SP (Brazil). Inst. de Quimica]. E-mail: airoldi@iqm.unicamp.br

    2006-05-15

    The adsorption capacity of a-chitosan and its modified form with succinic anhydride was compared with the traditional adsorbent active carbon by using the dye methylene blue, employed in the textile industry. The isotherms for both biopolymers were classified as SSA systems in the Giles model, more specifically iclass and subgroup 3. The dye concentration in the supernatant in the adsorption assay was determined through electronic spectroscopy. By calorimetric titration thermodynamic data of the interaction between methylene blue and the chemically modified chitosan at the solid/liquid interface were obtained. The enthalpy of the dye/chitosan interaction gave 2.47 {+-} 0.02 kJ mol-1 with an equilibrium constant of 7350 {+-} 10 and for the carbon/dye interaction this constant gave 5951 {+-} 8. The spontaneity of these adsorptions are reflected by the free Gibbs energies of -22.1 {+-} 0.4 and -21.5 {+-} 0.2 kJ mol-1, respectively, found for these systems. This new adsorbent derived from a natural polysaccharide is as efficient as activated carbon. However 97% of the bonded dye can be eluted by sodium chloride solution, while this same operation elutes only 42% from carbon. Chitosan is efficient in dye removal with the additional advantage of being cheap, non-toxic, biocompatible and biodegradable. (author)

  8. Limitations in determining enantiomeric excess of alcohols by 31 P-NMR of the phosphonate derivatives

    International Nuclear Information System (INIS)

    Laverde Junior, Antonio; Conceicao, Jelson J.A. da; Pilli, Ronaldo A.; Marsaioli, Anita J.; Miranda, Domingos S. de; Schirmer, Heiko; Meijere, Armin de

    1999-01-01

    The use of diastereomeric alcohol dialkyl-phosphonate derivatives to determine the enantiomeric excesses via 31 P-NMR signal ratios of anisochronous meso and threo isomers was successfully applied to secondary alcohols (Feringa's method). Expansion of the methodology to primary alcohols processing the hydroxyl groups tethered to the stereogenic centers by two or more methylene groups proved the method to be inefficient. The comparison between the coupled and decoupled spectra is important in order to identify the signals corresponding to the dialkyl-phosphonates. Nevertheless the methodology should be applied whenever the amount of the alcohol and its structure are not the limiting factors. (author)

  9. Studies on the preparation and stability of samarium-153 propylene diamine tetramethylene phosphonate (PDTMP) complex as a bone seeker

    International Nuclear Information System (INIS)

    Majali, M.A.; Mathakar, A.R.; Shimpi, H.H.; Banerjee, Sharmila; Samuel, Grace

    2000-01-01

    Propylene diamine tetra methylene phosphonate (PDTMP) was synthesised by modifying a method reported for the synthesis of EDTMP. Complexation of the synthesised phosphonate ligand with 153 Sm was carried out by varying the experimental parameters and the complex was radiochemically characterized. Biodistribution studies showed that the uptake by bone in rats was 2% per g of bone, which was retained up to 48 h. The uptake by other organs was insignificant, except by the liver which showed a slightly higher absorption

  10. Synthesis of N-oleyl O-sulfate chitosan from methyl oleate with O-sulfate chitosan as edible film material

    Science.gov (United States)

    Daniel; Sihaloho, O.; Saleh, C.; Magdaleni, A. R.

    2018-04-01

    The research on the synthesis of N-oleyl O-sulfate chitosan through sulfonation reaction on chitosan with ammonium sulfate and followed by amidation reaction using methyl oleate has been done. In this study, chitosan was chemically modified into N-oleyl O-sulfatechitosan as an edible film making material. N-oleyl O-sulfate chitosan was synthesized by reaction between methyl oleate and O-sulfate chitosan. Wherein the depleted chitosan of O-sulfate chitosan into O-sulfate chitosan was obtained by reaction of sulfonation between ammonium sulfate and chitosan aldimine. While chitosan aldimine was obtained through reaction between chitosan with acetaldehyde. The structure of N-oleyl O-sulfate chitosan was characterized by FT-IR analysis which showed vibration uptake of C-H sp3 group, S=O group, and carbonyl group C=O of the ester. The resulting of N-oleyl O-sulfate chitosan yielded a percentage of 93.52%. Hydrophilic-Lipophilic Balance (HLB) test results gave a value of 6.68. In the toxicity test results of N-oleyl O-sulfate chitosan obtained LC50 value of 3738.4732 ppm. In WVTR (Water Vapor Transmission Rate) test results for chitosan film was 407.625 gram/m2/24 hours and N-oleylO-sulfate chitosan film was 201.125 gram/m2/24 hours.

  11. Studies on the obtention and characterization of N,N,N-trimethyl chitosan (TMC)

    International Nuclear Information System (INIS)

    Curti, Elisabete; Campana Filho, Sergio P.

    2001-01-01

    In this work, a study was developed on the obtention of N,N,N-trimethyl chitosan (TMC) aiming the preparation of samples with different average degrees of quaternization under controlled experimental conditions. The effects of previous treatments of chitosan on the reactivity toward its N-alkylation were evaluated and it was concluded that the purification method previously applied to chitosan strongly influenced the reaction yield. The average degrees of quaternization of the TMC samples were determined by nuclear magnetic resonance spectroscopy and they ranged from 4,0% to 22%, depending on the previous treatment to which the chitosan was submitted and on the reaction conditions. It was also concluded that an average degree of quaternization close to 4,0% is already high enough to impart water solubility to this chitosan derivative. (author)

  12. Synthesis, characterization, and antibacterial activity of N,O-quaternary ammonium chitosan.

    Science.gov (United States)

    Xu, Tao; Xin, Meihua; Li, Mingchun; Huang, Huili; Zhou, Shengquan; Liu, Juezhao

    2011-11-08

    N,N,N-Trimethyl O-(2-hydroxy-3-trimethylammonium propyl) chitosans (TMHTMAPC) with different degrees of O-substitution were synthesized by reacting O-methyl-free N,N,N-trimethyl chitosan (TMC) with 3-chloro-2-hydroxy-propyl trimethyl ammonium chloride (CHPTMAC). The products were characterized by (1)H NMR, FTIR and TGA, and investigated for antibacterial activity against Staphylococcus aureus and Escherichia coli under weakly acidic (pH 5.5) and weakly basic (pH 7.2) conditions. TMHTMAPC exhibited enhanced antibacterial activity compared with TMC, and the activity of TMHTMAPC increased with an increase in the degree of substitution. Divalent cations (Ba(2+) and Ca(2+)) strongly reduced the antibacterial activity of chitosan, O-carboxymethyl chitosan and N,N,N-trimethyl-O-carboxymethyl chitosan, but the repression on the antibacterial activity of TMC and TMHTMAPC was weaker. This indicates that the free amino group on chitosan backbone is the main functional group interacting with divalent cations. The existence of 100 mM Na(+) slightly reduced the antibacterial activity of both chitosan and its derivatives. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Enhanced adsorption of methyl violet and congo red by using semi and full IPN of polymethacrylic acid and chitosan.

    Science.gov (United States)

    Maity, Jayabrata; Ray, Samit Kumar

    2014-04-15

    Semi and full interpenetrating polymer network (IPN) type hydrogels were prepared by free radical in situ polymerization of methacrylic acid in presence of chitosan using N,N'-methylene-bis-acrylamide (MBA) and glutaraldehyde (for full IPN) as crosslinker. Several semi and full IPN type hydrogels were prepared by varying initiator and crosslinker concentration and also monomer to chitosan mass ratio. These hydrogels were characterized and used for removal of methyl violet and congo red dye from water. Isotherms and kinetics of dye adsorption were also evaluated. Copyright © 2014 Elsevier Ltd. All rights reserved.

  14. Exploiting the high-affinity phosphonate-hydroxyapatite nanoparticle interaction for delivery of radiation and drugs

    International Nuclear Information System (INIS)

    Ong, Hooi Tin; Loo, Joachim S. C.; Boey, Freddy Y. C.; Russell, Stephen J.; Ma Jan; Peng, Kah-Whye

    2008-01-01

    Hydroxyapatite is biocompatible and used in various biomedical applications. Here, we generated hydroxyapatite nanoparticles (HNPs) of various sizes (40-200 nm) and demonstrated that they can be stably loaded with drugs or radioisotopes by exploiting the high-affinity HA-(poly)phosphonate interaction. Clinically available phosphonates, clodronate, and Tc-99m-methylene-diphosphonate (Tc-99m-MDP), were efficiently loaded onto HNPs within 15 min. Biodistribution of radiolabeled HNP-MDP-Tc99m in mice was monitored non-invasively using microSPECT-CT. Imaging and dosimetry studies indicated that the HNPs, regardless of size, were quickly taken up by Kupffer cells in the liver after systemic administration into mice. Clodronate loaded onto HNPs remained biologically active and were able to result in selective depletion of Kupffer cells. This method of drug or isotope loading on HA is fast and easy as it eliminates the need for additional surface modifications of the nanoparticles

  15. Experimental and theoretical studies on extraction of actinides and lanthanides by alicyclic H-phosphonates

    Energy Technology Data Exchange (ETDEWEB)

    Annam, Suresh; Sivaramakrishna, Akella; Vijayakrishna, Kari [VIT Univ., Tamil Nadu (India). Dept. of Chemistry; Gopakumar, Gopinadhanpillai; Rao, C.V.S. Brahmmananda; Sivaraman, N. [Indira Gandhi Centre for Atomic Research (IGCAR), Tamil Nadu (India). Chemistry Group

    2017-06-01

    Three different alicyclic substituents H-phosphonates, namely, dicyclopentyl H-phosphonate, dicyclohexyl H-phosphonate and dimenthyl H-phosphonate were synthesized and used for liquid-liquid extraction of actinide elements (U, Am and Th) and lanthanide (Gd) in n-dodecane from nitric acid medium. The physicochemical properties of the extractants, such as density, viscosity, solubility were determined. At lower acidities, these H-phosphonates exhibit higher distribution values and the extraction following cation exchange mechanism through P-OH group of tri-coordinated phosphite form. At higher acidities (2N), the extraction is primarily via solvation mechanism through P=O group of penta-coordinated phosphonate form. Amongst the three H-phosphonates, examined dimenthyl H-phosphonate showed the best results for the actinide extraction. Density functional theory (DFT) calculations were applied to understand the electronic structure of the ligands and the metal complexes. The calculated large complexation energy of UO{sub 2}(NO{sub 3}){sub 2}.@2DMnHP is in agreement with the observed trend in experimental distribution ratio data.

  16. Assembly of phosphonic acids on GaN and AlGaN

    Energy Technology Data Exchange (ETDEWEB)

    Simpkins, B S; Stine, R; Theodore, N D; Pehrsson, P E [Chemistry Division, Naval Research Laboratory, Washington DC (United States); Hong, S [Thomas Jefferson High School, McClean, VA (United States); Maekinen, A J [Optical Sciences Division, Naval Research Laboratory, Washington, DC (United States); Mastro, M A; Eddy, C R Jr [Electronics Science and Technology Division, Naval Research Laboratory, Washington, DC (United States)

    2010-01-13

    Self-assembled monolayers of octadecylphosphonic acid and 16-phosphonohexadecanoic acid (PHDA) were formed on the semiconductor substrates gallium nitride (GaN) and aluminium gallium nitride (AlGaN). The presence of the molecular layers was verified through x-ray photoelectron spectroscopy and ultraviolet photoelectron spectroscopy. Structural information was acquired with infrared spectroscopy which verified the bonding orientation of the carboxyl-containing PHDA. The impact of the molecular layers on the channel conductivity and the surface electronic structure of an AlGaN/GaN heterostructure was measured. Our results indicate that pinning of the surface Fermi level prohibits modification of the channel conductivity by the layer. However, a surface dipole of {approx}0.8 eV is present and associated with both phosphonic acid layers. These results are of direct relevance to field-effect-based biochemical sensors and metal-semiconductor contact formation for this system and provide a fundamental basis for further applications of GaN and AlGaN technology in the fields of biosensing and microelectronics.

  17. Synthesize and Characterization of Hydroxypropyl-N-octanealkyl Chitosan Ramification

    Science.gov (United States)

    Tan, Fu-neng

    2018-03-01

    A new type of amphiphilic ramification, hydroxypropyl-N-octanealkyl chitosan was prepared from chitosan via hydrophilic group and hydrophobic group were introduced. We could protect the amino group of chitosan via the reaction of chitosan and benzaldehyde could get Schiff base structure. Structures of the products were characterized with FT-IR, elemental analysis, themogrammetry (TG) analysis and X-ray diffraction. The degree of substitution of hydrophobic group was studied by elemental analysis. The result showed this chitosan ramification was soluble, biocompatible, biodegradable and nontoxic.

  18. Development of new additive for drilling fluid from the partial hydrophobization N,N,N-trimethyl chitosan (TMC)

    International Nuclear Information System (INIS)

    Carmo, Thacyla C. do; Lopes, Grazielle; Silva, Joaquim F.M. da; Nascimento, Regina S.V.

    2009-01-01

    N,N,N-trimethyl chitosan (TMC) hydrophobically modified can act as an excellent additive for drilling fluids water based, working as inhibitor of reactive shales and rheological modifiers. The cationic chitosan was obtained by reaction of chitosan with CH 3 I in N-methyl-2-pyrrolidone to obtain the TMC and chitosan was also hydrophobically modified with palmitoil chloride to get Quit P. Through another route, Quit P was modified to obtain the cationic TMCP. The derivatives were characterized by FT-IR and 1 HNMR spectrophotometry allowing the calculation of the degree of quaternization of the TMC. The rheology tests showed that the system with TMCP presented pseudo plastic behavior, while the system with TMC behaved as a Newtonian fluid. The results indicated that TMCP can act as rheology modifier for water-based drilling fluids. (author)

  19. Novel open-framework architectures in lanthanide phosphonates

    Science.gov (United States)

    Groves, John A.; Stephens, Nicholas F.; Wright, Paul A.; Lightfoot, Philip

    2006-03-01

    Two novel three-dimensional lanthanide coordination polymers have been prepared hydrothermally with the phosphonic acid N,N-piperazine bis(methylenephosphonic acid), H 2O 3PCH 2N(C 2H 4) 2NCH 2PO 3H 2 ( LH 4). The structures of Gd 2( LH 2) 3ṡ3H 2O (I) and Nd 2( LH 2) 3ṡ9H 2O (II) have been characterised by single crystal X-ray techniques. One-dimensional 'lanthanide-phosphate' chains are a key feature in both structures, although there are major structural differences between the chains, with (I) displaying octahedral GdO 6 coordination and (II) showing eight-coordinate NdO 8 polyhedra. In each case, three-dimensional connectivity is completed by coordination of the phosphonate group resulting in open framework structures encapsulating loosely bound water molecules. Isostructural Y 3+ and Yb 3+ analogues of (I) have been prepared, suggesting that cation size is a key factor in controlling the differing reaction products. In the case of Y 2( LH 2) 3ṡ5H 2O, isostructural to (I), it is shown that the extra-framework water molecules may be removed reversibly without framework collapse. Structural relationships to other known lanthanide phosphonates are discussed.

  20. Mesoporous-activated carbon prepared from chitosan flakes via single-step sodium hydroxide activation for the adsorption of methylene blue.

    Science.gov (United States)

    Marrakchi, F; Ahmed, M J; Khanday, W A; Asif, M; Hameed, B H

    2017-05-01

    In this work, mesoporous-activated carbon (CSAC) was prepared from chitosan flakes (CS) via single-step sodium hydroxide activation for the adsorption of methylene blue (MB). CSAC was prepared using different impregnation ratios of NaOH:CS (1:1, 2:1, 3:1, and 4:1) at 800°C for 90min. The adsorption performance of CSAC was evaluated for MB at different adsorption variables, such MB initial concentrations (25-400mg/L), solution pH (3-11), and temperature (30-50°C). The adsorption isotherm data of CSAC-MB were well fitted to Langmuir model with a maximum adsorption capacity 143.53mg/g at 50°C. Best representation of kinetic data was obtained by the pseudo-second order model. CSAC exhibited excellent adsorption uptake for MB and can potentially be used for other cationic dyes. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Fluoride-Mediated Dephosphonylation of α-Diazo-β-carbonyl Phosphonates.

    Science.gov (United States)

    Phatake, Ravindra S; Mullapudi, Venkannababu; Wakchaure, Vivek C; Ramana, Chepuri V

    2017-01-20

    The possibility of fluoride-mediated selective dephosphonylation of α-diazo-β-carbonyl phosphonates such as the Ohira-Bestmann reagent has been proposed and executed. The resulting α-diazocarbonyl intermediates undergo a (3 + 2)-cycloaddition at room temperature with conjugated olefins and benzynes. Interestingly, under the current conditions, the resulting cycloaddition products underwent either N-acylation (with excess α-diazo-β-carbonyl phosphonates) or Michael addition (with conjugated olefins).

  2. Synthesis, self-assembly and lipoplex formulation of two novel cyclic phosphonate lipids

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    JenniferYeh

    2013-05-01

    Full Text Available Background: Synthetic cationic lipids hold much potential as gene packaging and delivery agents for the treatment of inherited and acquired life threatening diseases, such as cancer, AIDS, cardiovascular diseases, and certain autoimmune disorders. Methods: We report the synthesis, self-assembly as characterized by critical micelle concentrations and plasmid DNA gel retardation using two novel cyclic, phosphonate cationic lipids 2a and 2b, which were synthesized by derivatizing two diastereomeric macrocyclic phosphonates 1a and 1b with a 2-carbon hydroxylamine linker, N, N-dimethylethanolamine (3. Results: The production of cyclic phosphonate lipids 2a and 2b in 73% and 60% yields, respectively, was achieved using classical synthetic methods involving nucleophilic substitution at the phosphorus centre. Conclusions: The synthesis, aggregation and DNA binding properties of these novel cyclic phosphonate lipids suggest that they may have utility serving as gene packaging and delivery agents.

  3. Proton conducting membranes prepared by incorporation of organophosphorus acids into alcohol barrier polymers for direct methanol fuel cells

    Science.gov (United States)

    Jiang, Zhongyi; Zheng, Xiaohong; Wu, Hong; Pan, Fusheng

    A novel type of DMFC membrane was developed via incorporation of organophosphorus acids (OPAs) into alcohol barrier materials (polyvinyl alcohol/chitosan, PVA/CS) to simultaneously acquire high proton conductivity and low methanol permeability. Three kinds of OPAs including amino trimethylene phosphonic acid (ATMP), ethylene diamine tetra(methylene phosphonic acid) (EDTMP) and hexamethylene diamine tetra(methylene phosphonic acid) (HDTMP), with different molecular structure and phosphonic acid groups content were added into PVA/CS blends and served the dual functions as proton conductor as well as crosslinker. The as-prepared OPA-doped PVA/CS membranes exhibited remarkably enhanced proton conducting ability, 2-4 times higher than that of the pristine PVA/CS membrane, comparable with that for Nafion ®117 membrane (5.04 × 10 -2 S cm -1). The highest proton conductivities 3.58 × 10 -2, 3.51 × 10 -2 and 2.61 × 10 -2 S cm -1 for ATMP-, EDTMP- and HDTMP-doped membranes, respectively were all achieved at highest initial OPA doping content (23.1 wt.%) at room temperature. The EDTMP-doped PVA/CS membrane with an acid content of 13.9 wt.% showed the lowest methanol permeability of 2.32 × 10 -7 cm 2 s -1 which was 16 times lower than that of Nafion ®117 membrane. In addition, the thermal stability and oxidative durability were both significantly improved by the incorporation of OPAs in comparison with pristine PVA/CS membranes.

  4. Adsorbed States of phosphonate derivatives of N-heterocyclic aromatic compounds, imidazole, thiazole, and pyridine on colloidal silver: comparison with a silver electrode.

    Science.gov (United States)

    Podstawka, Edyta; Olszewski, Tomasz K; Boduszek, Bogdan; Proniewicz, Leonard M

    2009-09-03

    Here, we report a systematic surface-enhanced Raman spectroscopy (SERS) study of the structures of phosphonate derivatives of the N-heterocyclic aromatic compounds imidazole (ImMeP ([hydroxy(1H-imidazol-5-yl)methyl]phosphonic acid) and (ImMe)(2)P (bis[hydroxy-(1H-imidazol-4-yl)-methyl]phosphinic acid)), thiazole (BAThMeP (butylaminothiazol-2-yl-methyl)phosphonic acid) and BzAThMeP (benzylaminothiazol-2-yl-methyl)phosphonic acid)), and pyridine ((PyMe)(2)P (bis[(hydroxypyridin-3-yl-methyl)]phosphinic acid)) adsorbed on nanometer-sized colloidal particles. We compared these structures to those on a roughened silver electrode surface to determine the relationship between the adsorption strength and the geometry. For example, we showed that all of these biomolecules interact with the colloidal surface through aromatic rings. However, for BzAThMeP, a preferential interaction between the benzene ring and the colloidal silver surface is observed more so than that between the thiazole ring and this substrate. The PC(OH)C fragment does not take part in the adsorption process, and the phosphonate moiety of ImMeP and (ImMe)(2)P, being removed from the surface, only assists in this process.

  5. Rhodium(iii)-catalyzed ortho-olefination of aryl phosphonates.

    Science.gov (United States)

    Chary, Bathoju Chandra; Kim, Sunggak

    2013-09-25

    Rhodium(iii)-catalyzed C-H olefination of aryl phosphonic esters is reported for the first time. In this mild and efficient process, the phosphonic ester group is utilized successfully as a new directing group. In addition, mono-olefination for aryl phosphonates is observed using a phosphonic diamide directing group.

  6. Graft copolymerization of N-maleoyl-N-phthaloyl-chitosan (MAPHCS) and acrylic acid via γ-ray irradiation

    International Nuclear Information System (INIS)

    Mu Qing; Fang Yue'e

    2006-01-01

    Chitosan is a well-known abundant natural polymer with good biodegradability, biocompatibility and bioactivity. But its insolubility in common organic solvents of chitosan have hindered its utilization and basic research. N-maleoyl-N-phthaloyl-chitosan (MAPHCS), soluble in DMF or DMSO, was synthesized and characterized by Fourier transform infrared spectra analysis (FT-IR) and 1 H-NMR. The graft copolymerization of acrylic acid onto chitosan was carried out with N-maleoyl-N-phthaloyl-chitosan as intermediate in homogeneous system and initiated by γ-irradiation. The double bond of MAPHCS may be the grafting site because the grafting field was much higher than that of the graft copolymerization of acrylic acid and phthaloylchitosan via γ-ray irradiation. The chemical structure of the graft copolymer was characterized by FT-IR and 1 H-NMR. As indicated in FTIR spectra, the evidence of the stronger absorbance at 2800-3000 cm -1 for C-H and at 1720 cm -1 for carboxyl group implied significantly the successful introduction of the poly (acrylic acid) on the chitosan chain. Differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were also used to characterize the copolymer. Effects of synthesis variables on the graft copolymerization were studied in light of the grafting percentage. The grafting percentage increased with the dose at lower doses, and then decreased. The maximum grafting percentage was up to 132%. (authors)

  7. Hydrothermal syntheses, characterizations and crystal structures of a new lead(II) carboxylate-phosphonate with a double layer structure and a new nickel(II) carboxylate-phosphonate containing a hydrogen-bonded 2D layer with intercalation of ethylenediamines

    International Nuclear Information System (INIS)

    Song, J.-L.; Mao, J.-G.; Sun, Y.-Q.; Zeng, H.-Y.; Kremer, R.K.; Clearfield, Abraham

    2004-01-01

    Hydrothermal reactions of N,N-bis(phosphonomethyl)aminoacetic acid (HO 2 CCH 2 N(CH 2 PO 3 H 2 ) 2 ) with metal(II) salts afforded two new metal carboxylate-phosphonates, namely, Pb 2 [O 2 CCH 2 N(CH 2 PO 3 )(CH 2 PO 3 H)]·H 2 O (1) and {NH 3 CH 2 CH 2 NH 3 }{Ni[O 2 CCH 2 N(CH 2 PO 3 H) 2 ](H 2 O) 2 } 2 (2). Among two unique lead(II) ions in the asymmetric unit of complex 1, one is five coordinated by five phosphonate oxygen atoms from 5 ligands, whereas the other one is five-coordinated by a tridentate chelating ligand (1 N and 2 phosphonate O atoms) and two phosphonate oxygen atoms from two other ligands. The carboxylate group of the ligand remains non-coordinated. The bridging of above two types of lead(II) ions through phosphonate groups resulted in a double layer with the carboxylate group of the ligand as a pendant group. These double layers are further interlinked via hydrogen bonds between the carboxylate groups into a 3D network. The nickel(II) ion in complex 2 is octahedrally coordinated by a tetradentate chelating ligand (two phosphonate oxygen atoms, one nitrogen and one carboxylate oxygen atoms) and two aqua ligands. These {Ni[O 2 CCH 2 N(CH 2 PO 3 H) 2 ][H 2 O] 2 } - anions are further interlinked via hydrogen bonds between non-coordinated phosphonate oxygen atoms to form a hydrogen bonded 2D layer. The 2H-protonated ethylenediamine cations are intercalated between two layers, forming hydrogen bonds with the non-coordinated carboxylate oxygen atoms. Results of magnetic measurements for complex 2 indicate that there is weak Curie-Weiss behavior with θ=-4.4 K indicating predominant antiferromagnetic interaction between the Ni(II) ions. Indication for magnetic low-dimension magnetism could not be detected

  8. Synthesis of highly phosphonic acid functionalized benzene-bridged periodic mesoporous organosilicas for use as efficient dye adsorbents

    International Nuclear Information System (INIS)

    Deka, Juti Rani; Liu, Chia-Ling; Wang, Tzu-Hua; Chang, Wei-Chieh; Kao, Hsien-Ming

    2014-01-01

    Highlights: • Synthesis of highly phosphonic acid functionalized benzene-bridged PMOs. • Phosphonic acid loaded PMOs as adsorbent for cationic and anionic dyes. • Due to electrostatic interaction the adsorbent has high dye adsorption capacity. • π–π stacking interaction between benzene and dye enhances adsorption capacity. • Intraparticle diffusion played a dominant role in the adsorption process. - Abstract: Periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall were functionalized with a tunable content of phosphonic acid groups. These bifunctional materials were synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic conditions using nonionic surfactant Brij-S10 as template. The materials exhibited well-ordered mesostructures and were characterized by X-ray diffraction, nitrogen sorption, TEM, TGA, FTIR, and solid-state NMR measurements. The materials thus obtained were employed as adsorbents to remove different types of dyes, for example, cationic dyes methylene blue and phenosafranine, anionic orange II, and amphoteric rhodamine B, from aqueous solutions. The materials exhibited a remarkably high adsorption capacity than activated carbon due to their ordered mesostructures, a large number of phosphonic acid groups, and high surface areas. The adsorption was mainly governed by electrostatic interaction, but also involved π–π stacking interaction as well as hydrogen bonding. The adsorption kinetics can be better fitted by the pseudo-second order model. The adsorption process was controlled by the mechanisms of external mass transfer and intraparticle diffusion. The materials retained more than 97% dye removal efficiency after use for five consecutive cycles

  9. Proton conducting membranes prepared by incorporation of organophosphorus acids into alcohol barrier polymers for direct methanol fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Zhongyi; Zheng, Xiaohong; Wu, Hong; Pan, Fusheng [Key Laboratory for Green Chemical Technology, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China)

    2008-10-15

    A novel type of DMFC membrane was developed via incorporation of organophosphorus acids (OPAs) into alcohol barrier materials (polyvinyl alcohol/chitosan, PVA/CS) to simultaneously acquire high proton conductivity and low methanol permeability. Three kinds of OPAs including amino trimethylene phosphonic acid (ATMP), ethylene diamine tetra(methylene phosphonic acid) (EDTMP) and hexamethylene diamine tetra(methylene phosphonic acid) (HDTMP), with different molecular structure and phosphonic acid groups content were added into PVA/CS blends and served the dual functions as proton conductor as well as crosslinker. The as-prepared OPA-doped PVA/CS membranes exhibited remarkably enhanced proton conducting ability, 2-4 times higher than that of the pristine PVA/CS membrane, comparable with that for Nafion {sup registered} 117 membrane (5.04 x 10{sup -2} S cm{sup -1}). The highest proton conductivities 3.58 x 10{sup -2}, 3.51 x 10{sup -2} and 2.61 x 10{sup -2} S cm{sup -1} for ATMP-, EDTMP- and HDTMP-doped membranes, respectively were all achieved at highest initial OPA doping content (23.1 wt.%) at room temperature. The EDTMP-doped PVA/CS membrane with an acid content of 13.9 wt.% showed the lowest methanol permeability of 2.32 x 10{sup -7} cm{sup 2} s{sup -1} which was 16 times lower than that of Nafion {sup registered} 117 membrane. In addition, the thermal stability and oxidative durability were both significantly improved by the incorporation of OPAs in comparison with pristine PVA/CS membranes. (author)

  10. Copper-Catalyzed Synthesis of Mixed Alkyl Aryl Phosphonates

    NARCIS (Netherlands)

    Fañanás-Mastral, Martín; Feringa, Ben L

    2014-01-01

    Copper-catalysis allows the direct oxygenarylation of dialkyl phosphonates with diaryliodonium salts. This novel methodology proceeds with a wide range of phosphonates and phosphoramidates under mild conditions and gives straightforward access to valuable mixed alkyl aryl phosphonates in very good

  11. Textile Dye Removal from Aqueous Solution using Modified Graphite Waste/Lanthanum/Chitosan Composite

    Science.gov (United States)

    Kusrini, E.; Wicaksono, B.; Yulizar, Y.; Prasetyanto, EA; Gunawan, C.

    2018-03-01

    We investigated various pre-treatment processes of graphite waste using thermal, mechanical and chemical methods. The aim of this work is to study the performance of modified graphite waste/lanthanum/chitosan composite (MG) as adsorbent for textile dye removal from aqueous solution. Effect of graphite waste resources, adsorbent size and lanthanum concentration on the dye removal were studied in batch experiments. Selectivity of MG was also investigated. Pre-heated graphite waste (NMG) was conducted at 80°C for 1 h, followed by mechanical crushing of the resultant graphite to 75 μm particle size, giving adsorption performance of ˜58%, ˜67%, ˜93% and ˜98% of the model dye rhodamine B (concentration determined by UV-vis spectroscopy at 554 nm), methyl orange (464 nm), methylene blue (664 nm) and methyl violet (580 nm), respectively from aqueous solution. For this process, the system required less than ˜5 min for adsorbent material to be completely saturated with the adsorbate. Further chemical modification of the pre-treated graphite waste (MG) with lanthanum (0.01 – V 0.03 M) and chitosan (0.5% w/w) did not improve the performance of dye adsorption. Under comparable experimental conditions, as those of the ‘thermal-mechanical-pre-treated-only’ (NMG), modification of graphite waste (MG) with 0.03 M lanthanum and 0.5% w/w chitosan resulted in ˜14%, ˜47%, ˜72% and ˜85% adsorption of rhodamine B, methyl orange, methylene blue and methyl violet, respectively. Selective adsorption of methylene blue at most to ˜79%, followed by methyl orange, methyl violet and rhodamine B with adsorption efficiency ˜67, ˜38, and ˜9% sequentially using MG with 0.03 M lanthanum and 0.5% w/w chitosan.

  12. Synthesis of novel castor oil phosphonates

    Science.gov (United States)

    Castor oil has served as a versatile hydroxy fatty acid (HFA); its principle component, ricinoleic acid, can be isolated from castor oil and has been modified extensively for a number of applications. Additionally, phosphonates and their corresponding phosphonic acids are a functional moiety that ha...

  13. Flame retardant cotton fabrics by electron beam-induced polymerization of vinyl phosphonate oligomer

    International Nuclear Information System (INIS)

    Sawai, Takeshi; Ametani, Kazuo; Enomoto, Ichiro

    1988-01-01

    Vinyl phosphonate oligomer is presently used commercially as a cellulosic flame retardant in conjugation with N-methylol acrylamide, using a persulfate catalyst and a thermal cure. This combination can also be cured at room temperature with electron beams, as can the vinyl phosphonate alone. For the textile application, fixation of flame retardants by electron beams with low energy is one of the most promising applications. For the purpose of preparing flame resistant cotton fabrics such as bed sheets and pajamas, flame retardant curing of vinyl phosphonate oligomer on cotton fabrics was examined using electron beams from a self-sealed electron beam processor and gamma rays from a 60 Co source. A joint investigation was undertaken by the Tokyo Metropolitan Textile Research Institute and Tokyo Metropolitan Isotope Research Center to determine the feasibility of curing vinyl phosphonate oligomer on the cotton fabrics for textile finishing. (author)

  14. Recent advances in H-phosphonate chemistry. Part 1. H-phosphonate esters: synthesis and basic reactions.

    Science.gov (United States)

    Sobkowski, Michal; Kraszewski, Adam; Stawinski, Jacek

    2015-01-01

    This review covers recent progress in the preparation of H-phosphonate mono- and diesters, basic studies on mechanistic and stereochemical aspects of this class of phosphorus compounds, and their fundamental chemistry in terms of transformation of P-H bonds into P-heteroatom bonds. Selected recent applications of H-phosphonate derivatives in basic organic phosphorus chemistry and in the synthesis of biologically important phosphorus compounds are also discussed.

  15. ESI(+-MS and GC-MS Study of the Hydrolysis of N-Azobenzyl Derivatives of Chitosan

    Directory of Open Access Journals (Sweden)

    Fernanda S. Pereira

    2014-10-01

    Full Text Available New N-p-chloro-, N-p-bromo-, and N-p-nitrophenylazobenzylchitosan derivatives, as well as the corresponding azophenyl and azophenyl-p-sulfonic acids, were synthesized by coupling N-benzylvchitosan with aryl diazonium salts. The synthesized molecules were analyzed by UV-Vis, FT-IR, 1H-NMR and 15N-NMR spectroscopy. The capacity of copper chelation by these materials was studied by AAS. Chitosan and the derivatives were subjected to hydrolysis and the products were analyzed by ESI(+-MS and GC-MS, confirming the formation of N-benzyl chitosan. Furthermore, the MS results indicate that a nucleophilic aromatic substitution (SnAr reaction occurs under hydrolysis conditions, yielding chloroaniline from N-p-bromo-, and N-p-nitrophenylazo-benzylchitosan as well as bromoaniline from N-p-chloro-, and N-p-nitrophenylazobenzyl-chitosan.

  16. Synthesis and configurational analysis of phosphonate cavitands

    NARCIS (Netherlands)

    Jacopozzi, Paola; Dalcanale, Enrico; Spera, Silvia; Chrisstoffels, L.A.J.; Reinhoudt, David; Lippmann, Tino; Mann, Gerhard

    1998-01-01

    Synthesis, separation and configurational analysis of phosphonated and partially phosphonated cavitands derived from resorcinarenes are described. The configuration of all diastereomers has been elucidated by their 1H, 31P NMR spectra and 13C relaxation times. In all cases the course of the bridging

  17. Phosphonate removal from discharged circulating cooling water using iron-carbon micro-electrolysis.

    Science.gov (United States)

    Zhou, Zhen; Qiao, Weimin; Lin, Yangbo; Shen, Xuelian; Hu, Dalong; Zhang, Jianqiao; Jiang, Lu-Man; Wang, Luochun

    2014-01-01

    Phosphonate is a commonly used corrosion and scale inhibitor for a circulating cooling water (CCW) system. Its discharge could cause eutrophication of receiving waters. The iron-carbon (Fe/C) micro-electrolysis technology was used to degrade and remove phosphonate from discharged CCW. The influences of initial pH, Fe/C ratio (FCR) and temperature on phosphonate removal were investigated in a series of batch tests and optimized by response surface methodology. The quadratic model of phosphonate removal was obtained with satisfactory degrees of fitness. The optimum conditions with total phosphorus removal efficiency of 95% were obtained at pH 7.0, FCR of 1.25, and temperature of 45 °C. The phosphonate removal mechanisms were also studied. Phosphonate removal occurred predominantly via two consecutive reactive phases: the degradation of phosphonate complexes (Ca-phosphonate) and the precipitation of Fe/C micro-electrolysis products (PO₄(3-), Ca²⁺ and Fe³⁺).

  18. Development of new additive for drilling fluid from the partial hydrophobization N,N,N-trimethyl chitosan (TMC); Desenvolvimento de novos aditivos para fluidos de perfuracao a partir da hidrofobizacao parcial da N,N,N trimetilquitosana (TMQ)

    Energy Technology Data Exchange (ETDEWEB)

    Carmo, Thacyla C. do; Lopes, Grazielle; Silva, Joaquim F.M. da; Nascimento, Regina S.V., E-mail: cycyla@hotmail.co [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Polo de Xistoquimica

    2009-07-01

    N,N,N-trimethyl chitosan (TMC) hydrophobically modified can act as an excellent additive for drilling fluids water based, working as inhibitor of reactive shales and rheological modifiers. The cationic chitosan was obtained by reaction of chitosan with CH{sub 3}I in N-methyl-2-pyrrolidone to obtain the TMC and chitosan was also hydrophobically modified with palmitoil chloride to get Quit P. Through another route, Quit P was modified to obtain the cationic TMCP. The derivatives were characterized by FT-IR and {sup 1}HNMR spectrophotometry allowing the calculation of the degree of quaternization of the TMC. The rheology tests showed that the system with TMCP presented pseudo plastic behavior, while the system with TMC behaved as a Newtonian fluid. The results indicated that TMCP can act as rheology modifier for water-based drilling fluids. (author)

  19. Oral Methylated N-Aryl Chitosan Derivatives for Inducing Immune ...

    African Journals Online (AJOL)

    TM-CM-CS) and methylated N-(4-pyridinylmethyl) chitosan (TM-Py-CS), with Eqiva degree (equivalent degree) were studied by in vitro absorption enhancement on the transepithelial electrical resistance (TEER) in Caco-2 cell monolayers as ...

  20. Calixarene methylene bisphosphonic acids as promising effectors of biochemical processes

    Directory of Open Access Journals (Sweden)

    S. V. Komisarenko

    2013-12-01

    rim have been studied with respect to their effects on fibrin polymerization. The most potent inhibitor proved to be calix[4]arene tetrakis-methylene-bis-phosphonic acid (C-192, in which case the maximum rate of fibrin polymerization in the fibrinogen + thrombin reaction decreased by 50% at concentrations of 0.52·10-6 M (IC50. At this concentration, the molar ratio of the compound to fibrinogen was 1.7 : 1. For the case of desAB fibrin polymerization, the IC50 was 1.26·10-6 M at a molar ratio of C-192 to fibrin monomer of 4 : 1. Dipropoxycalix[4]-arene bis-methylene-bis-phosphonic acid (C-98 inhibited fibrin desAB polymerization with an IC50 = 1.31·10-4 M. We hypothesized that C-192 blocks fibrin formation by combining with polymerization site ‘A’ (Aa17–19, which ordinarily initiates protofibril formation in a ‘knob-hole’ manner. This suggestion was confirmed by an HPLC assay, which showed a host–guest inclusion complex of C-192 with the synthetic peptide Gly-Pro-Arg-Pro, an analogue of site ‘A’. Further confirmation that the inhibitor was acting at the initial step of the reaction was obtained by electron microscopy, with no evidence of protofibril formation being evident. Calixarene C-192 also doubled both the prothrombin time and the activated partial thromboplastin time in normal human blood plasma at concentrations of 7.13·10-5 and 1.10·10-5 M, respectively. These experiments demonstrate that C-192 is a specific inhibitor of fibrin polymerization and blood coagulation and can be used for the design of a new class of antithrombotic agents.

  1. Self-ordered Porous Alumina Fabricated via Phosphonic Acid Anodizing

    OpenAIRE

    Akiya, Shunta; Kikuchi, Tatsuya; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

    2016-01-01

    Self-ordered periodic porous alumina with an undiscovered cell diameter was fabricated via electrochemical anodizing in a new electrolyte, phosphonic acid (H3PO3). High-purity aluminum plates were anodized in phosphonic acid solution under various operating conditions of voltage, temperature, concentration, and anodizing time. Phosphonic acid anodizing at 150-180 V caused the self-ordering behavior of porous alumina, and an ideal honeycomb nanostructure measuring 370-440 nm in cell diameter w...

  2. Chitosan based metallic nanocomposite scaffolds as antimicrobial wound dressings.

    Science.gov (United States)

    Mohandas, Annapoorna; Deepthi, S; Biswas, Raja; Jayakumar, R

    2018-09-01

    Chitosan based nanocomposite scaffolds have attracted wider applications in medicine, in the area of drug delivery, tissue engineering and wound healing. Chitosan matrix incorporated with nanometallic components has immense potential in the area of wound dressings due to its antimicrobial properties. This review focuses on the different combinations of Chitosan metal nanocomposites such as Chitosan/nAg, Chitosan/nAu, Chitosan/nCu, Chitosan/nZnO and Chitosan/nTiO 2 towards enhancement of healing or infection control with special reference to the antimicrobial mechanism of action and toxicity.

  3. Preparation of thermal-responsive chitosan-graft-N-isopropylacrylamide membranes via γ-ray irradiation

    International Nuclear Information System (INIS)

    Mu Qing; Fang Yue'e

    2006-01-01

    Poly(N-isopropylacrylamide) (PNIPAAm) has been attracting increasing attention because of its thermosensitivity. Many authors have studied the reaction of chitosan with NIPAAm, with most of the interest being focused on hydrogels. Few research programs, however, were about chitosan membranes grafted with NIPAAm monomer. In this study, a novel thermo-sensitive switching membrane was prepared by radiation-induced simultaneous grafting of NIPAAm onto chitosan membrane. Fourier transform infrared spectroscopy (FT-IR) was used to identify structure of the grafted membranes. Compared to FT-IR spectra of pristine chitosan, the new band at 1535 cm-1 in the grafted membrane was attributed to amide II of PNIPAAm. This indicated that NIPAAm was introduced onto the chitosan membrane. Surface morphology of the grafted membrane was different from the pristine chitosan membrane. The SEM images revealed cypress leaf-like structures adhered tightly to the grafted membrane surface, in comparison to smooth surface of the pristine chitosan membrane. Pure water flux measurements showed that the grafted membrane decreased with the increasing temperature, while water flux of pristine chitosan membrane was constant. It was found that the grafted membrane was sensitive to temperature. The effects of dose, dose rate and the concentration of NIPAAm on the grafting percentage were discussed. The graft yield increased with the monomer concentration and the absorbed dose. (authors)

  4. Room-Temperature Alternative to the Arbuzov Reaction: The Reductive Deoxygenation of Acyl Phosphonates

    OpenAIRE

    Kedrowski, Sean M. A.; Dougherty, Dennis A.

    2010-01-01

    The reductive deoxygenation of acyl phosphonates using a Wolff−Kishner-like sequence is described. This transformation allows direct access to alkyl phosphonates from acyl phosphonates at room temperature. The method can be combined with acyl phosphonate synthesis into a one pot, four-step procedure for the conversion of carboxylic acids into alkyl phosphonates. The methodology works well for a variety of aliphatic acids and shows a functional group tolerance similar to that of other hydrazon...

  5. Quantitative structure-property relationship (correlation analysis) of phosphonic acid-based chelates in design of MRI contrast agent.

    Science.gov (United States)

    Tiwari, Anjani K; Ojha, Himanshu; Kaul, Ankur; Dutta, Anupama; Srivastava, Pooja; Shukla, Gauri; Srivastava, Rakesh; Mishra, Anil K

    2009-07-01

    Nuclear magnetic resonance imaging is a very useful tool in modern medical diagnostics, especially when gadolinium (III)-based contrast agents are administered to the patient with the aim of increasing the image contrast between normal and diseased tissues. With the use of soft modelling techniques such as quantitative structure-activity relationship/quantitative structure-property relationship after a suitable description of their molecular structure, we have studied a series of phosphonic acid for designing new MRI contrast agent. Quantitative structure-property relationship studies with multiple linear regression analysis were applied to find correlation between different calculated molecular descriptors of the phosphonic acid-based chelating agent and their stability constants. The final quantitative structure-property relationship mathematical models were found as--quantitative structure-property relationship Model for phosphonic acid series (Model 1)--log K(ML) = {5.00243(+/-0.7102)}- MR {0.0263(+/-0.540)}n = 12 l r l = 0.942 s = 0.183 F = 99.165 quantitative structure-property relationship Model for phosphonic acid series (Model 2)--log K(ML) = {5.06280(+/-0.3418)}- MR {0.0252(+/- .198)}n = 12 l r l = 0.956 s = 0.186 F = 99.256.

  6. Nanocomposites of phosphonic-acid-functionalized polyethylenes with inorganic quantum dots.

    Science.gov (United States)

    Rünzi, Thomas; Baier, Moritz C; Negele, Carla; Krumova, Marina; Mecking, Stefan

    2015-01-01

    Insertion of diethyl vinyl phosphonates and free vinyl phosphonic acid, respectively, into [(P^O)Pd(Me)(dmso)] ((P^O) = κ(2)-P,O-Ar2PC6H4SO2O with Ar = 2-MeOC6H4) (1-dmso) occurs in a 2,1- as well as 1,2-fashion, to form a four-and a five-membered chelate [(P^O)Pd{κ(2)-C,O-CH(P(O)(OR)2)CH2CH3}] and [(P^O)Pd{κ(2)-C,O-CH2CH(P(O)(OR)2)CH3}] (R = H, Et). No decomposition or other reactions of 1 by free phosphonic acid moieties occur. Copolymerization in a pressure reactor by 1-dmso yields linear random poly(ethylene-co-diethyl vinyl phosphonate) and poly(ethylene-co-vinyl phosphonic acid). In these copolymerizations, reversible coordination of the phosphonate moieties of free monomer as well as chelate formation by incorporated monomer retards chain growth as also evidenced by relative binding studies of diethyl phosphonate towards 1. Post-polymerization emulsification of poly(ethylene-co-vinyl phosphonic acid) together with CdSe/CdS quantum dots (QDs) yields submicron (ca. 50 nm from dynamic light scattering (DLS) and transmission electron microscopy (TEM)) polymer particles with the QDs embedded in the functionalized polyethylene in a nonaggregated fashion. This embedding benefits the fluorescence behavior in terms of continuous emission and life-time as revealed by wide-field fluorescence measurements. These composite particle dispersions are employed as a ″masterbatch" together with an aqueous high density polyethylene (HDPE) dispersion to generate thin films (by spin-coating) and bulk materials (from the melt), respectively, in which the inorganic nanoparticles remain highly disperse. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Thermodynamics and kinetics of thermal decomposition of dibutylalkyl and dipentylalkyl phosphonate-nitric acid systems

    International Nuclear Information System (INIS)

    Chandran, K.; Brahmananda, C.V.S.; Anthonysamy, S.; Srinivasan, T.G.; Ganesan, V.

    2013-01-01

    Tributyl phosphate (TBP) is used in the reprocessing industry for the separation of uranium and plutonium from the spent nuclear fuels by PUREX process. A variety of dialkylalky/phosphonates were synthesised and their extraction behaviour on actinides was studied in this laboratory. The superior extraction characteristics of phosphonates make them useful for several metal recovery applications in the nuclear fuel cycle. However, higher solubility of phosphonates in aqueous phase as compared to TBP, introduces higher chances of the formation of thermally active 'red oil' like substances during the evaporation of aqueous streams. Thermal stability of neat and nitric acid solvated homologues of four dibutylalkyl phosphonates namely, dibutylpropyl phosphonate (DBPrP), dibutylbutyl phosphonate (DBBP), dibutylpentyl phosphonate (DBPP), dibutylhexyl phosphonate (DBHeP), and two dipentylalkyl phosphonates viz. dipentylbutyl phosphonate (DPBP), dipentylhexyl phosphonate (DPHeP) were studied. Experiments were conducted using an adiabatic calorimeter in heat-wait-search mode. Various stoichiometry of nitric acid-solvated DBalP and DPalP were prepared by equilibrating the respective organic with 4-15.6 M nitric acid followed by separation. Neat DBalP and DPalP are stable up to the temperature of ∼ 555 K while their acid-solvates decomposed in the temperature range 380-403 K. The results also indicated that the presence of nitric acid accelerated the decomposition of phosphonates. Decomposition of these acid solvated phosphonates is found to be exothermic and follows first order kinetics. The onset temperature, adiabatic temperature rise, pressure rise, decomposition enthalpy and activation energy were found to strongly depend on the nitric acid content of the acid-solvates. The studies also indicate that dibutylalkyl and dipentylalkyl phosphonates are also prone to form 'red oil' like substances under extreme conditions and can lead to run-away reactions

  8. The use of cross-linked chitosan beads for nutrients (nitrate and orthophosphate) removal from a mixture of P-PO4, N-NO2 and N-NO3.

    Science.gov (United States)

    Jóźwiak, Tomasz; Filipkowska, Urszula; Szymczyk, Paula; Kuczajowska-Zadrożna, Małgorzata; Mielcarek, Artur

    2017-11-01

    A hydrogel chitosan sorbent ionically cross-linked with sodium citrate and covalently cross-linked with epichlorohydrin was used to remove nutrients from an equimolar mixture of P-PO 4 , N-NO 2 and N-NO 3 . The scope of the study included, among other things, determination of the influence of pH on nutrient sorption effectiveness, nutrient sorption kinetics as well as determination of the maximum sorption capacity of cross-linked chitosan sorbents regarding P-PO 4 (H 2 PO 4 - , HPO 4 2- ), N-NO 2 (HNO 2 , NO 2 - ), and N-NO 3 (NO 3 - ). The effect of the type of the cross-linking agent on the affinity of the modified chitosan to each nutrient was studied as well. The kinetics of nutrient sorption on the tested chitosan sorbents was best described with the pseudo-second order model. The model of intramolecular diffusion showed that P-PO 4 , N-NO 2 and N-NO3 sorption on cross-linked hydrogel chitosan beads proceeded in two phases. The best sorbent of nutrients turned out to be chitosan cross-linked covalently with epichlorohydrin; with P-PO 4 , N-NO 2 and N-NO 3 sorption capacity reaching: 1.23, 0.94 and 0.76mmol/g, respectively (total of 2.92mmol/g). For comparison, the sorption capacity of chitosan cross-linked ionically with sodium citrate was: 0.43, 0.39 and 0.39mmol/g for P-PO 4 , N-NO 2 and N-NO 3 , respectively (total of 1.21mmol/g). Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Photocatalytic degradation of methylene blue by C 3 N 4 /ZnO

    Indian Academy of Sciences (India)

    The photocatalytic activities of prepared samples were investigated under the illumination of blacklight and fluorescent lamps as the low wattage light source. The C 3 N 4 /ZnO showed a better photocatalytic activity than ZnO to degrade a methylene blue (MB) dye solution using blacklight lamps, but there is no significant ...

  10. Interactions between chitosan and cells measured by AFM

    Energy Technology Data Exchange (ETDEWEB)

    Hsiao, Sheng-Wen; Thien, Doan Van Hong; Ho, Ming-Hua [Department of Chemical Engineering, National Taiwan University of Science and Technology, Taipei 10617, Taiwan (China); Hsieh, Hsyue-Jen [Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan (China); Li, Chung-Hsing [Division of Orthodontics and Pediatric Dentistry, Department of Dentistry, Tri-Service General Hospital, Taipei, Taiwan (China); Hung, Chang-Hsiang [Department of Dentistry, Kinmen Hospital Department of Health, Taiwan (China); Li, Hsi-Hsin, E-mail: mhho@mail.ntust.edu.t [Deputy Superintendent, Kinmen Hospital Department of Health, Taiwan (China)

    2010-10-01

    Chitosan, a biocompatible material that has been widely used in bone tissue engineering, is believed to have a high affinity to osteoblastic cells. This research is the first to prove this hypothesis. By using atomic force microscopy (AFM) with a chitosan-modified cantilever, quantitative evaluation of the interforce between chitosan and cells was carried out. A chitosan tip functionalized with Arg-Gly-Asp (RGD) was also used to measure the interforce between RGD-chitosan and osteoblastic cells. This research concluded by examining cell adhesion and spreading of chitosan substrates as further characterization of the interactions between cells and chitosan. The force measured by AFM showed that the interforce between chitosan and osteoblasts was the highest (209 nN). The smallest adhesion force (61.8 nN) appeared between chitosan and muscle fibroblasts, which did not demonstrate any osteoblastic properties. This result proved that there was a significant interaction between chitosan and bone cells, and correlated with the observations of cell attachment and spreading. The technique developed in this research directly quantified the adhesion between chitosan and cells. This is the first study to demonstrate that specific interaction exists between chitosan and osteoblasts.

  11. Interactions between chitosan and cells measured by AFM

    International Nuclear Information System (INIS)

    Hsiao, Sheng-Wen; Thien, Doan Van Hong; Ho, Ming-Hua; Hsieh, Hsyue-Jen; Li, Chung-Hsing; Hung, Chang-Hsiang; Li, Hsi-Hsin

    2010-01-01

    Chitosan, a biocompatible material that has been widely used in bone tissue engineering, is believed to have a high affinity to osteoblastic cells. This research is the first to prove this hypothesis. By using atomic force microscopy (AFM) with a chitosan-modified cantilever, quantitative evaluation of the interforce between chitosan and cells was carried out. A chitosan tip functionalized with Arg-Gly-Asp (RGD) was also used to measure the interforce between RGD-chitosan and osteoblastic cells. This research concluded by examining cell adhesion and spreading of chitosan substrates as further characterization of the interactions between cells and chitosan. The force measured by AFM showed that the interforce between chitosan and osteoblasts was the highest (209 nN). The smallest adhesion force (61.8 nN) appeared between chitosan and muscle fibroblasts, which did not demonstrate any osteoblastic properties. This result proved that there was a significant interaction between chitosan and bone cells, and correlated with the observations of cell attachment and spreading. The technique developed in this research directly quantified the adhesion between chitosan and cells. This is the first study to demonstrate that specific interaction exists between chitosan and osteoblasts.

  12. Chitosan nanoparticles from marine squid protect liver cells against N-diethylnitrosoamine-induced hepatocellular carcinoma.

    Science.gov (United States)

    Subhapradha, Namasivayam; Shanmugam, Vairamani; Shanmugam, Annaian

    2017-09-01

    Rationale of this study was framed to investigate the protective effect and anti-cancer property of nanoparticles based on chitosan isolated from squid, Sepioteuthis lessoniana, on hepatic cells in N-Nitrosodiethylamine-induced hepatocellular carcinoma in rats. The results conferred that the chitosan nanoparticle supplementation had a protective effect on liver cells by reducing the levels of marker enzymes and bilirubin and thus increasing the albumin levels. The level of reduced glutathione, ascorbic acid and α-tocopherol significantly increased in both post- and pre-treatment with chitosan nanoparticles. The levels of antioxidant enzymes were enhanced and lipid peroxidation products were diminished while treating nitrosodiethylamine-induced hepatocellular carcinoma with chitosan nanoparticles. Supplementation of chitosan nanoparticles had potent anti-hyperlipidemic property that was evidenced by monitoring the serum lipid levels and its components. Animals pre-treated with chitosan nanoparticles along with nitrosodiethylamine showed a significant reduction in the total cholesterol and triglycerides levels with increase in the levels of phospholipids and free fatty acids. Chitosan nanoparticles treated rats showed significant increment in high-density lipoprotein cholesterol and reduction in low-density lipoprotein and very low-density lipoprotein cholesterol when compared with levels in nitrosodiethylamine-induced hepatocellular carcinoma. Nitrosodiethylamine-induced carcinoma changes on circulation and hepatic antioxidant defense mechanism were regulated by chitosan nanoparticles, concluding that the chitosan nanoparticles have a potent protective effect on liver cells which might be due to its robust antioxidant and anti-lipidemic property. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Polyphosphonate induced coacervation of chitosan: Encapsulation of proteins/enzymes and their biosensing

    International Nuclear Information System (INIS)

    Liu, Hailing; Cui, Yanyun; Li, Pan; Zhou, Yiming; Chen, Yu; Tang, Yawen; Lu, Tianhong

    2013-01-01

    Graphical abstract: Based on the coacervation of chitosan via the ionotropic crosslinking interaction, proteins/enzymes can be encapsulated in situ into chitosan matrix. -- Highlights: •The ionotropic crosslinking interactions result in the coacervation of chitosan. •A phosphonate-assisted encapsulation of proteins in chitosan matrix is introduced. •The encapsulated proteins retain their bioactivity. •The encapsulation method can be used to fabricate various chitosan-based biosensors. -- Abstract: Based on the polyphosphonate-assisted coacervation of chitosan, a simple and versatile procedure for the encapsulation of proteins/enzymes in chitosan–carbon nanotubes (CNTs) composites matrix was developed. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), energy dispersive spectrum (EDS) mapping demonstrated the hemoglobin (Hb) uniformly distributed into chitosan–CNTs composites matrix. Raman measurements indicated the CNTs in composites matrix retained the electronic and structural integrities of the pristine CNTs. Fourier transform infrared (FT-IR), ultraviolet–visible (UV–vis) and circular dichroism (CD) spectroscopy displayed the encapsulated Hb preserved their near-native structure, indicating the polyphosphonate–chitosan–CNTs composites possessed excellent biocompatibility for the encapsulation of proteins/enzymes. Electrochemical measurements indicated the encapsulated Hb could directly exchange electron with the substrate electrode. Moreover, the modified electrode showed excellent bioelectrocatalytic activity for the reduction of hydrogen peroxide. Under optimum experimental conditions, the fabricated electrochemical sensor displayed the fast response (less than 3 s), wide linear range (7.0 × 10 −7 to 2.0 × 10 −3 M) and low detection limit (4.0 × 10 −7 M) for the determination of hydrogen peroxide. This newly developed protocol was simple and mild and would certainly

  14. Polyphosphonate induced coacervation of chitosan: Encapsulation of proteins/enzymes and their biosensing

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hailing; Cui, Yanyun; Li, Pan; Zhou, Yiming; Chen, Yu, E-mail: ndchenyu@yahoo.cn; Tang, Yawen; Lu, Tianhong

    2013-05-07

    Graphical abstract: Based on the coacervation of chitosan via the ionotropic crosslinking interaction, proteins/enzymes can be encapsulated in situ into chitosan matrix. -- Highlights: •The ionotropic crosslinking interactions result in the coacervation of chitosan. •A phosphonate-assisted encapsulation of proteins in chitosan matrix is introduced. •The encapsulated proteins retain their bioactivity. •The encapsulation method can be used to fabricate various chitosan-based biosensors. -- Abstract: Based on the polyphosphonate-assisted coacervation of chitosan, a simple and versatile procedure for the encapsulation of proteins/enzymes in chitosan–carbon nanotubes (CNTs) composites matrix was developed. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), energy dispersive spectrum (EDS) mapping demonstrated the hemoglobin (Hb) uniformly distributed into chitosan–CNTs composites matrix. Raman measurements indicated the CNTs in composites matrix retained the electronic and structural integrities of the pristine CNTs. Fourier transform infrared (FT-IR), ultraviolet–visible (UV–vis) and circular dichroism (CD) spectroscopy displayed the encapsulated Hb preserved their near-native structure, indicating the polyphosphonate–chitosan–CNTs composites possessed excellent biocompatibility for the encapsulation of proteins/enzymes. Electrochemical measurements indicated the encapsulated Hb could directly exchange electron with the substrate electrode. Moreover, the modified electrode showed excellent bioelectrocatalytic activity for the reduction of hydrogen peroxide. Under optimum experimental conditions, the fabricated electrochemical sensor displayed the fast response (less than 3 s), wide linear range (7.0 × 10{sup −7} to 2.0 × 10{sup −3} M) and low detection limit (4.0 × 10{sup −7} M) for the determination of hydrogen peroxide. This newly developed protocol was simple and mild and

  15. Characterization of bioactive chitosan and sulfated chitosan from Doryteuthis singhalensis (Ortmann, 1891).

    Science.gov (United States)

    Ramasamy, Pasiyappazham; Subhapradha, Namasivayam; Thinesh, Thangadurai; Selvin, Joseph; Selvan, Kanagaraj Muthamizh; Shanmugam, Vairamani; Shanmugam, Annaian

    2017-06-01

    Chitosan was extracted from the pen of squid Doryteuthis singhalensis and characterized using FT-IR, NMR, CHN, SEM and DSC analysis. Purified chitosan was sulfated with chlorosulfonic acid in N,N-dimethylformamide and the added sulfate group was confirmed with FT-IR analysis. The molecular weight and degree of deacetylation (DDA) of chitosan was found 226.6kDa and 83.76% respectively. Chitosan exhibited potent antioxidant activity evidenced by reducing power, chelating ability on ferrous ions and scavenging activity on DPPH, superoxide and hydroxyl radicals. The anticoagulant assay using activated partial thromboplastin time (APTT) and prothrombin time (PT) showed chitosan as a strong anticoagulant. The results of this study showed possibility of using D. singhalensis pen as a non-conventional source of natural antioxidants and anticoagulant which can be incorporated in functional food formulations. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. N-Branched acyclic nucleoside phosphonates as monomers for the synthesis of modified oligonucleotides

    Czech Academy of Sciences Publication Activity Database

    Hocková, Dana; Rosenbergová, Šárka; Ménová, Petra; Páv, Ondřej; Pohl, Radek; Novák, Pavel; Rosenberg, Ivan

    2015-01-01

    Roč. 13, č. 15 (2015), s. 4449-4458 ISSN 1477-0520 R&D Projects: GA ČR GAP207/11/0108; GA ČR GA13-26526S Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonates * oligonucleotides * solid phase synthesis Subject RIV: CC - Organic Chemistry Impact factor: 3.559, year: 2015

  17. Reactions of acetylenes with hypophosphorous and phosphonous acids

    International Nuclear Information System (INIS)

    Nifant'ev, E.E.; Solovetskaya, L.A.; Maslennikova, V.I.; Magdeeva, R.K.; Sergeev, N.M.

    1986-01-01

    Alkenylphosphonous, alkenylphosphinic, and alkylenebisphosphinic acids were prepared for the first time. The course of the hydrophosphorylation of 1-alkynes depends on the form of the reagent used. The homolytic hydrophosphorylation of acetylenes with hypophosphorous acid proceeds mainly with the participation of one molecule of the acid. The addition of phosphonous acids to acetylenic hydrocarbons leads to both mono- and di-phosphorylated adducts. The nature of the phosphonous acid taken has a substantial influence on the readiness with which the alkylenebisphosphinic acids are formed. Study of the stereoselectivity of the reactions showed that in the case of the monoaddition of hypophosphorous and phosphonous acids to acetylenes mixtures of cis and trans isomeric products are always formed. Phosphorous 31 and carbon 13 NMR spectra are analyzed

  18. Crystal structure of the complex of carboxypeptidase A with a strongly bound phosphonate in a new crystalline form: comparison with structures of other complexes.

    Science.gov (United States)

    Kim, H; Lipscomb, W N

    1990-06-12

    O-[[(1R)-[[N-(Phenylmethoxycarbonyl)-L-alanyl]amino]ethyl] hydroxyphosphinyl]-L-3-phenyllacetate [ZAAP(O)F], an analogue of (benzyloxycarbonyl)-Ala-Ala-Phe or (benzyloxycarbonyl)-Ala-Ala-phenyllactate, binds to carboxypeptidase A with great affinity (Ki = 3 pM). Similar phosphonates have been shown to be transition-state analogues of the CPA-catalyzed hydrolysis [Hanson, J. E., Kaplan, A. P., & Bartlett, P. A. (1989) Biochemistry 28, 6294-6305]. In the present study, the structure of the complex of this phosphonate with carboxypeptidase A has been determined by X-ray crystallography to a resolution of 2.0 A. The complex crystallizes in the space group P2(1)2(1)2(1) with cell dimensions a = 61.9 A, b = 67.2 A, and c = 76.2 A. The structure of the complex was solved by molecular replacement. Refinement of the structure against 20,776 unique reflections between 10.0 and 2.0 A yields a crystallographic residual of 0.193, including 140 water molecules. The two phosphinyl oxygens of the inhibitor bind to the active-site zinc at 2.2 A on the electrophilic (Arg-127) side and 3.1 A on the nucleophilic (Glu-270) side. Various features of the binding mode of this phosphonate inhibitor are consistent with the hypothesis that carboxypeptidase A catalyzed hydrolysis proceeds through a general-base mechanism in which the carbonyl carbon of the substrate is attacked by Zn-hydroxyl (or Zn-water). An unexpected feature of the bound inhibitor, the cis carbamoyl ester bond at the benzyloxycarbonyl linkage to alanine, allows the benzyloxycarbonyl phenyl ring of the inhibitor to interact favorably with Tyr-198. This complex structure is compared with previous structures of carboxypeptidase A, including the complexes with the potato inhibitor, a hydrated keto methylene substrate analogue, and a phosphonamidate inhibitor. Comparisons are also made with the complexes of thermolysin with some phosphonamidate inhibitors.

  19. Gas chromatography-mass spectrometric studies of O-alkyl O-2-(N,N-dialkylamino) ethyl alkylphosphonites(phosphonates) for chemical weapons convention verification.

    Science.gov (United States)

    Saeidian, Hamid; Babri, Mehran; Ramezani, Atefeh; Ashrafi, Davood; Sarabadani, Mansour; Naseri, Mohammad Taghi

    2013-01-01

    The electron ionization (EI) mass spectra of a series of O-alkyl O-2-(N,N-dialkylaminolethyl alkylphosphonites(phosphonates), which are precursors of nerve agents, were studied for Chemical Weapons Convention (CWC) verification. General El fragmentation pathways were constructed and discussed. Proposed fragment structures were confirmed through analyzing fragment ions of deuterated analogs and density functional theory (DFT) calculations. The observed fragment ions are due to different fragmentation pathways such as hydrogen and McLafferty+1 rearrangements, alkene, amine and alkoxy elimination by alpha- or beta-cleavage process. Fragment ions distinctly allow unequivocal identification of the interested compounds including those of isomeric compounds. The presence and abundance of fragment ions were found to depend on the size and structure of the alkyl group attached to nitrogen, phosphorus and oxygen atoms.

  20. Methyleneation of peptides by N,N,N,N-tetramethylethylenediamine (TEMED) under conditions used for free radical polymerization: a mechanistic study.

    Science.gov (United States)

    Shirangi, Mehrnoosh; Sastre Toraño, Javier; Sellergren, Börje; Hennink, Wim E; Somsen, Govert W; van Nostrum, Cornelus F

    2015-01-21

    Free radical polymerization is often used to prepare protein and peptide-loaded hydrogels for the design of controlled release systems and molecular imprinting materials. Peroxodisulfates (ammonium peroxodisulfates (APS) or potassium peroxodisulfates (KPS)) with N,N,N,N-tetramethylethylenediamine (TEMED) are frequently used as initiator and catalyst. However, exposure to these free radical polymerization reagents may lead to modification of the protein and peptide. In this work, we show the modification of lysine residues by ammonium peroxodisulfate (APS)/TEMED of the immunostimulant thymopentin (TP5). Parallel studies on a decapeptide and a library of 15 dipeptides were performed to reveal the mechanism of modification. LC-MS of APS/TEMED-exposed TP5 revealed a major reaction product with an increased mass (+12 Da) with respect to TP5. LC-MS(2) and LC-MS(3) were performed to obtain structural information on the modified peptide and localize the actual modification site. Interpretation of the obtained data demonstrates the formation of a methylene bridge between the lysine and arginine residue in the presence of TEMED, while replacing TEMED with a sodium bisulfite catalyst did not show this modification. Studies with the other peptides showed that the TEMED radical can induce methyleneation on peptides when lysine is next to arginine, proline, cysteine, aspargine, glutamine, histidine, tyrosine, tryptophan, and aspartic acid residues. Stability of peptides and protein needs to be considered when using APS/TEMED in in situ polymerization systems. The use of an alternative catalyst such as sodium bisulfite may preserve the chemical integrity of peptides during in situ polymerization.

  1. Hydrothermal synthesis, crystal structure and properties of a novel chain coordination polymer constructed by tetrafunctional phosphonate anions and cobalt ions

    International Nuclear Information System (INIS)

    Guan, Lei; Wang, Ying

    2015-01-01

    A novel cobalt phosphonate, [Co(HL)(H 2 O) 3 ] n (1) (L=N(CH 2 PO 3 H) 3 3− ) has been synthesized by hydrothermal reaction at 150 °C and structurally characterized by X-ray diffraction, infrared spectroscopy, elemental and thermogravimetric analysis. Complex 1 features a 1D chain structure with double-channel built from CoO 6 octahedra bridged together by the phosphonate groups. Each cobalt ion is octahedrally coordinated by three phosphonate oxygen atoms and three water molecules. The coordinated water molecules can form the hydrogen bonds with the phosphonate oxygen atoms to link the 1D chains, building a 2D layered structure, further resulting in a 3D network. The luminescence spectrum indicates an emission maximum at 435 nm. The magnetic susceptibility curve exhibits a dominant antiferromagnetic behavior with a weakly ferromagnetic component at low temperatures. - Graphical abstract: The connectivity between cobalt ions and the ligands results in a chain structure with a 1D double-channel structure, which is constructed by A-type subrings and B-type subrings. - Highlights: • The tetrafunctional phosphonate ligand was used as the ligand. • A novel chain structure can be formed by A-type rings and B-type rings. • Two types of rings can form a 1D double-channel structure, along the c-axis

  2. Actinide phosphonate complexes in aqueous solutions

    International Nuclear Information System (INIS)

    Nash, K.L.

    1993-01-01

    Complexes formed by actinides with carboxylic acids, polycarboxylic acids, and aminopolycarboxylic acids play a central role in both the basic and process chemistry of the actinides. Recent studies of f-element complexes with phosphonic acid ligands indicate that new ligands incorporating doubly ionizable phosphonate groups (-PO 3 H 2 ) have many properties which are unique chemically, and promise more efficient separation processes for waste cleanup and environmental restoration. Simple diphosphonate ligands form much stronger complexes than isostructural carboxylates, often exhibiting higher solubility as well. In this manuscript recent studies of the thermodynamics and kinetics of f-element complexation by 1,1 and 1,2 diphosphonic acid ligands are described

  3. New N-Acetyltransferase Fold in the Structure and Mechanism of the Phosphonate Biosynthetic Enzyme FrbF

    Energy Technology Data Exchange (ETDEWEB)

    Bae, Brian; Cobb, Ryan E.; DeSieno, Matthew A.; Zhao, Huimin; Nair, Satish K. (UIUC)

    2015-10-15

    The enzyme FrbF from Streptomyces rubellomurinus has attracted significant attention due to its role in the biosynthesis of the antimalarial phosphonate FR-900098. The enzyme catalyzes acetyl transfer onto the hydroxamate of the FR-900098 precursors cytidine 5'-monophosphate-3-aminopropylphosphonate and cytidine 5'-monophosphate-N-hydroxy-3-aminopropylphosphonate. Despite the established function as a bona fide N-acetyltransferase, FrbF shows no sequence similarity to any member of the GCN5-like N-acetyltransferase (GNAT) superfamily. Here, we present the 2.0 {angstrom} resolution crystal structure of FrbF in complex with acetyl-CoA, which demonstrates a unique architecture that is distinct from those of canonical GNAT-like acetyltransferases. We also utilized the co-crystal structure to guide structure-function studies that identified the roles of putative active site residues in the acetyltransferase mechanism. The combined biochemical and structural analyses of FrbF provide insights into this previously uncharacterized family of N-acetyltransferases and also provide a molecular framework toward the production of novel N-acyl derivatives of FR-900098.

  4. Catalytic phosphonation of high performance polymers and POSS. Novel components for polymer blend and nanocomposite fuel cell membranes

    Energy Technology Data Exchange (ETDEWEB)

    Bock, T.R.

    2006-10-15

    Aim of this thesis was the preparation and evaluation of phosphonated high performance (HP) polyelectrolytes and polyhedral oligomeric silsesquioxanes (POSS) for polyelectrolyte membrane fuel cell (PEMFC) application. Brominated derivatives of the commercial high performance (HP) polymers poly(ethersulfone) (PES), poly(etheretherketone) (PEEK), poly(phenylsulfone) (PPSu), poly(sulfone) (PSU) and of octaphenyl-POSS of own production were phosphonated by Ni-catalysed Arbuzov reaction. Phosphonated PSU was cast into pure and blend films with sulfonated PEEK (s-PEEK) to investigate H+-conductivity, water uptake and film morphology. Blend films' properties were referenced to films containing unmodified blend partners. Solution-compounding of phosphonated octaphenyl-POSS and s-PEEK was used to produce novel nanocomposite films. An in-situ zirconisation method was assessed as convenient strategy for novel ionically crosslinked membranes of enhanced swelling resistance. Dibromo isocyanuric acid (DBI) and N-bromo succinimide (NBS) as brominating agents allowed polymer analogous preparation of the novel brominated PES and PEEK with precise reaction control. A random distribution of functional groups, i.e. polyelectrolytes' microstructural homogeneity was revealed as decisive factor concerning solubility of phosphonated PSU. Brominated phT8 was prepared with Br2 by a high temperature approach in tetrachloroethane (TCE). Brominated polymers were phosphonated by Ni-catalysis in non-coordinating high temperature solvents, such as diphenylether, benzophenone and diphenylsulfone without notable solvent influence. The lack of solvent - catalyst complexes and high reaction temperatures of 180-200 C led to halogen-free phosphonates with unprecedented high functionalities. Polymer analogous application of P(OSiMe3)3 offered a novel direct access to easily cleavable disilyl ester derivatives. These were obtained from PEEK and PSU in near quantitative yields at NiCl2-loads as

  5. Extraction of uranium from aqueous solution by phosphonic acid-imbedded polyurethane foam

    International Nuclear Information System (INIS)

    Katragadda, S.; Gesser, H.D.; Chow, A.

    1997-01-01

    Phenylphosphonic acid was imbedded into the matrix of the polyurethane foam during the fabrication process of the polymer. The extraction of uranium by phosphonic acid-imbedded polyurethane foam and blank polyurethane (i.e., foam without phosphonic acid functional groups) was investigated. Phosphonic acid-imbedded foam showed superior extractability of uranium from solutions with pH = 7.0 ± 1.5 over a wide range of temperatures. (author)

  6. Transport mechanism of chitosan-N-acetylcysteine, chitosan oligosaccharides or carboxymethyl chitosan decorated coumarin-6 loaded nanostructured lipid carriers across the rabbit ocular.

    Science.gov (United States)

    Li, Jinyu; Tan, Guoxin; Cheng, Bingchao; Liu, Dandan; Pan, Weisan

    2017-11-01

    To facilitate the hydrophobic drugs modeled by coumarin-6 (Cou-6) acrossing the cornea to the anterior chamber of the rabbit eye, chitosan (CS) derivatives including chitosan-N-acetyl-l-cysteine (CS-NAC), chitosan oligosaccharides (COS) and carboxymethyl chitosan (CMCS) modified nanostructured lipid carriers (NLCs) were designed and characterized. We found that, with similar size distribution and positivecharges, different CS derivatives based on NLCs led to distinctive delivery performance. In vivo precorneal retention study on rabbits revealed that these CS derivatives coating exhibited a stronger resistant effect than Cou-6 eye drops and Cou-6-NLC (P<0.05), moreover, the AUC (0-∞) , C max and MRT (0-∞) of them followed the sequence of CMCS-Cou-6-NLC

  7. Determination of the parameters of binding between lipopolysaccharide and chitosan and its N-acetylated derivative using a gravimetric piezoquartz biosensor.

    Science.gov (United States)

    Naberezhnykh, G A; Gorbach, V I; Kalmykova, E N; Solov'eva, T F

    2015-03-01

    The interaction of endotoxin (lipopolysaccharide - LPS) with low molecular weight chitosan (5.5 kDa), its N-acylated derivative and chitoliposomes was studied using a gravimetric piezoelectric quartz crystal microbalance biosensor. The optimal conditions for the formation of a biolayer based on immobilized LPS on the resonator surface and its regeneration were elaborated. The association and dissociation rate constants for LPS binding to chitosans were determined and the affinity constants (Kaf) were calculated based on the data on changes in the oscillation frequency of the quartz crystal resonator. The Kaf values correlated with the ones obtained using other methods. The affinity of N-acylated chitosan binding to LPS was higher than that of the parent chitosan binding to LPS. Based on the results obtained, we suggest that water-soluble N-acylated derivatives of chitosan with low degree of substitution of amino groups could be useful compounds for endotoxin binding and neutralization. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Alkyl phosphonic acids and sulfonic acids in the Murchison meteorite

    Science.gov (United States)

    Cooper, George W.; Onwo, Wilfred M.; Cronin, John R.

    1992-01-01

    Homologous series of alkyl phosphonic acids and alkyl sulfonic acids, along with inorganic orthophosphate and sulfate, are identified in water extracts of the Murchison meteorite after conversion to their t-butyl dimethylsilyl derivatives. The methyl, ethyl, propyl, and butyl compounds are observed in both series. Five of the eight possible alkyl phosphonic acids and seven of the eight possible alkyl sulfonic acids through C4 are identified. Abundances decrease with increasing carbon number as observed of other homologous series indigenous to Murchison. Concentrations range downward from approximately 380 nmol/gram in the alkyl sulfonic acid series, and from 9 nmol/gram in the alkyl phosphonic acid series.

  9. Controlled synthesis of N,N,N-trimethyl chitosan for modulated bioadhesion and nasal membrane permeability.

    Science.gov (United States)

    Pardeshi, Chandrakantsing V; Belgamwar, Veena S

    2016-01-01

    In an experiment to explore the bioadhesion, biocompatibility, and membrane permeation properties, the controlled synthesis of N,N,N-trimethyl chitosan (TMC) was carried out by two-step reductive methylation of chitosan (CHT). Methylation was confirmed by (1)H NMR (δ=3.1 ppm) and FTIR analysis (CH stretch at 1,485 cm(-1)). The TMC was further characterized by DSC, TGA, XRD, HR-TEM, SEM, and elemental analysis. Findings revealed improved solubility, enhanced viscosity, increased swelling index and higher molecular weight of TMC over CHT. Comparative evaluation validated increased bioadhesion potential, and improved ex vivo biocompatibility of TMC compared to CHT. Increased bioadhesion of TMC NPs over CHT NPs can be attributed to the strong electrostatic interactions between cationic amino groups with anionic sialic and sulfonic acid moieties contained in the mucin of the nasal mucus. Ex vivo biocompatibility studies suggested that the NP formulations of both biopolymers were biocompatible and could be applied safely on the nasal epithelium. Ex vivo permeation studies executed on excised cattle nasal mucosa illustrated improved permeability of TMC NPs over CHT NPs. In the author's opinion, two-step reductive methylation of CHT could be an attractive strategy to improve its solubility, bioadhesion, and permeation characteristics without affecting biocompatibility across the mucosal surfaces. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Geminal difunctionalization of α-diazo arylmethylphosphonates: synthesis of fluorinated phosphonates.

    Science.gov (United States)

    Zhou, Yujing; Zhang, Yan; Wang, Jianbo

    2016-11-08

    A general approach towards diverse fluorinated phosphonates via geminal difunctionalization reactions of α-diazo arylmethylphosphonates is described. The diazo functionality (RR'C[double bond, length as m-dash]N 2 ) is successfully converted to RR'CF 2 , RR'CHF, RR'CFBr or RR'CFNR'' 2 groups by employing different fluorination reagents. A variety of fluorinated organophosphorus compounds were readily accessed in good to excellent yields from a common type of precursor.

  11. Radiation-induced changes in carboxymethylated chitosan

    International Nuclear Information System (INIS)

    Huang Ling; Peng Jing; Zhai Maolin; Li Jiuqiang; Wei Genshuan

    2007-01-01

    This study focuses on the radiation effect of γ-ray on carboxymethylated chitosan (CM-chitosan) in solid state. The changes in molecular weight of CM-chitosan with absorbed dose were monitored by viscosity method. Experimental results indicated that random chain scissions took place under irradiation. Radiation chemical yield (G d ) of CM-chitosan in solid state with N 2 -saturated was 0.49, which showed CM-chitosan has high radiation stability. Biomaterials composed of CM-chitosan can be thought to sterilize with low absorbed dose. FTIR and UV spectra showed that main chain structures of CM-chitosan were retained, carbonyl/carboxyl groups were formed and partial amino groups were eliminated in high absorbed dose. XRD patterns identified that the degradation of CM-chitosan occurred mostly in amorphous region

  12. Ab initio computational study of –N-C and –O-C bonding formation : functional group modification reaction based chitosan

    Science.gov (United States)

    Siahaan, P.; Salimah, S. N. M.; Sipangkar, M. J.; Hudiyanti, D.; Djunaidi, M. C.; Laksitorini, M. D.

    2018-04-01

    Chitosan application in pharmaceutics and cosmeceutics industries is limited by its solubility issue. Modification of -NH2 and -OH fuctional groups of chitosan by adding carboxyl group has been shown to improve its solubility and application. Attempt to synthesize carboxymethyl chitosan (CMC) from monocloroacetic acid (MCAA) has been done prior this report. However no information is available wether –OH (-O-C bonding formation) or -NH2 (-N-C bonding formation) is the preference for - CH2COOH to attach. In the current study, the reaction mechanism between chitosan and MCAA reactants into carboxymethyl chitosan (CMC) was examined by computational approach. Dimer from of chitosan used as a molecular model in calculation All the molecular structure involved in the reaction mechanism was optimized by ab initio computational on the theory and basis set HF/6-31G(d,p). The results showed that the - N-C bonding formation via SN2 than the -O-C bonding formation via SN2 which have activation energy 469.437 kJ/mol and 533.219 kJ/mol respectively. However, the -O-C bonding formation more spontaneous than the -N-C bonding formation because ΔG the formation of O-CMC-2 reaction is more negative than ΔG of formation N-CMC-2 reaction is -4.353 kJ/mol and -1.095 kJ/mol respectively. The synthesis of N,O-CMC first forms -O-CH2COOH, then continues to form -NH-CH2COOH. This information is valuable to further optimize the reaction codition for CMC synthesis.

  13. One-Pot Facile Methodology to Synthesize Chitosan-ZnO-Graphene Oxide Hybrid Composites for Better Dye Adsorption and Antibacterial Activity

    Directory of Open Access Journals (Sweden)

    Anandhavelu Sanmugam

    2017-11-01

    Full Text Available Novel chitosan–ZnO–graphene oxide hybrid composites were prepared using a one-pot chemical strategy, and their dye adsorption characteristics and antibacterial activity were demonstrated. The prepared chitosan and the hybrids such as chitosan–ZnO and chitosan–ZnO–graphene oxide were characterized by UV-Vis absorption spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and transmission electron microscopy. The thermal and mechanical properties indicate a significant improvement over chitosan in the hybrid composites. Dye adsorption experiments were carried out using methylene blue and chromium complex as model pollutants with the function of dye concentration. The antibacterial properties of chitosan and the hybrids were tested against Gram-positive and Gram-negative bacterial species, which revealed minimum inhibitory concentrations (MICs of 0.1 µg/mL.

  14. Prolinol-based nucleoside phosphonic acids: new isosteric conformationally flexible nucleotide analogues

    Czech Academy of Sciences Publication Activity Database

    Vaněk, Václav; Buděšínský, Miloš; Rinnová, Markéta; Rosenberg, Ivan

    2009-01-01

    Roč. 65, č. 4 (2009), s. 862-876 ISSN 0040-4020 R&D Projects: GA ČR GA203/05/0827; GA MŠk(CZ) LC06077; GA MŠk LC512; GA MŠk(CZ) LC06061 Institutional research plan: CEZ:AV0Z40550506 Keywords : nucleotide analogues * phosphonates * prolinol derivatives * N- alkylation Subject RIV: CC - Organic Chemistry Impact factor: 3.219, year: 2009

  15. Synthesis and X-ray structures of dilithium complexes of the phosphonate anions [PhP(E)(N(t)Bu)(2)](2-) (E = O, S, Se, Te) and dimethylaluminum derivatives of [PhP(E)(N(t)Bu)(NH(t)Bu)](-) (E = S, Se).

    Science.gov (United States)

    Briand, Glen G; Chivers, Tristram; Krahn, Mark; Parvez, Masood

    2002-12-16

    The dilithium salts of the phosphonate dianions [PhP(E)(N(t)Bu)(2)](2-) (E = O, S, Se) are generated by the lithiation of [PhP(E)(NH(t)Bu)(2)] with n-butyllithium. The formation of the corresponding telluride (E = Te) is achieved by oxidation of [Li(2)[PhP(N(t)Bu)(2)

  16. Thermo-responsive wound dressings by grafting chitosan and poly(N-isopropylacrylamide) to plasma-induced graft polymerization modified non-woven fabrics

    International Nuclear Information System (INIS)

    Chen, Jyh-Ping; Kuo, Chang-Yi; Lee, Wen-Li

    2012-01-01

    Highlights: ► Poly(N-isopropylacrylamide) and chitosan were grafted to polypropylene non-wovens. ► An easily stripped off thermo-responsive wound dressing was developed. ► The wound dressing is biocompatible, has antibacterial and wound healing abilities. ► The bigraft non-woven will be a potential wound dressing for biomedical use. - Abstract: To obtain a chitosan wound dressings with temperature-responsive characteristics, polypropylene (PP) non-woven fabric (NWF) was modified by direct current pulsed oxygen plasma-induced grafting polymerization of acrylic acid (AAc) to improve hydrophilicity and to introduce carboxylic acid groups. Conjugation of chitosan and poly(N-isopropylacrylamide) (PNIPAAm) followed by using water-soluble carbodiimide as a coupling agent to form a novel bigraft PP-g-chitosan-g-PNIPAAm wound dressing. The amount of chitosan and PNIPAAm grafted to PP-g-chitosan-g-PNIPAAm were 83.0 ± 4.6 μg/cm 2 and 189.5 ± 8.2 μg/cm 2 , respectively. The surface chemical composition and microstructure of the NWF were studied by electron spectroscopy for chemical analysis (ESCA) and scanning electron microscopy (SEM). The linkages between AAc, chitosan, and PNIPAAm were confirmed with the formation of amide bonds. Physical properties of the NWF were characterized and potentials of these NWFs as wound dressings were evaluated using SD rat as the animal model. NWFs contained PNIPAAm were better than those contained only chitosan in wound healing rates and the wound areas covered by PP-g-chitosan-g-PNIPAAm wound dressings healed completely in 17 days.

  17. N,O6-partially acetylated chitosan nanoparticles hydrophobically-modified for controlled release of steroids and vitamin E

    DEFF Research Database (Denmark)

    Quinones, Javier Perez; Gothelf, Kurt Vesterager; Kjems, Jørgen

    2013-01-01

    Diosgenin, two synthetic analogs of brassinosteroids, testosterone and dl-α-tocopherol were covalently linked to synthetic water-soluble N,O6-partially acetylated chitosan, for their controlled release. Drug linking was confirmed by FTIR spectroscopy and proton NMR. Conjugates were also character......Diosgenin, two synthetic analogs of brassinosteroids, testosterone and dl-α-tocopherol were covalently linked to synthetic water-soluble N,O6-partially acetylated chitosan, for their controlled release. Drug linking was confirmed by FTIR spectroscopy and proton NMR. Conjugates were also...

  18. Phosphonates as alternative to tributyl phosphate for the separation of actinides from fission products

    International Nuclear Information System (INIS)

    Vyas, Chirag K.; Joshirao, Pranav M.; Manchanda, Vijay K.; Rao, C.V.S. Brahmmananda; Jayalakshmi, S.

    2015-01-01

    The present work investigates the role of increase in the basicity of organophosphorus extractant (dialkylalkyl phosphonates) on the uptake of actinides and fission products vis-a-vis tributyl phosphate (TBP), currently employed as a universal extractant. Two dialkylalkyl phosphonates viz. dibutylpropyl phosphonate (DBPrP) and dibutylpentyl phosphonate (DBPeP) were synthesized, characterized and evaluated for their solvent extraction behavior towards U(VI), Th(IV), Eu(III) and Tc(VII) in nitric acid medium ranging from 0.01-6 M. It was observed that increasing the basicity of the phosphoryl oxygen enhanced the uptake of the actinides and the distribution coefficient values were significantly larger as compared to TBP. The limiting organic concentration (LOC) value was estimated for Th(IV) for these extractants and compared with the TBP system. The separation factors of actinides with phosphonates over Tc(VII) are distinctly better than that with TBP.

  19. Microwave-assisted hydrolysis of phosphonate diesters: an efficient protocol for the preparation of phosphonic acids

    Czech Academy of Sciences Publication Activity Database

    Jansa, Petr; Baszczyňski, Ondřej; Procházková, Eliška; Dračínský, Martin; Janeba, Zlatko

    2012-01-01

    Roč. 14, č. 8 (2012), s. 2282-2288 ISSN 1463-9262 R&D Projects: GA MV VG20102015046 Institutional research plan: CEZ:AV0Z40550506 Keywords : acyclic nucleoside phosphonates * DNA virus * retrovirus infections * cidofovir * organic-synthesis Subject RIV: CC - Organic Chemistry Impact factor: 6.828, year: 2012

  20. Cytotoxicity and metal ions removal using antibacterial biodegradable hydrogels based on N-quaternized chitosan/poly(acrylic acid).

    Science.gov (United States)

    Mohamed, Riham R; Elella, Mahmoud H Abu; Sabaa, Magdy W

    2017-05-01

    Physically crosslinked hydrogels resulted from interaction between N,N,N-trimethyl chitosan chloride (N-Quaternized Chitosan) (NQC) and poly(acrylic acid) (PAA) were synthesized in different weight ratios (3:1), (1:1) and (1:3) taking the following codes Q3P1, Q1P1 and Q1P3, respectively. Characterization of the mentioned hydrogels was done using several analysis tools including; FTIR, XRD, SEM, TGA, biodegradation in simulated body fluid (SBF) and cytotoxicity against HepG-2 liver cancer cells. FTIR results proved that the prepared hydrogels were formed via electrostatic and H-bonding interactions, while XRD patterns proved that the prepared hydrogels -irrespective to their ratios- were more crystalline than both matrices NQC and PAA. TGA results, on the other hand, revealed that Q1P3 hydrogel was the most thermally stable compared to the other two hydrogels (Q3P1 and Q1P1). Biodegradation tests in SBF proved that these hydrogels were more biodegradable than the native chitosan. Examination of the prepared hydrogels for their potency in heavy metal ions removal revealed that they adsorbed Fe (III) and Cd (II) ions more than chitosan, while they adsorbed Cr (III), Ni (II) and Cu (II) ions less than chitosan. Moreover, testing the prepared hydrogels as antibacterial agents towards several Gram positive and Gram negative bacteria revealed their higher antibacterial activity as compared with NQC when used alone. Evaluating the cytotoxic effect of these hydrogels on an in vitro human liver cancer cell model (HepG-2) showed their good cytotoxic activity towards HepG-2. Moreover, the inhibition rate increased with increasing the hydrogels concentration in the culture medium. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. N-mercapto acetyl-N'-octyl-O, N″-glycol chitosan as an efficiency oral delivery system of paclitaxel.

    Science.gov (United States)

    Huo, Meirong; Fu, Ying; Liu, Yanhong; Chen, Qinyu; Mu, Yan; Zhou, Jianping; Li, Lingchao; Xu, Wei; Yin, Tingjie

    2018-02-01

    Herein, thioglycolic acid modified N-octyl-O, N'-glycol chitosan (N-mercapto acetyl-N'-octyl-O, N″-glycol chitosan, abbreviated as SH-OGC) was synthesized to improve the oral bioavailability of paclitaxel (PTX). PTX was readily solubilized into the hydrophobic inner core of SH-OGC. Pharmacokinetic studies demonstrated that the bioavailability of PTX was greatly enhanced when delivered by SH-OGC compared to Taxol ® or non-sulfhydrylated OGC micelles. Caco-2 cell experiments confirmed PTX or rhodamine-123-loaded SH-OGC demonstrated effective cellular accumulation via caveola-mediated endocytosis along with the inhibition of P-gp efflux. Furthermore, Caco-2 transport studies demonstrated that the mechanistic basis of SH-OGC efficacy was attributed to P-gp inhibition, enhanced permeability of tight junctions and clathrin-mediated transcytosis across the endothelium. In addition, SH-OGC exhibited increased intestinal retention through thiol-mediated mucoadhesion compared with OGC according to results of mucoadhesion evaluation on freshly excised rat intestine. In summary, SH-OGC micelles may present as a promising delivery vehicle for enhancing the oral bioavailability of P-gp substrates. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Chitosan-edible oil based materials as upgraded adsorbents for textile dyes.

    Science.gov (United States)

    Dos Santos, Clayane Carvalho; Mouta, Rodolpho; Junior, Manoel Carvalho Castro; Santana, Sirlane Aparecida Abreu; Silva, Hildo Antonio Dos Santos; Bezerra, Cícero Wellington Brito

    2018-01-15

    Biopolymer chitosan is a low cost, abundant, environmentally friendly, very selective and efficient anionic dyes adsorbent, being a promising material for large-scale removal of dyes from wastewater. However, raw chitosan (CS) is an ineffective cationic dyes adsorbent and its performance is pH sensitive, thus, CS modifications that address these issues need to be developed. Here, we report the preparation and characterization of two new CS modifications using edible oils (soybean oil or babassu oil), and their adsorption performance for two dyes, one anionic (remazol red, RR) and one cationic (methylene blue, MB). Both modifications extended the pH range of RR adsorption. The babassu oil modification increased adsorption capacity of the cationic dye MB, whereas the soybean oil modification increased that of RR. Such improvements demonstrate the potential of these two new CS modifications as adsorbent candidates for controlling dyes pollution in effluents. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Selective extraction of hydrocarbons, phosphonates and phosphonic acids from soils by successive supercritical fluid and pressurized liquid extractions.

    Science.gov (United States)

    Chaudot, X; Tambuté, A; Caude, M

    2000-01-14

    Hydrocarbons, dialkyl alkylphosphonates and alkyl alkylphosphonic acids are selectively extracted from spiked soils by successive implementation of supercritical carbon dioxide, supercritical methanol-modified carbon dioxide and pressurized water. More than 95% of hydrocarbons are extracted during the first step (pure supercritical carbon dioxide extraction) whereas no organophosphorus compound is evidenced in this first extract. A quantitative extraction of phosphonates is achieved during the second step (methanol-modified supercritical carbon dioxide extraction). Polar phosphonic acids are extracted during a third step (pressurized water extraction) and analyzed by gas chromatography under methylated derivatives (diazomethane derivatization). Global recoveries for these compounds are close to 80%, a loss of about 20% occurring during the derivatization process (co-evaporation with solvent). The developed selective extraction method was successfully applied to a soil sample during an international collaborative exercise.

  4. C-H Phosphonation of Pyrrolopyrimidines: Synthesis of Substituted 7-and 9-Deazapurine-8-phosphonate Derivatives

    Czech Academy of Sciences Publication Activity Database

    Sabat, Nazarii; Poštová Slavětínská, Lenka; Klepetářová, Blanka; Hocek, Michal

    2016-01-01

    Roč. 81, č. 19 (2016), s. 9507-9514 ISSN 0022-3263 R&D Projects: GA ČR(CZ) GA16-00178S; GA MŠk(CZ) LO1304 Institutional support: RVO:61388963 Keywords : cross - coupling reactions * acyclic nucleoside phosphonates * biological activity Subject RIV: CC - Organic Chemistry Impact factor: 4.849, year: 2016

  5. Synthesis of tritium labelled phosphonate analogues of sphinganine-1-phosphate

    International Nuclear Information System (INIS)

    Schick, Andreas; Schwarzmann, Guenter; Kolter, Thomas; Sandhoff, Konrad

    1997-01-01

    Tritiated phosphonate analogues 9 and 10 are prepared as analogues of sphinganine-1-phosphate 4. The key step in this synthesis is the catalytic tritiation of the triple bond in reduction of the protected diethyl-3-(S)-tert.-butoxycarbonylamino -4-hydroxy-5-tridecinyl-1-phosphonate by means of sodium boro[ 3 H]hydride as tritium source. These compounds are synthesized to study their metabolic stability and to evaluate their biological properties. (author)

  6. Antioxidant and antimutagenic activity of N-(2-carboxyethyl)chitosan

    International Nuclear Information System (INIS)

    Kogan, Grigorij; Skorik, Yury A.; Zitnanova, Ingrid; Krizkova, Livia; Durackova, Zdenka; Gomes, Carlos A.R.; Yatluk, Yury G.; Krajcovic, Juraj

    2004-01-01

    The antioxidant and antimutagenic activities of the novel carboxyethyl derivatives of chitosan with three different degrees of substitution have been assayed in vitro in the unicellular flagellate Euglena gracilis subjected to the action of genotoxic agents acridine orange and ofloxacin. It has been demonstrated that chitosan derivatives exhibit concentration-dependent protective antigenotoxic activity against both mutagens. It is suggested that different mechanisms may be involved in its protective action--antioxidant activity in case of ofloxacin-induced DNA damage, as well as possible interaction with the cell membrane that prevents acridine orange from reaching the genetic compartments and subsequent damaging DNA through intercalative binding. Direct adsorption of acridine orange on chitosan derivatives was ruled out as a possible mechanism of protection on the basis of spectrophotometric measurements. Dependence of the antimutagenic properties of the studied chitosan derivatives on the degree of substitution was reversed in experiments involving acridine orange and ofloxacin, which also indicated different mechanisms of protection involved in these two cases

  7. Anti-HIV therapy with AZT prodrugs: AZT phosphonate derivatives, current state and prospects.

    Science.gov (United States)

    Khandazhinskaya, Anastasiya; Matyugina, Elena; Shirokova, Elena

    2010-06-01

    AIDS, a disease caused by human immunodeficiency virus, was called 'plague of the twentieth century'. 3'-Azido-3'-deoxythymidine (AZT), the first compound approved for the treatment of HIV, is still a mandatory component of treatment schemes. However, its toxicity stimulated a search for new agents. This review presents the history and current state of the design of AZT prodrugs based on its phosphonate derivatives. Although every effort was made to include as many AZT structures bearing phosphonate residues and demonstrate the variety they offer, we also concentrated on the studies performed in our laboratory. Special attention was also paid to AZT 5'-H-phosphonate (phosphazide, Nikavir) approved in the Russian Federation as a drug for the prevention and treatment of HIV infection. The prodrug strategy applied to AZT phosphonate derivatives enriched chemistry, biology and medicine not only with new knowledge, methods and structures, but also with a new anti-HIV drug Nikavir. Currently, study of another phosphonate, AZT 5'-aminocarbonylphosphonate, is underway. Slow release of AZT following oral administration and penetration into cells, decreased toxicity and the lack of cumulative properties make the compounds of this group promising as extended-release forms of AZT.

  8. Bis(2-ethylhexyl)-N,N-diethylcarbamoylmethyl phosphonate as a synergist in the extraction of trivalent lanthanides by 1-phenyl-3-methyl-4-trifluoroacetyl-pyrazolone-5

    International Nuclear Information System (INIS)

    Luxmi Varma, R.; Sujatha, S.; Reddy, M.L.P.; Prasada Rao, T.; Iyer, C.S.P.; Damodaran, A.D.

    1996-01-01

    Synergism in the extraction of trivalent lanthanides such as Nd. Eu and Lu has been investigated using mixtures of 1-phenyl-3-methyl-4-trifluoroacetyl-pyrazolone-5 (HPMTFP) and bis(2-ethylhexyl)-N,N-diethylcarbamoylmethyl phosphonate (CMP) in chloroform. Lanthanides are found to be extracted from 0.01 mol/dm 3 chloroacetate medium with HPMTFP as Ln(PMTFP) 3 or Ln(PMTFP) 3 . CMP in the absence or presence of CMP, respectively. The equilibrium constants of these synergistic species do not increase monotonically with atomic number but have a maximum at Eu. The addition of a synergist, CMP to the metal chelate system not only enhances the extraction efficiency but also improves the selectivities among these trivalent lanthanides. The IR results indicate that CMP acts as a bidentate ligand in these mixed-ligand systems. (orig.)

  9. Preparation of N,O-carboxymethyl chitosan coated alginate microcapsules and their application to Bifidobacterium longum BIOMA 5920

    International Nuclear Information System (INIS)

    Mi, Yu; Su, Ran; Fan, Dai-Di; Zhu, Xiao-Li; Zhang, Wen-Ni

    2013-01-01

    In order to greatly improve vitality of probiotic bacteria within the application, a novel biocompatible vehicle, N,O-carboxymethyl chitosan (NOCs) with appropriate degrees of substitution coat alginate (ALg) microparticles, was prepared by electrostatic droplet generation. The amount of chitosan (Cs) and N,O-carboxymethyl chitosan (NOCs) coated on the ALg microparticles was determined by differential scanning calorimetry. The surface morphology of ALg microparticles, Cs coated ALg microparticles and NOCs coated ALg microparticles was determined using scanning electron microscopy. The coating thickness of Cs coated ALg microparticles and that of NOCs coated ALg microparticles was directly observed with confocal laser scanning microscopy. In order to assess pH sensitivity of microparticles, the bovine serum albumin release from the microspheres was tested in acid solution (pH 2.0) for 2 h and subsequently in alkaline solution (pH 7.0) for 2 h. The survival of Bifidobacterium longum BIOMA 5920 loaded in NOCs coated with ALg microparticle was improved in simulated gastric juice (pH 2.0, for 2 h) compared to that of B. longum BIOMA 5920 loaded in ALg microparticles and Cs coated ALg microparticles. After incubation in simulated intestinal juices (pH 7.0, 2 h), the release of microencapsulated B. longum BIOMA 5920 was investigated. - Highlights: • Synthesised N,O-carboxymethyl chitosan (NOCs) coated alginate (ALg) microspheres. • Their effect on intestinal microflora was investigated in simulated gastric juices. • NOCs A coated ALg microspheres improved Bifidobacterium longum survival in SGJ. • The modified chitosan layer improved the pH-response of alginate microspheres. • NOCs A coated microspheres could be used to deliver oral bioactive compounds

  10. Preparation of N,O-carboxymethyl chitosan coated alginate microcapsules and their application to Bifidobacterium longum BIOMA 5920

    Energy Technology Data Exchange (ETDEWEB)

    Mi, Yu; Su, Ran [Shaanxi R and D Center of Biomaterials and Fermentation Engineering, School of Chemical Engineering, Northwest University (China); Fan, Dai-Di, E-mail: fandaidi@nwu.edu.cn [Shaanxi R and D Center of Biomaterials and Fermentation Engineering, School of Chemical Engineering, Northwest University (China); Zhu, Xiao-Li [Shaanxi R and D Center of Biomaterials and Fermentation Engineering, School of Urban and Environmental Science, Northwest University, Taibai North Road 229, Xi' an, Shaanxi 710069 (China); Zhang, Wen-Ni [Shaanxi R and D Center of Biomaterials and Fermentation Engineering, School of Chemical Engineering, Northwest University (China); Shaanxi Key Laboratory of Degradable Biomedical Materials, School of Chemical Engineering, Northwest University (China)

    2013-07-01

    In order to greatly improve vitality of probiotic bacteria within the application, a novel biocompatible vehicle, N,O-carboxymethyl chitosan (NOCs) with appropriate degrees of substitution coat alginate (ALg) microparticles, was prepared by electrostatic droplet generation. The amount of chitosan (Cs) and N,O-carboxymethyl chitosan (NOCs) coated on the ALg microparticles was determined by differential scanning calorimetry. The surface morphology of ALg microparticles, Cs coated ALg microparticles and NOCs coated ALg microparticles was determined using scanning electron microscopy. The coating thickness of Cs coated ALg microparticles and that of NOCs coated ALg microparticles was directly observed with confocal laser scanning microscopy. In order to assess pH sensitivity of microparticles, the bovine serum albumin release from the microspheres was tested in acid solution (pH 2.0) for 2 h and subsequently in alkaline solution (pH 7.0) for 2 h. The survival of Bifidobacterium longum BIOMA 5920 loaded in NOCs coated with ALg microparticle was improved in simulated gastric juice (pH 2.0, for 2 h) compared to that of B. longum BIOMA 5920 loaded in ALg microparticles and Cs coated ALg microparticles. After incubation in simulated intestinal juices (pH 7.0, 2 h), the release of microencapsulated B. longum BIOMA 5920 was investigated. - Highlights: • Synthesised N,O-carboxymethyl chitosan (NOCs) coated alginate (ALg) microspheres. • Their effect on intestinal microflora was investigated in simulated gastric juices. • NOCs A coated ALg microspheres improved Bifidobacterium longum survival in SGJ. • The modified chitosan layer improved the pH-response of alginate microspheres. • NOCs A coated microspheres could be used to deliver oral bioactive compounds.

  11. Magnetic chitosan/clay beads: A magsorbent for the removal of cationic dye from water

    Energy Technology Data Exchange (ETDEWEB)

    Bée, Agnès, E-mail: agnes.bee@upmc.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Laboratoire PHENIX, F-75005 Paris (France); Obeid, Layaly, E-mail: lghannoum@hotmail.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Laboratoire PHENIX, F-75005 Paris (France); CertiNergy Solutions, 33 avenue du Maine, BP 195, 75755 Paris Cedex 15 (France); Mbolantenaina, Rakotomalala, E-mail: mbolantenaina@yahoo.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Laboratoire PHENIX, F-75005 Paris (France); Welschbillig, Mathias, E-mail: welschbillig@certinergysolutions.com [CertiNergy Solutions, 33 avenue du Maine, BP 195, 75755 Paris Cedex 15 (France); Talbot, Delphine, E-mail: delphine.talbot@upmc.fr [Sorbonne Universités, UPMC Univ Paris 06, CNRS, Laboratoire PHENIX, F-75005 Paris (France)

    2017-01-01

    A magnetic composite material composed of magnetic nanoparticles and clay encapsulated in cross-linked chitosan beads was prepared, characterized and used as a magsorbent for the removal of a cationic dye, methylene blue (MB), from aqueous solutions. The magnetic properties of these beads represent an advantage to recover them at the end of the depollution process. The optimal weight ratio R=clay:chitosan for the removal of MB in a large range of pH was determined. For beads without clay, the maximal adsorption capacity of MB occurs in the pH range [9–12], while for beads with clay, the pH range extends by increasing the amount of clay to reach [3–12] for R>0.5. Adsorption isotherms show that the adsorption capacity of magnetic beads is equal to 82 mg/g. Moreover, the kinetics of dye adsorption is relatively fast since 50% of the dye is removed in the first 13 min for an initial MB concentration equal to 100 mg/L. The estimation of the number of adsorption sites at a given pH shows that the main driving force for adsorption of MB in a large range of pH is the electrostatic interaction between the positively charged dye and the permanent negative charges of clay. - Highlights: • A magsorbent based on magnetic nanoparticles and clay encapsulated in chitosan beads was prepared and characterized. • Clay played significant role for the removal of a cationic dye. • The magnetic beads exhibit a maximum adsorption capacity of 82 mg/g for methylene blue. • The pH range of the maximum adsorption extends from [9–12] to [3–12] by increasing the amount of clay. • The magsorbent could be magnetically removed from solution.

  12. Structure-activity relationships of amide-phosphonate derivatives as inhibitors of the human soluble epoxide hydrolase.

    Science.gov (United States)

    Kim, In-Hae; Park, Yong-Kyu; Nishiwaki, Hisashi; Hammock, Bruce D; Nishi, Kosuke

    2015-11-15

    Structure-activity relationships of amide-phosphonate derivatives as inhibitors of the human soluble epoxide hydrolase (sEH) were investigated. First, a series of alkyl or aryl groups were substituted on the carbon alpha to the phosphonate function in amide compounds to see whether substituted phosphonates can act as a secondary pharmacophore. A tert-butyl group (16) on the alpha carbon was found to yield most potent inhibition on the target enzyme. A 4-50-fold drop in inhibition was induced by other substituents such as aryls, substituted aryls, cycloalkyls, and alkyls. Then, the modification of the O-substituents on the phosphonate function revealed that diethyl groups (16 and 23) were preferable for inhibition to other longer alkyls or substituted alkyls. In amide compounds with the optimized diethylphosphonate moiety and an alkyl substitution such as adamantane (16), tetrahydronaphthalene (31), or adamantanemethane (36), highly potent inhibitions were gained. In addition, the resulting potent amide-phosphonate compounds had reasonable water solubility, suggesting that substituted phosphonates in amide inhibitors are effective for both inhibition potency on the human sEH and water solubility as a secondary pharmacophore. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Enhanced Photocatalytic Performance of NiO-Decorated ZnO Nanowhiskers for Methylene Blue Degradation

    Directory of Open Access Journals (Sweden)

    I. Abdul Rahman

    2014-01-01

    Full Text Available ZnO nanowhiskers were used for photodecomposition of methylene blue in aqueous solution under UV irradiation. The rate of methylene blue degradation increased linearly with time of UV irradiation. 54% of degradation rate was observed when the ZnO nanowhiskers were used as photocatalysts for methylene blue degradation for 80 min under UV irradiation. The decoration of p-type NiO nanoparticles on n-type ZnO nanowhiskers significantly enhanced photocatalytic activity and reached 72% degradation rate of methylene blue by using the same method. NiO-decorated ZnO was recycled for second test and shows 66% degradation from maximal peak of methylene blue within the same period. The increment of photocatalytic activity of NiO-decorated ZnO nanowhiskers was explained by the extension of the electron depletion layer due to the formation of nanoscale p-n junctions between p-type NiO and n-type ZnO. Hence, these products provide new alternative proficient photocatalysts for wastewater treatment.

  14. Flow Cytometry Detection of Bacterial Cell Entrapment within the Chitosan Hydrogel and Antibacterial Property of Extracted Chitosan

    Directory of Open Access Journals (Sweden)

    Nafise Sadat Majidi

    2016-09-01

    Full Text Available Background:   Chitosan is unbranched polysaccharide composed of D-glucosamine and N-acetyl-D-glucosamine. Chitosan, derived from shrimp shell, has broad antimicrobial properties against Gram-negative, Gram-positive bacteria and fungi. Methods:  Chitosan was extracted from shrimp shell and studied for cell entrapment and anti-bacterial properties. The hydrogel chitosan was used as the beads for cell entrapment and chitosan beads were designed to deliver cells and nutrients. These data confirmed with flow cytometric analyses.                 Results:   Experimental results exhibited that internal diffusion through the chitosan matrix was the main mechanism for whole gelation by TPP (Tri-polyphosphate. The minimum inhibitory concentration (MIC for chitosan against Staphylococcus aureus and Escherichia coli was 16 and 32 μg/ml respectively. Conclusion:  Despite the antimicrobial properties of chitosan, trapped bacteria in the gel network were alive and were chelated indicating that their access to the outside was limited.

  15. Synthesis of biodegradable plastic from tapioca with N-Isopropylacrylamid and chitosan using glycerol as plasticizer

    Science.gov (United States)

    Syaubari; Safwani, S.; Riza, M.

    2018-04-01

    One of natural polymers that can be used as raw material in the manufacture of biodegradable plastic is tapioca and chitosan. The addition of other compounds such as glycerol as plasticizer is to improve the characteristics of the plastic that already produced. N- Isopropylacrylamid (NIPAm) is an organic compound that can be synthesized into a polymer or polymer grafting which also biodegradable too. This research aims tostudy the synthesis of biodegradable plastics from tapioca with the addition of chitosan, NIPAm, poly(NIPAm) and analyze the characteristics of biodegradable plastics that already produced. This research was done in three stages, there are (1) polymerization NIPAm, (2) the grafting of chitosan-poly NIPAm and (3) the synthesis of biodegradable plastics from starch mixture with variation of addition chitosan, NIPAm, poly(NIPAm), chitosan-graft-poly(NIPAm) and also variations of glycerol as plasticizer. The results of this research is a thin sheet of plastic which is will get analyzed for the characteristics of functional groups, mechanical, morphological and its biodegradability. FTIR spectra showed the grafting process with the new group formation of CO single-bond at 850 cm-1. Plastic with the addition of NIPAm and 1 ml glycerol has the highest tensile strength value about 31.1 MPa. Plastic with poly(NIPAm) and 4 ml glycerol produces the highest elongation value about 153.72%. Plastic with Chitosan-graft-poly(NIPAm) with 1 ml glycerol has the longest biodegradation because of the small mass-loss for six weeks which is about 6.6%.

  16. Chitosan and carboxymethyl-chitosan capping ligands: Effects on the nucleation and growth of hydroxyapatite nanoparticles for producing biocomposite membranes

    Energy Technology Data Exchange (ETDEWEB)

    Dumont, Vitor C.; Mansur, Alexandra A.P.; Carvalho, Sandhra M.; Medeiros Borsagli, Fernanda G.L.; Pereira, Marivalda M.; Mansur, Herman S., E-mail: hmansur@demet.ufmg.br

    2016-02-01

    Synthetic biomaterials based on calcium phosphates (CaP) have been widely studied for bone tissue reconstruction therapies, but no definitive solution that fulfills all of the required properties has been identified. Thus, this study reports the synthesis of composite membranes based on nanohydroxyapatite particles (nHA) embedded in chitosan (CHI) and O-carboxymethyl chitosan (CMC) matrices produced using a one-step co-precipitation method in water media. Biopolymers were used as capping ligands for simultaneously controlling the nucleation and growth of the nHA particles during the precipitation process and also to form the polymeric network of the biocomposites. The bionanocomposites were extensively characterized using light microscopy (LM), scanning and transmission electron microscopy (SEM/TEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), atomic force microscopy (AFM), X-ray micro-CT analysis (μCT), and MTT (3-(4,5-dimethylthiazolyl-2)-2,5-diphenyltetrazolium bromide) cell proliferation assays for cell cytotoxicity. The results demonstrated that the ligands used during the synthesis highly affected the composites produced, primarily due the changes in the mechanisms and kinetics of nucleation and growth of the HA particles at the nanoscale level. The SEM images revealed that the use of carboxyl-functionalized chitosan (CMC) ligands significantly reduced the average size of the HA nanoparticles and caused the formation of a narrower size distribution (90 ± 20 nm) compared to the HA nanoparticles produced with chitosan ligands (220 ± 50 nm). The same trend was verified by the AFM analysis, where the nHA particles were formed evenly dispersed in the polymer matrix. However, the CMC-based composites were more homogeneously distributed, which was endorsed by the images collected via X-ray micro-CT. The FTIR spectra and the XRD analysis indicated that nanosized hydroxyapatite was the

  17. Vitamin D-fortified chitosan films from mushroom waste

    Science.gov (United States)

    Brown mushroom (Agaricus bisporus) stalk bases from mushroom waste were treated with UV-B light to rapidly increase vitamin D2 content. Chitin was also recovered from this waste and converted into chitosan by N-deacetylation. FTIR spectra showed that the mushroom chitosan were similar to chitosan fr...

  18. Comparison of Zirconium Phosphonate-Modified Surfaces for Immobilizing Phosphopeptides and Phosphate-Tagged Proteins.

    Science.gov (United States)

    Forato, Florian; Liu, Hao; Benoit, Roland; Fayon, Franck; Charlier, Cathy; Fateh, Amina; Defontaine, Alain; Tellier, Charles; Talham, Daniel R; Queffélec, Clémence; Bujoli, Bruno

    2016-06-07

    Different routes for preparing zirconium phosphonate-modified surfaces for immobilizing biomolecular probes are compared. Two chemical-modification approaches were explored to form self-assembled monolayers on commercially available primary amine-functionalized slides, and the resulting surfaces were compared to well-characterized zirconium phosphonate monolayer-modified supports prepared using Langmuir-Blodgett methods. When using POCl3 as the amine phosphorylating agent followed by treatment with zirconyl chloride, the result was not a zirconium-phosphonate monolayer, as commonly assumed in the literature, but rather the process gives adsorbed zirconium oxide/hydroxide species and to a lower extent adsorbed zirconium phosphate and/or phosphonate. Reactions giving rise to these products were modeled in homogeneous-phase studies. Nevertheless, each of the three modified surfaces effectively immobilized phosphopeptides and phosphopeptide tags fused to an affinity protein. Unexpectedly, the zirconium oxide/hydroxide modified surface, formed by treating the amine-coated slides with POCl3/Zr(4+), afforded better immobilization of the peptides and proteins and efficient capture of their targets.

  19. Synthesis and applications of gem-bis-phosphonates, powerful complexing agents of metals

    International Nuclear Information System (INIS)

    Lecercle, D.

    2007-12-01

    This thesis was devoted to the development of new ways to prepare gem-bis-phosphonates compounds (BPs), and was carried out under the Program of Nuclear and Environmental Toxicology (ToxNuc-E). Two applications of these compounds have been investigated, the preparation of potent ligands of the uranyl ion for a target of decorporation, and the preparation of new anticancer compounds. The first of these applications was the consequence of work done in the laboratory, that have shown the strong uranium-binding properties of bis-phosphonic ligands. The in vivo tests performed on these compounds have shown the tendency of these ligands to cause liver accumulation of uranium, we wanted to address this problem by modifying the method of anchoring of the bis-phosphonates functions. To this end we have developed a new way to access to these compounds using a metal-carbenoid mediated poly-ols and poly-amines insertion, the metal-carbenoid species bearing the bis-phosphonate function. Regarding the preparation of BPs as anticancer agents, we have developed a new synthetic pathway using a phosphine catalyzed α-P addition of phosphorated pro-nucleophiles to alkynyl-phosphonates as a key step. This enabled us to prepare thirty compound whose activity was evaluated on two cell lines (A431 and HuH7). Five of these compounds possess an activity equivalent to that of the compound described as the most active, the Zoledronate. (author)

  20. Removal of phosphonates from industrial wastewater with UV/FeII, Fenton and UV/Fenton treatment.

    Science.gov (United States)

    Rott, Eduard; Minke, Ralf; Bali, Ulusoy; Steinmetz, Heidrun

    2017-10-01

    Phosphonates are an important group of phosphorus-containing compounds due to their increasing industrial use and possible eutrophication potential. This study involves investigations into the methods UV/Fe II , Fenton and UV/Fenton for their removal from a pure water matrix and industrial wastewaters. It could be shown that the degradability of phosphonates by UV/Fe II (6 kWh/m 3 ) in pure water crucially depended on the pH and was higher the less phosphonate groups a phosphonate contains. The UV/Fe II method is recommended in particular for the treatment of concentrates with nitrogen-free phosphonates, only little turbidity and a low content of organic compounds. Using Fenton reagent, the degradation of polyphosphonates was relatively weak in a pure water matrix (Fenton method (6 kWh/m 3 ), those phosphonates with the smallest numbers of phosphonate groups were easier degraded as well at pH 3.5 in a pure water matrix (o-PO 4 3- formation rates of up to 80%). Despite an incomplete transformation of organically bound phosphorus to o-PO 4 3- with Fenton reagent in an organically highly polluted wastewater (max. 15%), an almost total removal of the total P occurred. The most efficient total P elimination rates were achieved in accordance with the following Fenton implementation: reaction → sludge separation (acidic) → neutralization of the supernatant → sludge separation (neutral). Accordingly, a neutralization directly after the reaction phase led to a lower total P removal extent. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering.

    Science.gov (United States)

    Lowe, Baboucarr; Venkatesan, Jayachandran; Anil, Sukumaran; Shim, Min Suk; Kim, Se-Kwon

    2016-12-01

    Solid three dimensional (3D) composite scaffolds for bone tissue engineering were prepared using the freeze-drying method. The scaffolds were composed of chitosan, natural nano-hydroxyapatite (nHA) and fucoidan in the following combinations: chitosan, chitosan-fucoidan, chitosan-nHA, and chitosan-nHA-fucoidan. Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and optical microscopy (OM) were used to determine the physiochemical constituents and the morphology of the scaffolds. The addition of nHA into the chitosan-fucoidan composite scaffold reduced the water uptake and water retention. FT-IR analysis confirmed the presence of a phosphate group in the chitosan-nHA-fucoidan scaffold. This group is present because of the presence of nHA (isolated via alkaline hydrolysis from salmon fish bones). Microscopic results indicated that the dispersion of nHA and fucoidan in the chitosan matrix was uniform with a pore size of 10-400μm. The composite demonstrated a suitable micro architecture for cell growth and nutrient supplementation. This compatibility was further elucidated in vitro using periosteum-derived mesenchymal stem cells (PMSCs). The cells demonstrated high biocompatibility and excellent mineralization for the chitosan-nHA-fucoidan scaffold. We believe that a chitosan-nHA-fucoidan composite is a promising biomaterial for the scaffold that can be used for bone tissue regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Various methods for determination of the degree of N-acetylation of chitin and chitosan: a review.

    Science.gov (United States)

    Kasaai, Mohammad R

    2009-03-11

    Chitin, chitosan, and their derivatives have been identified as versatile biopolymers for a broad range of agriculture and food applications. Up to now, several methods have been developed to determine degree of N-acetylation, DA, for chitin and chitosan. In this article, an effort has been made to review the available literature information on the DA determination. These methods are classified into three categories: (1) spectroscopy (IR, (1)H NMR, (13)C NMR, (15)N NMR, and UV); (2) conventional (various types of titration, conductometry, potentiometry, ninhydrin assay, adsorption of free amino groups of chitosan by pictric acid); (3) destructive (elemental analysis, acid or enzymatic hydrolysis of chitin/chitosan and followed by the DA measurement by colorimetry or high performance liquid chromatography, pyrolysis-gas chromatography, and thermal analysis using differential scanning calorimetry) methods. These methods have been compared for their performances and limitations as well as their advantages and disadvantages. The use of IR and NMR spectroscopy methods provides a number of advantages. They do not need long-term procedures to prepare samples, and they provide information on the chemical structure. (1)H NMR and UV techniques are more sensitive than IR, (13)C NMR, and (15)N NMR spectroscopy. The IR technique is mostly used for a qualitative evaluation and comparison studies. Conventional methods are not applicable for highly acetylated chitin. The results of the latter methods are affected by ionic strength of the solvent, pH, and temperature of solution. In destructive methods, longer times are needed for the measurements compared to spectroscopy and conventional methods, but they are applicable for the entire range of the DA.

  3. Injectable porous nano-hydroxyapatite/chitosan/tripolyphosphate scaffolds with improved compressive strength for bone regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Uswatta, Suren P.; Okeke, Israel U. [Department of Bioengineering, The University of Toledo, Toledo, OH 43614 (United States); Jayasuriya, Ambalangodage C., E-mail: a.jayasuriya@utoledo.edu [Department of Bioengineering, The University of Toledo, Toledo, OH 43614 (United States); Department of Orthopaedic Surgery, The University of Toledo, Toledo, OH 43614 (United States)

    2016-12-01

    In this study we have fabricated porous injectable spherical scaffolds using chitosan biopolymer, sodium tripolyphosphate (TPP) and nano-hydroxyapatite (nHA). TPP was primarily used as an ionic crosslinker to crosslink nHA/chitosan droplets. We hypothesized that incorporating nHA into chitosan could support osteoconduction by emulating the mineralized cortical bone structure, and improve the Ultimate Compressive Strength (UCS) of the scaffolds. We prepared chitosan solutions with 0.5%, 1% and 2% (w/v) nHA concentration and used simple coacervation and lyophilization techniques to obtain spherical scaffolds. Lyophilized spherical scaffolds had a mean diameter of 1.33 mm (n = 25). Further, portion from each group lyophilized scaffolds were soaked and dried to obtain Lyophilized Soaked and Dried (LSD) scaffolds. LSD scaffolds had a mean diameter of 0.93 mm (n = 25) which is promising property for the injectability. Scanning Electron Microscopy images showed porous surface morphology and interconnected pore structures inside the scaffolds. Lyophilized and LSD scaffolds had surface pores < 10 and 2 μm, respectively. 2% nHA/chitosan LSD scaffolds exhibited UCS of 8.59 MPa compared to UCS of 2% nHA/chitosan lyophilized scaffolds at 3.93 MPa. Standardize UCS values were 79.98 MPa and 357 MPa for 2% nHA/chitosan lyophilized and LSD particles respectively. One-way ANOVA results showed a significant increase (p < 0.001) in UCS of 1% and 2% nHA/chitosan lyophilized scaffolds compared to 0% and 0.5% nHA/chitosan lyophilized scaffolds. Moreover, 2% nHA LSD scaffolds had significantly increased (p < 0.005) their mean UCS by 120% compared to 2% nHA lyophilized scaffolds. In a drawback, all scaffolds have lost their mechanical properties by 95% on the 2nd day when fully immersed in phosphate buffered saline. Additionally live and dead cell assay showed no cytotoxicity and excellent osteoblast attachment to both lyophilized and LSD scaffolds at the end of 14th day of in vitro

  4. Injectable porous nano-hydroxyapatite/chitosan/tripolyphosphate scaffolds with improved compressive strength for bone regeneration

    International Nuclear Information System (INIS)

    Uswatta, Suren P.; Okeke, Israel U.; Jayasuriya, Ambalangodage C.

    2016-01-01

    In this study we have fabricated porous injectable spherical scaffolds using chitosan biopolymer, sodium tripolyphosphate (TPP) and nano-hydroxyapatite (nHA). TPP was primarily used as an ionic crosslinker to crosslink nHA/chitosan droplets. We hypothesized that incorporating nHA into chitosan could support osteoconduction by emulating the mineralized cortical bone structure, and improve the Ultimate Compressive Strength (UCS) of the scaffolds. We prepared chitosan solutions with 0.5%, 1% and 2% (w/v) nHA concentration and used simple coacervation and lyophilization techniques to obtain spherical scaffolds. Lyophilized spherical scaffolds had a mean diameter of 1.33 mm (n = 25). Further, portion from each group lyophilized scaffolds were soaked and dried to obtain Lyophilized Soaked and Dried (LSD) scaffolds. LSD scaffolds had a mean diameter of 0.93 mm (n = 25) which is promising property for the injectability. Scanning Electron Microscopy images showed porous surface morphology and interconnected pore structures inside the scaffolds. Lyophilized and LSD scaffolds had surface pores < 10 and 2 μm, respectively. 2% nHA/chitosan LSD scaffolds exhibited UCS of 8.59 MPa compared to UCS of 2% nHA/chitosan lyophilized scaffolds at 3.93 MPa. Standardize UCS values were 79.98 MPa and 357 MPa for 2% nHA/chitosan lyophilized and LSD particles respectively. One-way ANOVA results showed a significant increase (p < 0.001) in UCS of 1% and 2% nHA/chitosan lyophilized scaffolds compared to 0% and 0.5% nHA/chitosan lyophilized scaffolds. Moreover, 2% nHA LSD scaffolds had significantly increased (p < 0.005) their mean UCS by 120% compared to 2% nHA lyophilized scaffolds. In a drawback, all scaffolds have lost their mechanical properties by 95% on the 2nd day when fully immersed in phosphate buffered saline. Additionally live and dead cell assay showed no cytotoxicity and excellent osteoblast attachment to both lyophilized and LSD scaffolds at the end of 14th day of in vitro

  5. Synthesis and properties of ApA analogues with shortened phosphonate internucleotide linkage

    Czech Academy of Sciences Publication Activity Database

    Králíková, Šárka; Buděšínský, Miloš; Barvík, I.; Masojídková, Milena; Točík, Zdeněk; Rosenberg, Ivan

    2011-01-01

    Roč. 30, 7/9 (2011), s. 524-543 ISSN 1525-7770 R&D Projects: GA ČR GA202/09/0193; GA AV ČR KAN200520801; GA MŠk(CZ) LC06061 Institutional research plan: CEZ:AV0Z40550506 Keywords : alpha-hydroxy-phosphonate linkage * ApA analogues * phosphonate internucleotide bond * NMR conformational study Subject RIV: CC - Organic Chemistry Impact factor: 0.899, year: 2011

  6. Polymeric Materials For Scale Inhibition In Cooling Water Systems

    Directory of Open Access Journals (Sweden)

    Najwa S.Majeed

    2013-04-01

    Full Text Available Calcium carbonate deposition is generally predominant in cooling water-circulating system. For the control of calcium carbonate scale formation two types of polymeric scale inhibitors were used Polyamino polyether methylene phosphonate  (PAPEMPand polyacrylaminde(PAA.Model of cooling tower system have been built up in laboratory scale. Experiments were carried out using different inhibitor concentrations(0.5,1,1.5,2,3ppm ,at water temperature of  40oC and flow rate of 150 l/hr. It was found that Polyamino polyether methylene phosphonate    more effective than polyacryle amide'  as scale inhibitor in all used concentrations and the best inhibition efficiency (95% was at (2.5ppm of Polyamino polyether methylene phosphonate  and (85% with poly acryle amide at concentrations of (3 ppm. The performance of the polymeric scale inhibitors was compared with a method used to control heavy calcium carbonate scale forming by the deposition of sufficiently thin protective calcium carbonate scale using sulfuric acid and depending on Ryznar stability index controlling method. 

  7. Nerve transection repair using laser-activated chitosan in a rat model.

    Science.gov (United States)

    Bhatt, Neel K; Khan, Taleef R; Mejias, Christopher; Paniello, Randal C

    2017-08-01

    Cranial nerve transection during head and neck surgery is conventionally repaired with microsuture. Previous studies have demonstrated recovery with laser nerve welding (LNW), a novel alternative to microsuture. LNW has been reported to have poorer tensile strength, however. Laser-activated chitosan, an adhesive biopolymer, may promote nerve recovery while enhancing the tensile strength of the repair. Using a rat posterior tibial nerve injury model, we compared four different methods of nerve repair in this pilot study. Animal study. Animals underwent unilateral posterior tibial nerve transection. The injury was repaired by potassium titanyl phosphate (KTP) laser alone (n = 20), KTP + chitosan (n = 12), microsuture + chitosan (n = 12), and chitosan alone (n = 14). Weekly walking tracks were conducted to measure functional recovery (FR). Tensile strength (TS) was measured at 6 weeks. At 6 weeks, KTP laser alone had the best recovery (FR = 93.4% ± 8.3%). Microsuture + chitosan, KTP + chitosan, and chitosan alone all showed good FR (87.4% ± 13.5%, 84.6% ± 13.0%, and 84.1% ± 10.0%, respectively). One-way analysis of variance was performed (F(3,56) = 2.6, P = .061). A TS threshold of 3.8 N was selected as a control mean recovery. Three groups-KTP alone, KTP + chitosan, and microsuture + chitosan-were found to meet threshold 60% (95% confidence interval [CI]: 23.1%-88.3%), 75% (95% CI: 46.8%-91.1%), and 100% (95% CI: 75.8%-100.0%), respectively. In the posterior tibial nerve model, all repair methods promoted nerve recovery. Laser-activated chitosan as a biopolymer anchor provided good TS and appears to be a novel alternative to microsuture. This repair method may have surgical utility following cranial nerve injury during head and neck surgery. NA Laryngoscope, 127:E253-E257, 2017. © 2017 The American Laryngological, Rhinological and Otological Society, Inc.

  8. Preparation and characterization of β-cyclodextrin grafted N-maleoyl chitosan nanoparticles for drug delivery

    Directory of Open Access Journals (Sweden)

    Xinyu Hou

    2017-11-01

    Full Text Available β-cyclodextrin (CD grafted N-maleoyl chitosan (CD-g-NMCS with two different degrees of substitution (DS of N-maleoyl (DS = 21.2% and 30.5% were synthesized from maleic anhydride and chitosan bearing pendant cyclodextrin (CD-g-CS. CD-g-NMCS based nanoparticles were prepared via an ionic gelation method together with chitosan and CD-g-CS nanoparticles. The size and zeta potential of prepared CD-g-NMCS nanoparticles were 179.2~274.0 nm and 36.2~42.4 mV, respectively. In vitro stability test indicated that CD-g-NMCS nanoparticles were more stable in phosphate-buffered saline compared with chitosan nanoparticles. Moreover, a poorly water-soluble drug, ketoprofen (KTP, was selected as a model drug to study the obtained nanoparticle's potentials as drug delivery carriers. The drug loading efficiency of CD-g-NMCS20 nanoparticles were 14.8% for KTP. MTT assay showed that KTP loaded CD-g-NMCS nanoparticles were safe drug carriers. Notably, in vitro drug release studies showed that KTP was released in a sustained-release manner for the nanoparticles. The pharmacokinetic of drug loaded CD-g-NMCS20 nanoparticles were evaluated in rats after intravenous administration. The results of studies revealed that, compared with free KTP, KTP loaded CD-g-NMCS20 nanoparticles exhibited a significant increase in AUC0→24h and mean residence time by 6.6-fold and 2.9-fold, respectively. Therefore, CD-g-NMCS nanoparticles could be used as a novel promising nanoparticle-based drug delivery system for sustained release of poorly water-soluble drugs. The carboxylic acid groups of the CD-g-NMCS molecule provide convenient sites for further structural modifications including introduction of tissue- or disease- specific targeting groups.

  9. Sustainable Catalytic Process for Synthesis of Triethyl Citrate Plasticizer over Phosphonated USY Zeolite

    Directory of Open Access Journals (Sweden)

    Kakasaheb Y. Nandiwaleand

    2016-10-01

    Full Text Available Fruits wastage is harmful to health and environment concerning spreading diseases and soil pollution, respectively. To avoid this issue, use of citrus fruit waste for the production of citric acid (CA is one of viable mean to obtain value added chemicals. Moreover, synthesis of triethyl citrate (TEC, a non-toxic plasticizer by esterification of CA with ethanol over heterogeneous catalyst would be renewable and sustainable catalytic process. In this context, parent Ultrastable Y (USY and different percentage phosphonated USY (P-USY zeolites were used for the synthesis of TEC in a closed batch reactor, for the first time. The synthesized catalysts were characterized by N2-adsorption desorption isotherm, powder X-ray diffraction (XRD and NH3 temperature programmed desorption (TPD. Effect of reaction conditions, such as the molar ratio of ethanol to CA (5:1 - 20:1, the catalyst to CA ratio (0.05 - 0.25 and reaction temperature (363-403 K, were studied in view to maximizing CA conversion and TEC yield. Phosphonated USY catalysts were found to be superior in activity (CA conversion and TEC yield than parent USY, which is attributed to the increased in total acidity with phosphonation. Among the studied catalysts, the P2USY (2% phosphorous loaded on USY was found to be an optimum catalyst with 99% CA conversion and 82% TEC yield, which is higher than the reported values. This study opens new avenues of research demonstrating principles of green chemistry such as easy separable and reusable catalyst, non-toxic product, bio-renewable synthetic route, milder operating parameters and waste minimization. Copyright © 2016 BCREC GROUP. All rights reserved Received: 12nd October 2015; Revised: 22nd December 2015; Accepted: 29th January 2016 How to Cite: Nandiwale, K.Y., Bokade, V.V. (2016. Sustainable Catalytic Process for Synthesis of Triethyl Citrate Plasticizer over Phosphonated USY Zeolite. Bulletin of Chemical Reaction Engineering & Catalysis, 11 (3: 292

  10. Phosphonate biosynthesis and catabolism: a treasure trove of unusual enzymology.

    Science.gov (United States)

    Peck, Spencer C; van der Donk, Wilfred A

    2013-08-01

    Natural product biosynthesis has proven a fertile ground for the discovery of novel chemistry. Herein we review the progress made in elucidating the biosynthetic pathways of phosphonate and phosphinate natural products such as the antibacterial compounds dehydrophos and fosfomycin, the herbicidal phosphinothricin-containing peptides, and the antimalarial compound FR-900098. In each case, investigation of the pathway has yielded unusual, and often unprecedented, biochemistry. Likewise, recent investigations have uncovered novel ways to cleave the CP bond to yield phosphate under phosphorus starvation conditions. These include the discovery of novel oxidative cleavage of the CP bond catalyzed by PhnY and PhnZ as well as phosphonohydrolases that liberate phosphate from phosphonoacetate. Perhaps the crown jewel of phosphonate catabolism has been the recent resolution of the longstanding problem of the C-P lyase responsible for reductively cleaving the CP bond of a number of different phosphonates to release phosphate. Taken together, the strides made on both metabolic and catabolic fronts illustrate an array of fascinating biochemistry. Copyright © 2013 Elsevier Ltd. All rights reserved.

  11. Chitosan and Nanohydroxyapatite Roles in Physical and Chemical Characteristics of Gelatin/Chitosan/Nanohydroxyapatite Microspheres

    Directory of Open Access Journals (Sweden)

    S. Bagheri-Khoulenjani

    2010-12-01

    Full Text Available The effects of chitosan/biopolymer (C/P and nanohydroxyapatite/ biopolymer (nHA/P weight ratios on particle size and its uniformity, cross-linking density and NH2 content of nano-hydroxyapatite/chitosan/gelatin (nHA/C/G microspheres were investigated. Microspheres were fabricated using water-in-oil emulsion. Cross-linking of microspheres was performed using water soluble carbodiimide. Particle size and its uniformity were evaluated using an optical microscope. The morphology of microspheres was studied by scanning electron microscopy. The obtained data from particle size measurements revealed that increments in C/P ratio increased the particle size while reducing its uniformity, and increased the NH2 content and cross linking density of the microspheres. It was shown that incremental increase in nHA/P ratio increased the particle size and its uniformity and reduced the NH2 content and cross-linking density of the microspheres.Morphological studies showed that the fabricated microspheres had spherical shape in medium level of C/P ratio and nHA/P ratio. However, increasing in chitosan/biopolymer ratio induced some micro-cracks into the structure of microspheres.

  12. Oxygen isotope signature of UV degradation of glyphosate and phosphonoacetate: Tracing sources and cycling of phosphonates

    Energy Technology Data Exchange (ETDEWEB)

    Sandy, Edward H. [State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan 430074 (China); Department of Geology and Geophysics, Yale University, P.O. Box 208109, New Haven, CT 06520-8109 (United States); Department of Chemistry, University of Sierra Leone, Freetown (Sierra Leone); Blake, Ruth E., E-mail: ruth.blake@yale.edu [Department of Geology and Geophysics, Yale University, P.O. Box 208109, New Haven, CT 06520-8109 (United States); School of Civil and Environmental Engineering, and National “International Cooperation Base on Environment and Energy”, University of Science and Technology Beijing, Beijing 100084 (China); Chang, Sae Jung [Department of Geology and Geophysics, Yale University, P.O. Box 208109, New Haven, CT 06520-8109 (United States); Jun, Yao, E-mail: yaojun@ustb.edu.cn [State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan 430074 (China); Department of Geology and Geophysics, Yale University, P.O. Box 208109, New Haven, CT 06520-8109 (United States); School of Civil and Environmental Engineering, and National “International Cooperation Base on Environment and Energy”, University of Science and Technology Beijing, Beijing 100084 (China); Yu, Chan [Department of Geology and Geophysics, Yale University, P.O. Box 208109, New Haven, CT 06520-8109 (United States); School of Civil and Environmental Engineering, and National “International Cooperation Base on Environment and Energy”, University of Science and Technology Beijing, Beijing 100084 (China)

    2013-09-15

    Highlights: • Phosphonate (phon) hydrolysis by UVR (1.2 kW) attained ≥90% completion in 84 h. • Isotope study reveals both ambient H{sub 2}O and O{sub 2} involvements in phon C-P bond cleavage. • Mechanistic models proposed for phon C-P bond cleavage based on O-isotope analysis. • Model equations used to calculate δ{sup 18}O{sub P-org} of original phon P-moiety-useful as a tracer. • Study shows relevance in tracing phon sources and cycling in the environment. -- Abstract: The degradation of phosphonates in the natural environment constitutes a major route by which orthophosphate (Pi) is regenerated from organic phosphorus and recently implicated in marine methane production, with ramifications to environmental pollution issues and global climate change concerns. This work explores the application of stable oxygen isotope analysis in elucidating the C-P bond cleavage mechanism(s) of phosphonates by UV photo-oxidation and for tracing their sources in the environment. The two model phosphonates used, glyphosate and phosphonoacetic acid were effectively degraded after exposure to UV irradiation. The isotope results indicate the involvement of both ambient water and atmospheric oxygen in the C-P bond cleavage and generally consistent with previously posited mechanisms of UV-photon excitation reactions. A model developed to calculate the oxygen isotopic composition of the original phosphonate P-moiety, shows both synthetic phosphonates having distinctly lower values compared to naturally derived organophosphorus compounds. Such mechanistic models, based on O-isotope probing, are useful for tracing the sources and reactions of phosphonates in the environment.

  13. Biomedical Activity of Chitin/Chitosan Based Materials—Influence of Physicochemical Properties Apart from Molecular Weight and Degree of N-Acetylation

    Directory of Open Access Journals (Sweden)

    Mirko X. Weinhold

    2011-11-01

    Full Text Available The physicochemical nature of chitin and chitosan, which influences the biomedical activity of these compounds, is strongly related to the source of chitin and the conditions of the chitin/chitosan production process. Apart from widely described key factors such as weight-averaged molecular weight (MW and degree of N-acetylation (DA, other physicochemical parameters like polydispersity (MW/MN, crystallinity or the pattern of acetylation (PA have to be taken into consideration. From the biological point of view, these parameters affect a very important factor—the solubility of chitin and chitosan in water and organic solvents. The physicochemical properties of chitosan solutions can be controlled by manipulating solution conditions (temperature, pH, ionic strength, concentration, solvent. The degree of substitution of the hydroxyl and the amino groups or the degree of quaternization of the amino groups also influence the mechanical and biological properties of chitosan samples. Finally, a considerable research effort has been directed towards developing safe and efficient chitin/chitosan-based products because many factors, like the size of nanoparticles, can determine the biomedical characteristics of medicinal products. The influence of these factors on the biomedical activity of chitin/chitosan-based products is presented in this report in more detail.

  14. Syntheses and crystal structures of a series of new divalent metal phosphonates with imino-bis(methylphosphonic acid)

    International Nuclear Information System (INIS)

    Yang Bingping; Prosvirin, Andrey V.; Zhao, Han-Hua; Mao, Jiang-Gao

    2006-01-01

    Hydrothermal reactions of divalent transition metal salts with imino-bis(methylphosphonic acid), NH(CH 2 PO 3 H 2 ) 2 (H 4 L) afforded three new metal phosphonates, namely, Cu[NH(CH 2 PO 3 H) 2 ] 1, {Co[NH 2 (CH 2 PO 3 H)(CH 2 PO 3 )](H 2 O) 2 }.H 2 O 2 and Mn[NH 2 (CH 2 PO 3 H)(CH 2 PO 3 )](H 2 O) 3. When HO 2 C(CH 2 ) 3 N(CH 2 PO 3 H 2 ) 2 was used as the phosphonate ligand and 4,4'-bipy as the second metal linker, {Cu 4 [NH(CH 2 PO 3 ) 2 ] 2 (4,4'-bipy)(H 2 O) 4 }.9H 2 O 4 with a pillared layered architecture was obtained. The NH(CH 2 PO 3 ) 2 anion resulted from the cleavage of the HO 2 C(CH 2 ) 3 -group during the reaction. Although compounds 1-3 have a same M/L ratio (1:1), they exhibit totally different structures.Compound 1 has a linear chain structure, in which each pair of square-pyramidal coordinated copper(II) ions are bridged by two phosphonate oxygen atoms to form a Cu 2 O 2 dimeric unit, and such dimeric units are further interconnected via phosphonate groups to form a [010] chain. Compound 2 has a layered architecture built from CoO 6 octahedra bridged by phosphonate ligands. In compound 3, the interconnection of the manganese(II) ions by bridging imino-diphosphonate ligands leads to a 3D network. Compound 4 has a pillar-layered structure, the layers composed of Cu(II) ions bridged by aminodiphosphonate ligands are interconnected by 4,4'-bipy ligands to form channels along c-axis. Several factors that affect the structures of the metal phosphonates formed have also been discussed. Compounds 2 and 3 show predominant antiferromagnetic interactions between magnetic centers. -- Graphical abstract: Four new metal phosphonates, namely, Cu[NH(CH 2 PO 3 H) 2 ] 1, {Co[NH 2 (CH 2 PO 3 H)(CH 2 PO 3 )](H 2 O) 2 }.H 2 O 2, Mn[NH 2 (CH 2 PO 3 H)(CH 2 PO 3 )](H 2 O) 3 and {Cu 4 [NH(CH 2 PO 3 ) 2 ] 2 (4,4'-bipy)(H 2 O) 4 }.9H 2 O 4 have been synthesized and structurally characterized. Compound 1 has a linear chain structure, and compound 2 is layered. Compound 3 is

  15. Glycol chitosan

    DEFF Research Database (Denmark)

    Danielsen, E Thomas; Danielsen, E Michael

    2017-01-01

    Chitosan is a polycationic polysaccharide consisting of β-(1-4)-linked glucosamine units and due to its mucoadhesive properties, chemical derivatives of chitosan are potential candidates as enhancers for transmucosal drug delivery. Recently, glycol chitosan (GC), a soluble derivative of chitosan...

  16. Impact of salt form and molecular weight of chitosan on swelling and drug release from chitosan matrix tablets.

    Science.gov (United States)

    Huanbutta, Kampanart; Cheewatanakornkool, Kamonrak; Terada, Katsuhide; Nunthanid, Jurairat; Sriamornsak, Pornsak

    2013-08-14

    Magnetic resonance imaging (MRI) and gravimetric techniques were used to assess swelling and erosion behaviors of hydrophilic matrix tablets made of chitosan. The impact of salt form, molecular weight (MW) and dissolution medium on swelling behavior and drug (theophylline) release was studied. The matrix tablets made of chitosan glycolate (CGY) showed the greatest swelling in both acid and neutral media, compared to chitosan aspartate, chitosan glutamate and chitosan lactate. MRI illustrated that swelling region of CGY in both media was not different in the first 100 min but glassy region (dry core) in 0.1N HCl was less than in pH 6.8 buffer. The tablets prepared from chitosan with high MW swelled greater than those of low MW. Moreover, CGY can delay drug release in the acid condition due to thick swollen gel and low erosion rate. Therefore, CGY may be suitably applied as sustained drug release polymer or enteric coating material. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Synthesis of difluorinated compounds starting from phosphonates

    Czech Academy of Sciences Publication Activity Database

    Alexandrova, Anastasia; Beier, Petr

    2008-01-01

    Roč. 102, č. 11 (2008), s. 1023-1023 ISSN 0009-2770. [Pokroky v organické, bioorganické a farmaceutické chemii /43./. 14.11.2008-16.11.2008, Liblice] Institutional research plan: CEZ:AV0Z40550506 Keywords : phosphonates * nucleophilic addition Subject RIV: CC - Organic Chemistry

  18. Amphiphilic chitosan derivatives as carrier agents for rotenone

    Science.gov (United States)

    Kamari, Azlan; Aljafree, Nurul Farhana Ahmad

    2017-08-01

    In the present study, the feasibility of amphiphilic chitosan derivatives, namely oleoyl carboxymethyl chitosan (OCMCs), N,N-dimethylhexadecyl carboxymethyl chitosan (DCMCs) and deoxycholic acid carboxymethyl chitosan (DACMCs) as carrier agents for rotenone in water-insoluble pesticide formulations was investigated. Fourier Transform Infrared (FTIR) Spectrometer, CHN-O Elemental Analyser (CHN-O) and Transmission Electron Microscope (TEM) were used to characterise amphiphilic chitosan derivatives. The critical micelle concentration (CMC) of amphiphilic chitosan derivatives was determined using a Fluorescence Spectrometer. A High Performance Liquid Chromatography (HPLC) was used to determine the ability of OCMCs, DCMCs and DACMCs to load and release rotenone in an in vitro system. Based on TEM analysis, results have shown that amphiphilic chitosan derivatives formed self-assembly and exhibited spherical shape. The CMC values determined for OCMCs, DCMCs and DACMCs were 0.093, 0.098 and 0.468 mg/mL, respectively. The encapsulation efficiency (EE) values for the materials were more than 97.0%, meanwhile the loading capacity (LC) values were greater than 0.90%. OCMCs, DCMCs and DACMCs micelles exhibited an excellent ability to control the release of rotenone, of which 90.0% of rotenone was released within 40 to 52 h. In conclusion, OCMCs, DCMCs and DACMCs possess several key features to act as effective carrier agents for rotenone. Overall, amphiphilic chitosan derivatives produced in this study were successfully increased the solubility of rotenone by 49.0 times higher than free rotenone.

  19. Conformationally constrained nucleoside phosphonic acids - potent inhibitors of human mitochondrial and cytosolic 5'(3')-nucleotidases

    Czech Academy of Sciences Publication Activity Database

    Šimák, Ondřej; Pachl, Petr; Fábry, Milan; Buděšínský, Miloš; Jandušík, T.; Hnízda, Aleš; Skleničková, Radka; Petrová, Magdalena; Veverka, Václav; Řezáčová, Pavlína; Brynda, Jiří; Rosenberg, Ivan

    2014-01-01

    Roč. 12, č. 40 (2014), s. 7971-7982 ISSN 1477-0520 R&D Projects: GA ČR GA203/09/0820; GA ČR GA13-24880S; GA ČR GA13-26526S; GA MŠk(CZ) LK11205; GA AV ČR KAN200520801 Institutional support: RVO:61388963 ; RVO:68378050 Keywords : 5'(3')-nucleotidase * structure * inhibition * cdN * mdN * nucleoside * SAR * phosphonic acid Subject RIV: CC - Organic Chemistry Impact factor: 3.562, year: 2014

  20. Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

    International Nuclear Information System (INIS)

    Li Junjie; Zhu Dunwan; Yin Jianwei; Liu Yuxi; Yao Fanglian; Yao Kangde

    2010-01-01

    Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca 2+ ] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca 2+ ]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio ≤ 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

  1. Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

    Energy Technology Data Exchange (ETDEWEB)

    Li Junjie [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China); Zhu Dunwan [Institute of Biomedical Engineering, Chinese Academy of Medical Sciences and Peking Union Medical College, Tianjin, 300072 (China); Yin Jianwei; Liu Yuxi [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Fanglian, E-mail: yaofanglian@tju.edu.cn [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Kangde [Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China)

    2010-07-20

    Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca{sup 2+}] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca{sup 2+}]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio {<=} 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

  2. Complexation of 188Re-phosphonates: in vitro and in vivo studies

    International Nuclear Information System (INIS)

    Faintuch, B.L.; Muramoto, E.; Faintuch, S.

    2003-01-01

    MDP (methylenediphosphonate) and HEDP (hydroxyethylidene diphosphonate), both disphosphonates, and EDTMP (ethylenediamine tetramethylene phosphonic acid), a tetraphosphonate ligand, have been previously labeled with 188 Re for use in metastatic bone-pain palliation. The aim of this study was a comparison between the three complexes 188 Re-MDP, 188 Re-HEDP and 188 Re-EDTMP concerning the complexation conditions, in order to achieve maximum yield, stability and bone uptake. Methods: MDP was dissolved in water and HEDP and EDTMP were dissolved in NaOH 1 N followed by reduction of pH with HCl 1 N. To all mixtures stannous chloride and 188 ReO 4 - were added in a nitrogen atmosphere. The preparations were heated in boiling water bath for 15 min. Yield as well as radiochemical stability was estimated by ITLC. Different concentrations of phosphonates and stannous chloride were evaluated. Biodistribution studies in Swiss mice were done for the three 188 Re-phosphonates that presented the best radiochemical yield. The optimal ligand concentration for maximum complexation was 85.2 mM for MDP, 72.8 mM for HEDP and 45.8 mM for EDTMP. The best amount of SnCl 2 .2H 2 O was 1.5 mg/mL for 188 Re-HEDP and 1 mg/mL for both 188 Re-MDP and 188 Re-EDTMP. In these conditions the three complexes showed a complexation rate above 95%. Reasonable radiochemical stability for 24 hours was achieved by 188 Re-EDTMP when employing ascorbic acid. All products showed a great uptake by the kidneys. 188 Re-EDTMP had the greatest uptake by femur (3.1 ± 0.2% ID/g) followed by 188 Re-MDP (1.2 ± 0.1% ID/g) and 188 Re-HEDP (1.0 ± 0.1% ID/g), 4 hours post injection. 188 Re-EDTMP displayed a femur bone/muscle ratio of 28.5, 188 Re-MDP 4.9 and 188 Re-HEDP 4.9. In conclusion 188 Re-EDTMP demonstrated the best potential as a radiopharmaceutical for bone cancer pain relief, encouraging further dosimetric studies and clinical trials. (orig.)

  3. Chitosan dan Aplikasi Klinisnya Sebagai Biomaterial

    Directory of Open Access Journals (Sweden)

    Bambang Irawan

    2015-10-01

    Full Text Available The development of new materials with both organic and inorganic structures is of great interest to obtain special material properties. Chitosan [2-amino-2-deoxy-D-glucan] can be obtained by N-deacetylation of chitin. Chitin is the second most abundant biopolymer in nature and the supporting material of crustaceans, insects, fungi etc. Chitosan is unique polysaccharide and has been widely used in various biomedical application due to its biocompatibility, low toxicity, biodegradability, non-immunogenic and non-carcinogenic character. In the past few years, chitosan and some of its modifications have been reported for use in biomedical applications such as artificial skin, wound dressing, anticoagulant, suture, drug delivery, vaccine carrier and dietary fibers. Recently, the use of chitosan and its derivatives has received much attention as temporary scaffolding to promotie mineralization or stimulate endochodral ossification. This article aims to give a broad overview of chitosan and its clinical applications as biomaterial.

  4. Green synthesis approach: extraction of chitosan from fungus mycelia.

    Science.gov (United States)

    Dhillon, Gurpreet Singh; Kaur, Surinder; Brar, Satinder Kaur; Verma, Mausam

    2013-12-01

    Chitosan, copolymer of glucosamine and N-acetyl glucosamine is mainly derived from chitin, which is present in cell walls of crustaceans and some other microorganisms, such as fungi. Chitosan is emerging as an important biopolymer having a broad range of applications in different fields. On a commercial scale, chitosan is mainly obtained from crustacean shells rather than from the fungal sources. The methods used for extraction of chitosan are laden with many disadvantages. Alternative options of producing chitosan from fungal biomass exist, in fact with superior physico-chemical properties. Researchers around the globe are attempting to commercialize chitosan production and extraction from fungal sources. Chitosan extracted from fungal sources has the potential to completely replace crustacean-derived chitosan. In this context, the present review discusses the potential of fungal biomass resulting from various biotechnological industries or grown on negative/low cost agricultural and industrial wastes and their by-products as an inexpensive source of chitosan. Biologically derived fungal chitosan offers promising advantages over the chitosan obtained from crustacean shells with respect to different physico-chemical attributes. The different aspects of fungal chitosan extraction methods and various parameters having an effect on the yield of chitosan are discussed in detail. This review also deals with essential attributes of chitosan for high value-added applications in different fields.

  5. Synthesis and characterization of calcium hydroxy and fluoroapatite functionalized with methyl phosphonic dichloride

    Energy Technology Data Exchange (ETDEWEB)

    Agougui, Hassen; Aissa, Abdallah [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia); Debbabi, Mongi, E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer Surface reactivity of apatites toward methyl phosphonic dichloride is tested. Black-Right-Pointing-Pointer Chemical analysis shows that hydroxyapatite is more reactive. Black-Right-Pointing-Pointer NMR spectra show the formation of Ca-O-P{sub org} and P{sub inorg}-O-P{sub org} bonds. Black-Right-Pointing-Pointer AFM indicated that the texture surface was changed by grafting. - Abstract: The nature of apatite-organic molecule interaction was the subject of many investigations. Grafting the organic molecule onto the inorganic support may precede through either formation of covalent bonds or ionic interaction between superficial hydroxyl on the apatite surface and organic functions. The hybrid materials obtained by functionalization of apatite surfaces with phosphonate moieties are of interest for their potential applications such in catalysis, chromatography and biomedical domain. In this scope, calcium hydroxyl and fluoroapatite (CaHAp and CaFAp) were prepared in the presence of the methyl phosphonic dichloride (MPO), by contact method in organic solvent at 25 Degree-Sign C for 2 days. The products are rigorously characterized by chemical analysis, infrared (IR), MAS-NMR spectroscopies, powder X-ray diffraction (XRD), atomic force microscopy (AFM) and specific surface area (SSA). The X-ray powder analysis showed that the crystallinity was sensibly affected by the presence of organic moieties. The IR spectroscopy showed new vibration modes appearing related to phosphonate groups essentially at 2930, 1315, 945, 764 and 514 cm{sup -1}. The {sup 31}P MAS NMR spectrum for hydroxy and fluoroapatite exhibits a single signal at 2.8 ppm. After reaction with (MPO) the spectra show the presence of new signals, assigned to the formation of organic-inorganic bond between the superficial hydroxyl groups of the apatite ({identical_to}CaOH) and ({identical_to}POH) and methyl phosphonic dichloride. The SSA decreases with increasing

  6. Metal phosphonate hybrid mesostructures: environmentally friendly multifunctional materials for clean energy and other applications.

    Science.gov (United States)

    Ma, Tian-Yi; Yuan, Zhong-Yong

    2011-10-17

    The synthesis of porous hybrid materials has been extended to mesoporous non-silica-based organic-inorganic hybrid materials, in which mesoporous metal phosphonates represent an important family. By using organically bridged polyphosphonic acids as coupling molecules, the homogeneous incorporation of a considerable number of organic functional groups into the metal phosphonate hybrid framework has been realized. Small amounts of organic additives and the pH value of the reaction solution have a large impact on the morphology and textural properties of the resultant hybrid mesoporous metal phosphonate solids. Cationic and nonionic surfactants can be used as templates for the synthesis of ordered mesoporous metal phosphonates. The materials are used as efficient adsorbents for heavy metal ions, CO₂, and aldehydes, as well as in the separation of polycyclic aromatic hydrocarbons. They are also useful photocatalysts under UV and simulated solar light irradiation for organic dye degradation. Further functionalization of the synthesized mesoporous hybrids makes them oxidation and acid catalysts, both with impressive performances in the fields of sustainable energy and environment. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Titanium-Phosphonate-Based Metal-Organic Frameworks with Hierarchical Porosity for Enhanced Photocatalytic Hydrogen Evolution

    KAUST Repository

    Li, Hui

    2018-02-01

    Photocatalytic hydrogen production is crucial for solar-to-chemical conversion process, wherein high-efficiency photocatalysts lie in the heart of this area. Herein a new photocatalyst of hierarchically mesoporous titanium-phosphonate-based metal-organic frameworks, featuring well-structured spheres, periodic mesostructure and large secondary mesoporosity, are rationally designed with the complex of polyelectrolyte and cathodic surfactant serving as the template. The well-structured hierarchical porosity and homogeneously incorporated phosphonate groups can favor the mass transfer and strong optical absorption during the photocatalytic reactions. Correspondingly, the titanium phosphonates exhibit significantly improved photocatalytic hydrogen evolution rate along with impressive stability. This work can provide more insights into designing advanced photocatalysts for energy conversion and render a tunable platform in photoelectrochemical field.

  8. Titanium-Phosphonate-Based Metal-Organic Frameworks with Hierarchical Porosity for Enhanced Photocatalytic Hydrogen Evolution

    KAUST Repository

    Li, Hui; Sun, Ying; Yuan, Zhong-Yong; Zhu, Yun-Pei; Ma, Tianyi

    2018-01-01

    Photocatalytic hydrogen production is crucial for solar-to-chemical conversion process, wherein high-efficiency photocatalysts lie in the heart of this area. Herein a new photocatalyst of hierarchically mesoporous titanium-phosphonate-based metal-organic frameworks, featuring well-structured spheres, periodic mesostructure and large secondary mesoporosity, are rationally designed with the complex of polyelectrolyte and cathodic surfactant serving as the template. The well-structured hierarchical porosity and homogeneously incorporated phosphonate groups can favor the mass transfer and strong optical absorption during the photocatalytic reactions. Correspondingly, the titanium phosphonates exhibit significantly improved photocatalytic hydrogen evolution rate along with impressive stability. This work can provide more insights into designing advanced photocatalysts for energy conversion and render a tunable platform in photoelectrochemical field.

  9. Magnesium doped gallium phosphonates Ga{sub 1-x}Mg{sub x}[H{sub 3+x}(O{sub 3}PCH{sub 2}){sub 3}N] (x = 0, 0.20) and the influence on proton conductivity

    Energy Technology Data Exchange (ETDEWEB)

    Homburg, Thomas; Reinsch, Helge; Stock, Norbert [Institut fuer Anorganische Chemie, Christian-Albrechts-Universitaet, Kiel (Germany); Tschense, Carsten B.L.; Senker, Juergen [Dept. of Inorganic Chemistry III, University of Bayreuth (Germany); Wolkersdoerfer, Konrad; Wark, Michael [Institut fuer Chemie, Carl von Ossietzky Universitaet Oldenburg (Germany); Toebbens, Daniel; Zander, Stefan [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany)

    2018-02-01

    In our contribution to the development of new proton conductive coordination polymers (CPs) we focus on the impact of a partial replacement of Ga{sup 3+} by Mg{sup 2+}. This approach should come along with the introduction of additional protons due to charge balances. In a first step we have synthesized an isostructural compound to the literature known compound AlH{sub 3}P3N [H{sub 6}P3N = nitrilotris(methylene)triphosphonic acid], where Al{sup 3+} is replaced by Ga{sup 3+}, since all attempts to incorporate Mg{sup 2+} ions directly into AlH{sub 3}P3N were not successful. The relative amount of Mg{sup 2+} and Ga{sup 3+} was established by EDX analysis. Rietveld refinement of the synchrotron data located the Ga{sup 3+} and Mg{sup 2+} ions on a split position, proving the disordered incorporation of the Mg{sup 2+} ions. Solid-state NMR spectroscopy confirms a disordered protonation of the phosphonate groups as well and shows that all amine groups are protonated. In order to investigate the effect on the proton conductivity the compounds Ga[H{sub 3}(O{sub 3}PCH{sub 2}){sub 3}N], denoted GaH{sub 3}P3N as well as Ga{sub 0.80}Mg{sub 0.20}[H{sub 3.20}(O{sub 3}PCH{sub 2}){sub 3}N], denoted GaMgH{sub 3.20}P3N, were characterized by electrochemical impedance spectroscopy (EIS). Arrhenius behavior in the investigated temperature range (70-130 C) was found for both compounds (activation energies of E{sub a} = 0.15 eV for GaH{sub 3}P3N and 0.17 eV for GaMgH{sub 3.20}P3N). The GaMgH{sub 3.20}P3N sample shows a reduced proton mobility (σ = 1.2 x 10{sup -4} S.cm{sup -1}) of about one order of magnitude in comparison to GaH{sub 3}P3N (σ = 1.0 x 10{sup -3} S.cm{sup -1}). (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Chemistry of the Enaminone of 1-Acetylnaphthalene under Microwave Irradiation Using Chitosan as a Green Catalyst

    Directory of Open Access Journals (Sweden)

    Huwaida M. E. Hassaneen

    2011-01-01

    Full Text Available Enaminone 1 was reacted with hydrazonoyl halides 2a-d to yield 3,4-disubstituted pyrazoles 6a-d. Coupling with arenediazonium chlorides afforded the 2-(arylhydrazono-3-(1-naphthalenyl-3-oxopropionaldehydes 13a-c. Compounds 13 could be utilized for the synthesis of a variety of arylpyrazoles, arylazolopyrimidines, and pyridazinones via reaction with hydrazines, aminoazoles, and active methylene derivatives, respectively. A comparative study of aforementioned reactions was carried out with chitosan as a basic ecofriendly catalyst under conventional heating as well as under pressurized microwave irradiation conditions.

  11. A Pyrene- and Phosphonate-Containing Fluorescent Probe as Guest Molecule in a Host Polymer Matrix

    Directory of Open Access Journals (Sweden)

    Jacqueline Marchand-Brynaert

    2013-02-01

    Full Text Available New host-guest materials have been prepared by incorporation of a home-made organic probe displaying a pyrene motif and a phosphonate function into a regular amphiphilic copolymer. Using powder X-Ray diffraction, photoluminescence and FT-IR spectroscopy, we have been able to study the non-covalent interactions between the host matrix and the guest molecule in the solid state. Interestingly, we have shown that the matrix directs the guest spatial localization and alters its properties. Thanks to the comparison of pyrene vs. N-pyrenylmaleimide derivatives, the influence of the chemical nature of the guest molecules on the non-covalent interactions with the host have been studied. In addition, using polyethylene glycol as a reference host, we have been able to evidence a true matrix effect within our new insertion materials. The phosphonated guest molecule appears to be a novel probe targeting the hydrophilic domain of the host copolymer.

  12. 21 CFR 173.255 - Methylene chloride.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Methylene chloride. 173.255 Section 173.255 Food... Solvents, Lubricants, Release Agents and Related Substances § 173.255 Methylene chloride. Methylene chloride may be present in food under the following conditions: (a) In spice oleoresins as a residue from...

  13. Reaction of acid esters of methylenebis(phosphonous acid) with carbonyl compounds

    International Nuclear Information System (INIS)

    Novikova, Z.S.; Odinets, I.L.; Lutsenko, I.F.

    1987-01-01

    The reaction of methylenebis(phosphonites) containing two hydrophosphoryl groupings with aliphatic and aromatic aldehydes and ketones in the presence of alkali metal fluorides leads to methylenebis(α-hydroxyalkylphosphinates). The reaction of methylenebis(phosphonites) containing one hydrophosphoryl groupings with carbonyl compounds in the presence of alkali metal fluorides proceeds with the formation of a new type of heterocyclic phosphorus compound, viz., 1,2λ 3 ,4λ 5 -oxadiphospholanes. The reaction of acid esters of methylenebis(phosphonous) acid with carbonyl compounds in the presence of alkali metal alkoxides or a tertiary amine is accompanied by phosphinate-phosphonate rearrangement of the intermediately formed α-hydroxylalkylphosphinates

  14. Chitosan metal-crosslinked beads applied for n-alkylmonoamines removal from aqueous solutions – a thermodynamic study

    International Nuclear Information System (INIS)

    Oliveira, Margarete; Simoni, Jose A.; Airoldi, Claudio

    2014-01-01

    Highlights: • Chitosan beads were successfully synthesized with divalent cations. • Well-formed bead structures containing cations act as acceptor electron sites. • n-Alkylmonoamine/bead interactions are favorably sorbed at the solid/liquid interface. • The thermodynamic data were favorably obtained from calorimetric titrations. • Crosslinked metal–chitosan beads can remove amine-like substances from an ecosystem. - Abstract: Chitosan has ability in coordinating divalent cations when immersed in crosslinked beads, after dripping: (i) chitosan gel into a copper solution, (ii) nickel chitosan gel into sodium hydroxide and (iii) chitosan/cobalt gel into sodium tripolyphosphate. The amounts of (1.82; 1.27 and 0.44) mmol · g −1 for copper, nickel and cobalt cations in these well-formed structures were determined, to give nitrogen/metal ratios of 3.52; 2.09 and 8.51, indicating the least effectiveness for cobalt in the coordination. Copper cation is well-adjusted in the coordination model through free amino and hydroxyl electron pairs, while amino and acetamino groups for nickel and cobalt were used. The chitosan–hydrogen bond breaking in bead formation caused decreases in crystallinity to yield amorphous structures for cobalt and nickel. The water mass fraction released during heating depends on the hydration of the cations, with the highest value of 0.20 for cobalt. The quantitative aspects of the interaction among cations on beads and basic n-alkylmonoamines determined via sorption batch methodology adjusted to the Langmuir isothermal model, with maximum sorption quantities to saturate nickel of (2.50; 2.38; 2.03; 1.79) mmol · g −1 and copper of (2.59; 2.29; 2.28; 1.92) mmol · g −1 for ethyl- propyl-, butyl- and pentylamines, respectively. The interaction energies quantitatively determined from isothermal titration calorimetry (ITC) at the solid/liquid interface resulted in exothermic enthalpic values. These negative enthalpy values combined to

  15. Chitosan Based Self-Assembled Nanoparticles in Drug Delivery

    Directory of Open Access Journals (Sweden)

    Javier Pérez Quiñones

    2018-02-01

    Full Text Available Chitosan is a cationic polysaccharide that is usually obtained by alkaline deacetylation of chitin poly(N-acetylglucosamine. It is biocompatible, biodegradable, mucoadhesive, and non-toxic. These excellent biological properties make chitosan a good candidate for a platform in developing drug delivery systems having improved biodistribution, increased specificity and sensitivity, and reduced pharmacological toxicity. In particular, chitosan nanoparticles are found to be appropriate for non-invasive routes of drug administration: oral, nasal, pulmonary and ocular routes. These applications are facilitated by the absorption-enhancing effect of chitosan. Many procedures for obtaining chitosan nanoparticles have been proposed. Particularly, the introduction of hydrophobic moieties into chitosan molecules by grafting to generate a hydrophobic-hydrophilic balance promoting self-assembly is a current and appealing approach. The grafting agent can be a hydrophobic moiety forming micelles that can entrap lipophilic drugs or it can be the drug itself. Another suitable way to generate self-assembled chitosan nanoparticles is through the formation of polyelectrolyte complexes with polyanions. This paper reviews the main approaches for preparing chitosan nanoparticles by self-assembly through both procedures, and illustrates the state of the art of their application in drug delivery.

  16. The supramolecular architecture of tris(naphthalene-1,5-diaminium) bis(5-aminonaphthalen-1-aminium) octakis[hydrogen (5-carboxypyridin-3-yl)phosphonate].

    Science.gov (United States)

    Wilk, Magdalena; Janczak, Jan; Videnova-Adrabinska, Veneta

    2012-09-01

    The asymmetric unit of the title compound, 3C(10)H(12)N(2)(2+)·2C(10)H(11)N(2)(+)·8C(6)H(5)NO(5)P(-), contains one and a half naphthalene-1,5-diaminium cations, in which the half-molecule has inversion symmetry, one 5-aminonaphthalen-1-aminium cation and four hydrogen (5-carboxypyridin-3-yl)phosphonate anions. The crystal structure is layered and consists of hydrogen-bonded anionic monolayers between which the cations are arranged. The acid monoanions are organized into one-dimensional chains along the [101] direction via hydrogen bonds established between the phosphonate sites. (C)O-H···N(py) hydrogen bonds (py is pyridine) crosslink the chains to form an undulating (010) monolayer. The cations serve both to balance the charge of the anionic network and to connect neighbouring layers via multiple hydrogen bonds to form a three-dimensional supramolecular architecture.

  17. New copper aryl phosphonates with auxiliary nitrogen ligands

    Czech Academy of Sciences Publication Activity Database

    Zima, Vítězslav; Svoboda, Jan; Yang, Y.-Ch.; Wang, S.-L.

    2012-01-01

    Roč. 14, č. 10 (2012), s. 3469-3477 ISSN 1466-8033 R&D Projects: GA ČR GA203/08/0208 Institutional research plan: CEZ:AV0Z40500505 Keywords : copper * phosphonates * structure Subject RIV: CA - Inorganic Chemistry Impact factor: 3.879, year: 2012

  18. Comparison of chitosan nanoparticles and chitosan hydrogels for vaccine delivery

    DEFF Research Database (Denmark)

    Gordon, Sarah; Saupe, Anne; McBurney, Warren

    2008-01-01

    In this work the potential of chitosan nanoparticles (CNP) and thermosensitive chitosan hydrogels as particulate and sustained release vaccine delivery systems was investigated. CNP and chitosan hydrogels were prepared, loaded with the model protein antigen ovalbumin (OVA) and characterised...... of the release of fluorescently-labelled OVA (FITC-OVA) from CNP and chitosan hydrogels in-vitro showed that approximately 50% of the total protein was released from CNP within a period of ten days; release of antigen from chitosan gel occurred in a more sustained manner, with ... released after 10 days. The slow release from gel formulations may be explained by the strong interactions of the protein with chitosan. While OVA-loaded CNP showed no significant immunogenicity, formulations of OVA in chitosan gel were able to stimulate both cell-mediated and humoral immunity in-vivo....

  19. Functionalization of chitosan by click chemistry

    Science.gov (United States)

    Cheaburu-Yilmaz, Catalina Natalia; Karavana, Sinem Yaprak; Yilmaz, Onur

    2017-12-01

    Chitosan modification represents a challenge nowadays. The variety of compounds which can be obtained with various architectures and different functionalities made it attractive to be used in fields like pharmacy and material science. Presents study deals with the chemical modification of chitosan by using click chemistry technique. The study adopted the approach of clicking azidated chitosan with a synthesized alkyne terminated polymer i.e. poly N isopropylacrylamide with thermoresponsive properties. Structures were confirmed by the FT-IR and HNMR spectra. Thermal characterization was performed showing different thermal behaviour with the chemical modification. The final synthesized graft copolymer can play important role within pharmaceutical formulations carrying drugs for topical or oral treatments.

  20. Chitosan and chemically modified chitosan beads for acid dyes sorption

    Institute of Scientific and Technical Information of China (English)

    AZLAN Kamari; WAN SAIME Wan Ngah; LAI KEN Liew

    2009-01-01

    The capabilities of chitosan and chitosan-EGDE (ethylene glycol diglycidyl ether) beads for removing Acid Red 37 (AR 37) and Acid Blue 25 (AB 25) from aqueous solution were examined. Chitosan beads were cross-linked with EGDE to enhance its chemical resistance and mechanical strength. Experiments were performed as a function of pH, agitation period and concentration of AR 37 and AB 25. It was shown that the adsorption capacities of chitosan were comparatively higher than chitosan-EGDE for both acid dyes. This is mainly because cross-linking using EGDE reduces the major adsorption sites -NH3+ on chitosan. Langmuir isotherm model showed best conformity compared to Freundlich and BET. The kinetic experimental data agreed very well to the pseudo second-order kinetic model. The desorption study revealed that after three cycles of adsorption and desorption by NaOH and HCl, both adsorbents retained their promising adsorption abilities. FT-IR analysis proved that the adsorption of acid dyes onto chitosan-based adsorbents was a physical adsorption. Results also showed that chitosan and chitosan-EGDE beads were favourable adsorbers and could be employed as low-cost alternatives for the removal of acid dyes in wastewater treatment.

  1. Heavy Metal Removal by Chitosan and Chitosan Composite

    International Nuclear Information System (INIS)

    Abdel-Mohdy, F.A.; El-Sawy, S.; Ibrahim, M.S.

    2005-01-01

    Radiation grafting of diethyl aminoethyl methacrylate (DEAEMA) on chitosan to impart ion exchange properties and to be used for the separation of metal ions from waste water, was carried out. The effect of experimental conditions such as monomer concentration and the radiation dose on grafting were studied. On using chitosan, grafted chitosan and some chitosan composites in metal ion removal they show high up-take capacity for Cu 2+ and lower uptake capacities for the other divalent metal ions used (Zn and Co). Competitive study, performed with solutions containing mixture of metal salts, showed high selectivity for Cu 2+ than the other metal ion. Limited grafting of DEAEMA polymer -containing specific functional groups-onto the chitosan backbone improves the sorption performance

  2. High temperature proton exchange membranes prepared from epoxycyclohexylethyltrimethoxysilane and amino trimethylene phosphonic acid as anhydrous proton conductors

    International Nuclear Information System (INIS)

    Chen, Cheng; Shen, Chunhui; Kong, Gengjin; Gao, Shanjun

    2013-01-01

    High temperature anhydrous proton exchange membranes based on phosphonic acid were prepared from epoxycyclohexylethyltrimethoxysilane (EHTMS) and amino trimethylene phosphonic acid (ATMP) by sol–gel process. The structures and properties of membranes with different phosphonic acid content were extensively characterized by FTIR, TG-DSC and XRD. Their proton conductivity under dry condition was also investigated under different temperature. The results show that the proton conductivity of the prepared membranes strongly depends on temperature, and the proton conductivity ranges from 8.81 × 10 −5 S cm −1 at 20 °C to 4.65 × 10 −2 S cm −1 at 140 °C under anhydrous condition. It indicates that the increasing temperature is favorable for congregating of the grafted–PO 3 H 2 and increasing of the proton mobility. In addition, from the results of AFM images, it was confirmed that the continuous distribution of phosphonic acid groups is favorable for the formation of the proton transport channel, which can significantly enhance the proton conductivity of the membranes. Highlights: ► Hybrid membranes of Epoxycyclohexylethyltrimethoxysilane and Amino trimethylene phosphonic acid. ► The proton conductivity is 4.65 × 10 −2 S cm −1 at 140 °C under anhydrous condition. ► Continuous uniform distributions of phosphonic acid groups can be observed by AFM. ► There could be hydrogen bond network within high temperature membranes

  3. High temperature proton exchange membranes prepared from epoxycyclohexylethyltrimethoxysilane and amino trimethylene phosphonic acid as anhydrous proton conductors

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Cheng [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China); Shen, Chunhui, E-mail: shenchunhui@whut.edu.cn [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China); Kong, Gengjin; Gao, Shanjun [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China)

    2013-06-15

    High temperature anhydrous proton exchange membranes based on phosphonic acid were prepared from epoxycyclohexylethyltrimethoxysilane (EHTMS) and amino trimethylene phosphonic acid (ATMP) by sol–gel process. The structures and properties of membranes with different phosphonic acid content were extensively characterized by FTIR, TG-DSC and XRD. Their proton conductivity under dry condition was also investigated under different temperature. The results show that the proton conductivity of the prepared membranes strongly depends on temperature, and the proton conductivity ranges from 8.81 × 10{sup −5} S cm{sup −1} at 20 °C to 4.65 × 10{sup −2} S cm{sup −1} at 140 °C under anhydrous condition. It indicates that the increasing temperature is favorable for congregating of the grafted–PO{sub 3}H{sub 2} and increasing of the proton mobility. In addition, from the results of AFM images, it was confirmed that the continuous distribution of phosphonic acid groups is favorable for the formation of the proton transport channel, which can significantly enhance the proton conductivity of the membranes. Highlights: ► Hybrid membranes of Epoxycyclohexylethyltrimethoxysilane and Amino trimethylene phosphonic acid. ► The proton conductivity is 4.65 × 10{sup −2} S cm{sup −1} at 140 °C under anhydrous condition. ► Continuous uniform distributions of phosphonic acid groups can be observed by AFM. ► There could be hydrogen bond network within high temperature membranes.

  4. Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Agougui, H.; Aissa, A. [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia); Maggi, S. [CNR-IC Istituto di Cristallografia, via Amendola 122/O, 70126 Bari (Italy); Debbabi, M., E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia)

    2010-12-15

    Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ({sup 1}H and {sup 31}P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH{sup -} groups of the apatitic structure.

  5. Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

    International Nuclear Information System (INIS)

    Agougui, H.; Aissa, A.; Maggi, S.; Debbabi, M.

    2010-01-01

    Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ( 1 H and 31 P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH - groups of the apatitic structure.

  6. Chitosan and carboxymethyl-chitosan capping ligands: Effects on the nucleation and growth of hydroxyapatite nanoparticles for producing biocomposite membranes.

    Science.gov (United States)

    Dumont, Vitor C; Mansur, Alexandra A P; Carvalho, Sandhra M; Medeiros Borsagli, Fernanda G L; Pereira, Marivalda M; Mansur, Herman S

    2016-02-01

    Synthetic biomaterials based on calcium phosphates (CaP) have been widely studied for bone tissue reconstruction therapies, but no definitive solution that fulfills all of the required properties has been identified. Thus, this study reports the synthesis of composite membranes based on nanohydroxyapatite particles (nHA) embedded in chitosan (CHI) and O-carboxymethyl chitosan (CMC) matrices produced using a one-step co-precipitation method in water media. Biopolymers were used as capping ligands for simultaneously controlling the nucleation and growth of the nHA particles during the precipitation process and also to form the polymeric network of the biocomposites. The bionanocomposites were extensively characterized using light microscopy (LM), scanning and transmission electron microscopy (SEM/TEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), atomic force microscopy (AFM), X-ray micro-CT analysis (μCT), andMTT (3-(4,5-dimethylthiazolyl-2)-2,5-diphenyltetrazoliumbromide) cell proliferation assays for cell cytotoxicity. The results demonstrated that the ligands used during the synthesis highly affected the composites produced, primarily due the changes in the mechanisms and kinetics of nucleation and growth of the HA particles at the nanoscale level. The SEMimages revealed that the use of carboxyl-functionalized chitosan (CMC) ligands significantly reduced the average size of theHA nanoparticles and caused the formation of a narrower size distribution (90±20nm) compared to theHAnanoparticles producedwith chitosan ligands (220±50nm). The same trend was verified by the AFM analysis,where the nHA particles were formed evenly dispersed in the polymer matrix. However, the CMC-based composites were more homogeneously distributed, which was endorsed by the images collected via X-ray micro-CT. The FTIR spectra and the XRD analysis indicated that nanosized hydroxyapatite was the predominant calcium

  7. Cytocompatibility of chitosan and collagen-chitosan scaffolds for tissue engineering

    Directory of Open Access Journals (Sweden)

    Ligia L. Fernandes

    2011-01-01

    Full Text Available In this work, chitosan and collagen-chitosan porous scaffolds were produced by the freeze drying method and characterized as potential skin substitutes. Their beneficial effects on soft tissues justify the choice of both collagen and chitosan. Samples were characterized using scanning electron microscope, Fourier Transform InfraRed Spectroscopy (FTIR and thermogravimetry (TG. The in vitro cytocompatibility of chitosan and collagen-chitosan scaffolds was evaluated with three different assays. Phenol and titanium powder were used as positive and negative controls, respectively. Scanning electron microscopy revealed the highly interconnected porous structure of the scaffolds. The addition of collagen to chitosan increased both pore diameter and porosity of the scaffolds. Results of FTIR and TG analysis indicate that the two polymers interact yielding a miscible blend with intermediate thermal degradation properties. The reduction of XTT ((2,3-bis[2-methyloxy-4-nitro-5-sulfophenyl]-2H-tetrazolium-5-carboxanilide and the uptake of Neutral Red (NR were not affected by the blend or by the chitosan scaffold extracts, but the blend and the titanium powder presented greater incorporation of Crystal Violet (CV than phenol and chitosan alone. In conclusion, collagen-chitosan scaffolds produced by freeze-drying methods were cytocompatible and presented mixed properties of each component with intermediate thermal degradation properties.

  8. Tribology and stability of organic monolayers on CrN: a comparison among silane, phosphonate, alkene, and alkyne chemistries.

    Science.gov (United States)

    Pujari, Sidharam P; Li, Yan; Regeling, Remco; Zuilhof, Han

    2013-08-20

    The fabrication of chemically and mechanically stable monolayers on the surfaces of various inorganic hard materials is crucial to the development of biomedical/electronic devices. In this Article, monolayers based on the reactivity of silane, phosphonate, 1-alkene, and 1-alkyne moieties were obtained on the hydroxyl-terminated chromium nitride surface. Their chemical stability and tribology were systematically investigated. The chemical stability of the modified CrN surfaces was tested in aqueous media at 60 °C at pH 3, 7, and 11 and monitored by static water contact angle measurements, X-ray photoelectron spectroscopy (XPS), ellipsometry, and Fourier transform infrared reflection absorption spectroscopy (FT-IRRAS). The tribological properties of the resulting organic monolayers with different end groups (fluorinated or nonfluorinated) were studied using atomic force microscopy (AFM). It was found that the fluorinated monolayers exhibit a dramatic reduction of adhesion and friction force as well as excellent wear resistance compared to those of nonfluorinated coatings and bare CrN substrates. The combination of remarkable chemical stability and superior tribological properties makes these fluorinated monolayers promising candidates for the development of robust high-performance devices.

  9. Omics for Investigating Chitosan as an Antifungal and Gene Modulator

    Directory of Open Access Journals (Sweden)

    Federico Lopez-Moya

    2016-03-01

    Full Text Available Chitosan is a biopolymer with a wide range of applications. The use of chitosan in clinical medicine to control infections by fungal pathogens such as Candida spp. is one of its most promising applications in view of the reduced number of antifungals available. Chitosan increases intracellular oxidative stress, then permeabilizes the plasma membrane of sensitive filamentous fungus Neurospora crassa and yeast. Transcriptomics reveals plasma membrane homeostasis and oxidative metabolism genes as key players in the response of fungi to chitosan. A lipase and a monosaccharide transporter, both inner plasma membrane proteins, and a glutathione transferase are main chitosan targets in N. crassa. Biocontrol fungi such as Pochonia chlamydosporia have a low content of polyunsaturated free fatty acids in their plasma membranes and are resistant to chitosan. Genome sequencing of P. chlamydosporia reveals a wide gene machinery to degrade and assimilate chitosan. Chitosan increases P. chlamydosporia sporulation and enhances parasitism of plant parasitic nematodes by the fungus. Omics studies allow understanding the mode of action of chitosan and help its development as an antifungal and gene modulator.

  10. Green synthesis of antimicrobial and antitumor N,N,N-trimethyl chitosan chloride/poly (acrylic acid)/silver nanocomposites.

    Science.gov (United States)

    Abu Elella, Mahmoud H; Mohamed, Riham R; Abdel-Aziz, Marwa M; Sabaa, Magdy W

    2018-05-01

    The present study is imported to solve two critical problems we face in our daily life which are microbial pollution and colon cancer. One pot green synthesis of a water soluble polyelectrolyte complex (PEC) between cationic polysaccharide as N,N,N-trimethyl chitosan chloride (TMC) and anionic polymer as poly (acrylic acid) (PAA) in presence of silver nanoparticles to yield (TMC/PAA/Ag) nanocomposites with different Ag weight ratios. Structure of TMC, PAA and TMC/PAA (PEC) were proved via different analysis tools. TMC/PAA and its Ag nanocomposites are used as antimicrobial agents against different pathogenic bacteria and fungi to solve microbial pollution. TMC/PAA-Silver nanocomposites had the highest antimicrobial activity which increases with increasing Ag %. Cytotoxicity data confirmed also that TMC/PAA/Ag (3%) had the most cytotoxic effect (the less cell viability %) towards colon cancer. TMC/PAA (PEC) was formed through electrostatic interactions between N-quaternized (-N + R 3 ) groups in TMC and carboxylate (-COO - ) groups in PAA. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Understanding the properties of chitosan aryl substituted thioureas in their role and potential as antibacterial agents

    Science.gov (United States)

    Khairul, Wan M.; Daud, Adibah Izzati; Ismail, Noraznawati

    2018-02-01

    In this study, the effort was to design and synthesize a series of thiourea-chitosan derivatives featuring five aryl substituted members namely N-chitosan-N'-(4-nitrobenzoyl) thiourea (1), N-chitosan-N'-(4-chlorobenzoyl) thiourea (2), N-chitosan-N'-(4-methylbenzoyl) thiourea (3), N-chitosan-N'-(2-iodobenzoyl) thiourea (4), and N-chitosan-N'-(2-methylbenzoyl) thiourea (5) via SN2 reaction pathway having different donating and withdrawing groups. Their molecular structures were then characterised by FT-IR, UV-Vis, and thermogravimetric analysis (TGA). The antimicrobial activities of these derivatives against four species bacteria Bacillus cereus, Staphylococcus aureus, Salmonella typhi, and Escherichia coli of both Gram-positive and Gram-negative type bacteria at minimum concentration 6mg/ml were carried out to investigate their potential as antibacterial agents. Compound 1 exhibited specific activity as it can only inhibit Gram-positive bacteria while other compounds 2-5 showed broad range spectrum activity as they were able to inhibit both Gram-positive and Gram-negative bacteria. Therefore, 1-5 showed good antibacterial activity and have high potential to be further developed as active materials in pharmaceutical interests.

  12. Microwave-Assisted Hydrolysis of Chitosan from Shrimp Shell Waste for Glucosammine Hydrochlorid Production

    International Nuclear Information System (INIS)

    Zaeni, Ahmad; Safitri, Endang; Fuadah, Badrotul; Sudiana, I Nyoman

    2017-01-01

    Chitin is the most widespread renewable natural sources following cellulose as the main source of chitosan. Chitin is isolated from crustacean waste and shrimp shells. Chitosan is derived from chitin throuhgt demineralisation, deproteination, decolorisation and deacetylation process using chemicals such as sodium hydroxide, hydrogen chloride and acetone. Glucosamine hydrochloride (GlcN-Cl) can be produced by hydrolysis of chitosan by using hydrogen chloride. During deacetylation and hydrolysis the solution is heated by hotplate or furnace. In this paper we use microwave instead of hotplate for production chitosan and GlcN-Cl. The research investigates effect of microwaves to amount of rendemen and their property. The chitosan was characterized its moisture content, solubility, and degree of deacetylation (DDA). Whereas the glucosammine hydrochloride characterized its functional groups using FTIR and crystallization by using X-Ray Difraction (XRD). The experimental results show that the use of microwave energy on deacetilation of chitosan and hydrolisis processes can decrease time consuming and reactant concentration during production. the DDA value obtained was very high from 70 to 85%. The results also show that microwaves meet chitosan and GlcN-Cl standards. (paper)

  13. Microwave-Assisted Hydrolysis of Chitosan from Shrimp Shell Waste for Glucosammine Hydrochlorid Production

    Science.gov (United States)

    Zaeni, Ahmad; Safitri, Endang; Fuadah, Badrotul; Nyoman Sudiana, I.

    2017-05-01

    Chitin is the most widespread renewable natural sources following cellulose as the main source of chitosan. Chitin is isolated from crustacean waste and shrimp shells. Chitosan is derived from chitin throuhgt demineralisation, deproteination, decolorisation and deacetylation process using chemicals such as sodium hydroxide, hydrogen chloride and acetone. Glucosamine hydrochloride (GlcN-Cl) can be produced by hydrolysis of chitosan by using hydrogen chloride. During deacetylation and hydrolysis the solution is heated by hotplate or furnace. In this paper we use microwave instead of hotplate for production chitosan and GlcN-Cl. The research investigates effect of microwaves to amount of rendemen and their property. The chitosan was characterized its moisture content, solubility, and degree of deacetylation (DDA). Whereas the glucosammine hydrochloride characterized its functional groups using FTIR and crystallization by using X-Ray Difraction (XRD). The experimental results show that the use of microwave energy on deacetilation of chitosan and hydrolisis processes can decrease time consuming and reactant concentration during production. the DDA value obtained was very high from 70 to 85%. The results also show that microwaves meet chitosan and GlcN-Cl standards.

  14. Synthesis and properties of ApA analogues with shortened phosphonate internucleotide linkage.

    Science.gov (United States)

    Králíková, Sárka; Buděšínský, Miloš; Barvík, Ivan; Masojídková, Milena; Točík, Zdeněk; Rosenberg, Ivan

    2011-01-01

    A complete series of the 2 '-5 ' and 3 '-5 ' regioisomeric types of r(ApA) and 2 '-d(ApA) analogues with the α-hydroxy-phosphonate C3 '-O-P-CH(OH)-C4 ″ internucleotide linkage, isopolar but non-isosteric with the phosphodiester one, were synthesized and their hybridization properties with polyU studied. Due to the chirality on the 5 '-carbon atom of the modified internucleotide linkage bearing phosphorus and hydroxy moieties, each regioisomeric type of ApA dimer is split into epimeric pairs. To examine the role of the 5 '-hydroxyl of the α-hydroxy-phosphonate moiety during hybridization, the appropriate r(ApA) analogues with 3 '(2 ')-O-P-CH(2)-C4 ″ linkage lacking the 5 '-hydroxyl were synthesized. Nuclear magnetic resonance (NMR) spectroscopy study on the conformation of the modified sugar-phosphate backbone, along with the hybridization measurements, revealed remarkable differences in the stability of complexes with polyU, depending on the 5 '-carbon atom configuration. Potential usefulness of the α-hydroxy-phosphonate linkage in modified oligoribonucleotides is discussed.

  15. Synthesis, physiochemical and optical properties of chitosan based dye containing naphthalimide group.

    Science.gov (United States)

    Kumar, Santosh; Koh, Joonseok

    2013-04-15

    A new biopolymer dye containing naphthalimide moiety was synthesized by reaction of N-naphthaloyl chitosan with 1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-piperazino-3-quinolinecarboxylic acid. N-naphthaloyl chitosan was synthesized by reaction of chitosan with 4-bromo-1,8-naphthalic anhydride in aqueous media by greener approach. The degree of substitution of chitosan biopolymer dye is 0.55 with a yield of 70%. The synthesized materials were characterized by using UV-vis, (1)H NMR, FTIR, and FT-Raman spectroscopy. Some physical properties and surface morphology were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Optical properties of chitosan biopolymer dye were evaluated by photoluminescence (PL) spectroscopy that showed red shift (λ(em)) peak at 442 nm and 551 nm at excitation wavelength 325 nm in comparison to chitosan. The solubility of chitosan biopolymer dye increased in most of the organic solvents. These results may provide new perspectives in biomedical applications as an optical and sensitive biosensor material. Copyright © 2013 Elsevier Ltd. All rights reserved.

  16. Acid-base catalysis of N-[(morpholine)methylene]daunorubicin.

    Science.gov (United States)

    Krause, Anna; Jelińska, Anna; Cielecka-Piontek, Judyta; Klawitter, Maria; Zalewski, Przemysław; Oszczapowicz, Irena; Wąsowska, Małgorzata

    2012-08-01

    The stability of N-[(morpholine)methylene]-daunorubicin hydrochloride (MMD) was investigated in the pH range 0.44-13.54, at 313, 308, 303 and 298 K. The degradation of MMD as a result of hydrolysis is a pseudo-first-order reaction described by the following equation: ln c = ln c(0) - k(obs)• t. In the solutions of hydrochloric acid, sodium hydroxide, borate, acetate and phosphate buffers, k(obs) = k(pH) because general acid-base catalysis was not observed. Specific acid-base catalysis of MMD comprises the following reactions: hydrolysis of the protonated molecules of MMD catalyzed by hydrogen ions (k(1)) and spontaneous hydrolysis of MMD molecules other than the protonated ones (k(2)) under the influence of water. The total rate of the reaction is equal to the sum of partial reactions: k(pH) = k(1) • a(H)+ • f(1) + k(2) • f(2) where: k(1) is the second-order rate constant (mol(-1) l s(-1)) of the specific hydrogen ion-catalyzed degradation of the protonated molecules of MMD; k(2) is the pseudo-first-order rate constant (s(-1)) of the water-catalyzed degradation of MMD molecules other than the protonated ones, f(1) - f(2) are fractions of the compound. MMD is the most stable at approx. pH 2.5.

  17. Synthesis and characterization of Cis-5-Norbornene-2, 3-dicarboxylic anhydride-chitosan

    International Nuclear Information System (INIS)

    Ku Marshilla Ku Ishak; Zulkifli Ahmad; Hazizan Mohd Akil

    2009-01-01

    Chitosan was chemically modified with bulky structure, cis-5-norbornene-2, 3-dicarboxylic anhydride and the characteristic of this modified chitosan was studied. The resulting material was analyzed by FTIR, TGA, DSC, XRD and SEM to study the effect of N-acylation to the polysaccharide structure. FTIR results show that the anhydride monomer was successfully bound to amine group of chitosan. Thermal analysis of the modified structure provides the chitosan fibers with thermal stability while XRD and SEM show the lost of crystallinity of modified chitosan. XRD of modified chitosan shows broader peak pattern and a considerable increase in a dimension while SEM of chitosan presented the single particle morphology while norbornene-chitosan shows aggromolarate behaviour due to the hydrophobic nature of norbornene pendant group which induced aggromolaration of the particles in modified structure.(author)

  18. Antiviral acyclic nucleoside phosphonates: New structures and prodrugs

    Czech Academy of Sciences Publication Activity Database

    Krečmerová, Marcela; Tichý, Tomáš; Pomeisl, Karel; Andrei, G.; Balzarini, J.; Snoeck, R.

    2016-01-01

    Roč. 1, č. 2 (2016), s. 37 [PharmaMed-2016. International Conference on Medicinal and Pharmaceutical Chemistry . 05.12.2016-07.12.2016, Dubai] R&D Projects: GA ČR(CZ) GA14-00522S Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonates * prodrugs * antivirals * 5-azacytosine Subject RIV: CC - Organic Chemistry

  19. Performance and Compatibility of Phosphonate-Based Superplasticizers for Concrete

    Directory of Open Access Journals (Sweden)

    Luigi Coppola

    2017-07-01

    Full Text Available The paper deals with the effectiveness of an innovative phosphonate-based superplasticizer (PNH for ready mixed concrete. Concrete specimens were manufactured by considering a constant initial workability, equal to 220 mm slump at the end of the mixing procedure. Workability was measured at 0, 30, and 60 min to evaluate the workability retention performances of the innovative superplasticizer. Compressive tests at 1, 7, and 28 days were carried out to evaluate the influence of the phosphonate-based superplasticizer on concrete setting and hardening. The concrete mixes were designed by considering 13 different cements to assess the superplasticizer-cement compatibility. The PNH-based admixture showed a better performance in terms of water reduction and workability retention with respect to napthalenesulphonate based admixtures (NSF; however, a higher dosage of PNH with respect to polycarboxylate ethers (PCEs was needed to get the same initial fluidity.

  20. Chitosan-Coated Collagen Membranes Promote Chondrocyte Adhesion, Growth, and Interleukin-6 Secretion

    Directory of Open Access Journals (Sweden)

    Nabila Mighri

    2015-11-01

    Full Text Available Designing scaffolds made from natural polymers may be highly attractive for tissue engineering strategies. We sought to produce and characterize chitosan-coated collagen membranes and to assess their efficacy in promoting chondrocyte adhesion, growth, and cytokine secretion. Porous collagen membranes were placed in chitosan solutions then crosslinked with glutaraldehyde vapor. Fourier transform infrared (FTIR analyses showed elevated absorption at 1655 cm-1 of the carbon–nitrogen (N=C bonds formed by the reaction between the (NH2 of the chitosan and the (C=O of the glutaraldehyde. A significant peak in the amide II region revealed a significant deacetylation of the chitosan. Scanning electron microscopy (SEM images of the chitosan-coated membranes exhibited surface variations, with pore size ranging from 20 to 50 µm. X-ray photoelectron spectroscopy (XPS revealed a decreased C–C groups and an increased C–N/C–O groups due to the reaction between the carbon from the collagen and the NH2 from the chitosan. Increased rigidity of these membranes was also observed when comparing the chitosan-coated and uncoated membranes at dried conditions. However, under wet conditions, the chitosan coated collagen membranes showed lower rigidity as compared to dried conditions. Of great interest, the glutaraldehyde-crosslinked chitosan-coated collagen membranes promoted chondrocyte adhesion, growth, and interleukin (IL-6 secretion. Overall results confirm the feasibility of using designed chitosan-coated collagen membranes in future applications, such as cartilage repair.

  1. Antibacterial activity of irradiated and non-irradiated chitosan and chitosan derivatives against Escherichia coli growth

    International Nuclear Information System (INIS)

    Tg Ahbrizal Farizal Tg Ahmad; Norimah Yusof; Kamarudin Bahari; Kamaruddin Hashim

    2006-01-01

    Samples of chitosan and four chitosan derivatives [ionic chitosan, chitosan lactate, carboxymethyl chitosan (C) and carboxymethyl chitosan (L)] were studied for their antibacterial activities against Escherichia coli growth. Chitosan and chitosan derivatives were prepared at concentrations 20, 100, 1000, 10000 ppm and 250, 1000, 5000, 10000, 20000 ppm, respectively. Each of the samples was tested before and after irradiation with electron beam at 25 kGy. The turbidity of bacterial growth media was measured periodically at 0, 0.5, 1, 2, 4, 6 and 24 h after inoculation using the optical density method. The results indicated that non- irradiated chitosan inhibited E. coli growth at 20 and 100 ppm. Meanwhile, irradiated chitosan at 100 and 1000 ppm concentration inhibited E. coli growth. Both irradiated and non-irradiated ionic chitosan inhibited E. coli growth at all concentrations used. Chitosan lactate was found to inhibit E. coli at concentration as low as 5000 ppm for both irradiated and non-irradiated samples. E. coli growth was not inhibited by carboxymethyl chitosan (C) and carboxymethyl chitosan (L), before and after irradiation. The findings suggested that chitosan has greater antibacterial activity as compared to the chitosan derivative samples. (Author)

  2. Chitosan from shrimp shell ( Crangon crangon ) and fish scales ...

    African Journals Online (AJOL)

    Chitosan is a naturally available biopolymer. It has been prepared by alkaline N deacetylation process of shrimp (Crangon crangon) chitin and fish (Labeorohita) chitin. The physico-chemical properties such as the degree of deacetylation (DD), solubility, water binding capacity, fat binding capacity and chitosan yield have ...

  3. Cell Adhesion and Proliferation on Sulfonated and Non-Modified Chitosan Films.

    Science.gov (United States)

    Martínez-Campos, Enrique; Civantos, Ana; Redondo, Juan Alfonso; Guzmán, Rodrigo; Pérez-Perrino, Mónica; Gallardo, Alberto; Ramos, Viviana; Aranaz, Inmaculada

    2017-05-01

    Three types of chitosan-based films have been prepared and evaluated: a non-modified chitosan film bearing cationizable aliphatic amines and two films made of N-sulfopropyl chitosan derivatives bearing both aliphatic amines and negative sulfonate groups at different ratios. Cell adhesion and proliferation on chitosan films of C2C12 pre-myoblastic cells and B16 cells as tumoral model have been tested. A differential cell behavior has been observed on chitosan films due to their different surface modification. B16 cells have shown lower vinculin expression when cultured on sulfonated chitosan films. This study shows how the interaction among cells and material surface can be modulated by physicochemical characteristics of the biomaterial surface, altering tumoral cell adhesion and proliferation processes.

  4. Styrene-divinylbenzene copolymer grafted with phosphonic acid dialkylesters

    Directory of Open Access Journals (Sweden)

    SMARANDA ILIESCU

    2004-12-01

    Full Text Available The functionalization of a crosslinked chloromethylated polystyrene 8% divinylbenzene copolymer with phosphonic ester groups is detailed. The reacton conditions were studied in order to determine the optimal conditions for obtaining only diesters. A statistical method for the calculation of the fraction of repetive units for the inited and final resin is proposed.

  5. Preparation of N,O-carboxymethyl chitosan coated alginate microcapsules and their application to Bifidobacterium longum BIOMA 5920.

    Science.gov (United States)

    Mi, Yu; Su, Ran; Fan, Dai-Di; Zhu, Xiao-Li; Zhang, Wen-Ni

    2013-07-01

    In order to greatly improve vitality of probiotic bacteria within the application, a novel biocompatible vehicle, N,O-carboxymethyl chitosan (NOCs) with appropriate degrees of substitution coat alginate (ALg) microparticles, was prepared by electrostatic droplet generation. The amount of chitosan (Cs) and N,O-carboxymethyl chitosan (NOCs) coated on the ALg microparticles was determined by differential scanning calorimetry. The surface morphology of ALg microparticles, Cs coated ALg microparticles and NOCs coated ALg microparticles was determined using scanning electron microscopy. The coating thickness of Cs coated ALg microparticles and that of NOCs coated ALg microparticles was directly observed with confocal laser scanning microscopy. In order to assess pH sensitivity of microparticles, the bovine serum albumin release from the microspheres was tested in acid solution (pH 2.0) for 2 h and subsequently in alkaline solution (pH 7.0) for 2 h. The survival of Bifidobacterium longum BIOMA 5920 loaded in NOCs coated with ALg microparticle was improved in simulated gastric juice (pH 2.0, for 2 h) compared to that of B. longum BIOMA 5920 loaded in ALg microparticles and Cs coated ALg microparticles. After incubation in simulated intestinal juices (pH 7.0, 2 h), the release of microencapsulated B. longum BIOMA 5920 was investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Synthesis of PVA-Chitosan Hydrogels for Wound Dressing Using Gamma Irradiation. Part I: Radiation Degradation of Chitosan in Solid State and in Solution

    International Nuclear Information System (INIS)

    Mahlous, M.; Tahtat, D.; Benamer, S.; Nacer Khodja, A.; Larbi Youcef, S.

    2010-01-01

    Chitosan is a partially deacetylated product of chitin, a very abundant polysaccharide, existing in exoskeleton of crustaceans. It is a polymer consisting of glucosamine and N-acetylglucosamine units linked by β-1-4-glycosidic bonds. Chitosan, like others polysaccharides, such as cellulose derivatives, alginates and carrageenan is widely used in food, medicine and cosmetic fields. Chitosan presents a variety of distinctive properties, such as biocompatibility, biodegradability, nontoxicity and nonantigenicity. Chitosan obtained by the deacetylation of chitin has, generally, a high molecular weight, which limits its solubility in aqueous solvents. The reduction of its molecular weight by degradation is usually used in order to improve its water solubility. Water-soluble chitosan exhibit some specific properties, such as antifungal activity, antimicrobial activity and plant growth promotion. Among the methods that have been tried to produce low molecular weight chitosan, radiation processing is the most promising one, since the process is simple, it is carried out at room temperature and no purification of the product is required after processing

  7. Poly(N-isopropylacrylamide) hydrogel/chitosan scaffold hybrid for three-dimensional stem cell culture and cartilage tissue engineering.

    Science.gov (United States)

    Mellati, Amir; Kiamahalleh, Meisam Valizadeh; Madani, S Hadi; Dai, Sheng; Bi, Jingxiu; Jin, Bo; Zhang, Hu

    2016-11-01

    Providing a controllable and definable three-dimensional (3D) microenvironment for chondrogenic differentiation of mesenchymal stem cells (MSCs) remains a great challenge for cartilage tissue engineering. In this work, poly(N-isopropylacrylamide) (PNIPAAm) polymers with the degrees of polymerization of 100 and 400 (NI100 and NI400) were prepared and the polymer solutions were introduced into the preprepared chitosan porous scaffolds (CS) to form hybrids (CSNI100 and CSNI400, respectively). SEM images indicated that the PNIPAAm gel partially occupied chitosan pores while the interconnected porous structure of chitosan was preserved. MSCs were incorporated within the hybrid and cell proliferation and chondrogenic differentiation were monitored. After 7-day incubation of the cell-laden constructs in a growth medium, the cell viability in CSNI100 and CSNI400 were 54 and 108% higher than that in CS alone, respectively. Glycosaminoglycan and total collagen contents increased 2.6- and 2.5-fold after 28-day culture of cell-laden CSNI400 in the chondrogenic medium. These results suggest that the hybrid structure composed of the chitosan porous scaffold and the well-defined PNIPAAm hydrogel, in particular CSNI400, is suitable for 3D stem cell culture and cartilage tissue engineering. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2764-2774, 2016. © 2016 Wiley Periodicals, Inc.

  8. Evaluation of antioxidant activities and chemical analysis of sulfated chitosan from Sepia prashadi.

    Science.gov (United States)

    Seedevi, Palaniappan; Moovendhan, Meivelu; Vairamani, Shanmugam; Shanmugam, Annaian

    2017-06-01

    The chitin and chitosan of S. prashadi was prepared through demineralization, deproteinzation, deacetylation process and sulfation were carried by chlorosulfonic acid in N,N-dimethylformamide. The sulfate content in chitosan was found to be 18.9%. The carbon, hydrogen and nitrogen composition of the sulfated chitosan were recorded 39.09%, 6.95% and 6.58% respectively. The structural analysis was done by using FT-IR and NMR spectroscopy technique. The DSC curves of sulfated chitosan showed a large endothermic peak resolved with T o value of 54.57°C and T P value of 97.46°C. The morphology of sulfated chitin and sulfated chitosan were studied by SEM. The Further in vitro antioxidant activity of sulfated chitosan was screened by scavenging activity of superoxide radical assay, hydroxyl radical scavenging assay, metal-ion chelating effect and reducing power. Its anticoagulant activity was tested for human plasma with respect to Activated Partial Thromboplastin Time (APTT) and Prothrombin Time (PT). Results prove that sulfated chitosan has potent antioxidant and anticoagulant activity. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Structure and properties of polyaniline interacting with H-phosphonates

    Czech Academy of Sciences Publication Activity Database

    Bláha, Michal; Trchová, Miroslava; Bober, Patrycja; Morávková, Zuzana; Zujovic, Z. D.; Filippov, Sergey K.; Prokeš, J.; Pilař, Jan; Stejskal, Jaroslav

    2017-01-01

    Roč. 232, October (2017), s. 79-86 ISSN 0379-6779 R&D Projects: GA ČR(CZ) GA17-04109S Institutional support: RVO:61389013 Keywords : conducting polymers * polyaniline * H-phosphonate Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 2.435, year: 2016

  10. Tetrofuranose nucleoside phosphonic acids: Synthesis and properties

    Czech Academy of Sciences Publication Activity Database

    Poláková, Ivana; Buděšínský, Miloš; Točík, Zdeněk; Rosenberg, Ivan

    2011-01-01

    Roč. 76, č. 5 (2011), s. 503-536 ISSN 0010-0765 R&D Projects: GA AV ČR KAN200520801; GA ČR GA203/09/0820; GA MŠk(CZ) LC06061; GA MŠk(CZ) LC06077 Institutional research plan: CEZ:AV0Z40550506 Keywords : tetrofuranosyl phosphonate * nucleotide analogues * phosphonomethoxy nucleosides * sugar hydroxyphosphonates Subject RIV: CC - Organic Chemistry Impact factor: 1.283, year: 2011

  11. Isosteric phosphonate pyrrolidine-based dinucleoside monophosphate analogues

    Czech Academy of Sciences Publication Activity Database

    Vaněk, Václav; Buděšínský, Miloš; Kavenová, Ivana; Rinnová, Markéta; Rosenberg, Ivan

    2003-01-01

    Roč. 22, 5/8 (2003), s. 1065-1067 ISSN 1525-7770. [International Roundtable Nucleosides, Nucleotides and Nucleic Acids /15./. Leuven, 10.09.2002-14.09.2002] R&D Projects: GA ČR GA203/01/1166; GA AV ČR IAA4055101 Institutional research plan: CEZ:AV0Z4055905 Keywords : pyrrolidine-based phosphonate nucleotides * ApA analogues * triplex Subject RIV: CC - Organic Chemistry Impact factor: 0.813, year: 2003

  12. Hydrothermal synthesis for new multifunctional materials: A few examples of phosphates and phosphonate-based hybrid materials

    Energy Technology Data Exchange (ETDEWEB)

    Rueff, Jean-Michel, E-mail: jean-michel.rueff@ensicaen.fr [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Poienar, Maria [National Institute for Research and Development in Electrochemistry and Condensed Matter, Plautius Andronescu Str Nr. 1, 300224 Timisoara (Romania); Guesdon, Anne; Martin, Christine; Maignan, Antoine [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Jaffrès, Paul-Alain [Université de Brest, Université Européenne de Bretagne, CNRS UMR 6521, CEMCA, SFR 148 ScInBios, 6 Avenue Victor Le Gorgeu, 29238 Brest (France)

    2016-04-15

    Novel physical or chemical properties are expected in a great variety of materials, in connection with the dimensionality of their structures and/or with their nanostructures, hierarchical superstructures etc. In the search of new advanced materials, the hydrothermal technique plays a crucial role, mimicking the nature able to produce fractal, hyperbranched, urchin-like or snow flake structures. In this short review including new results, this will be illustrated by examples selected in two types of materials, phosphates and phosphonates, prepared by this method. The importance of the synthesis parameters will be highlighted for a magnetic iron based phosphates and for hybrids containing phosphonates organic building units crystallizing in different structural types. - Graphical abstract: Phosphate dendrite like and phosphonate platelet crystals.

  13. Synthesis of carboxymethylated and quaternized chitosans and their therapeutic effect on nonalcoholic Fatty liver disease.

    Science.gov (United States)

    Liu, Xiaofei; Yang, Fan; Song, Tao; Zeng, Anrong; Wang, Qi; Sun, Zhong; Shen, Jun

    2011-10-12

    O-Carboxymethyl chitosan (O-CMCs) and N-((2-hydroxy-3-N,N-dimethylhexadecylammonium)propyl)chitosan chloride (N-CQCs) were synthesized for nonalcoholic fatty liver disease (NAFLD) treatment. The weight-average weight and substitution degree of O-CMCs and N-CQCs were 6.5 × 10(4) and 0.72 and 7.9 × 10(4) and 0.21, respectively. O-CMCs was negatively charged with a zeta-potential value of -31.82 mV, whereas that of N-CQCs was +36.1 mV, and both showed low cytotoxcity. Serum lipid level and liver fat accumulation were reduced with chitosan and its two derivatives. Furthermore, mRNA and protein expression assay of hepatic lipid metabolism enzymes and low-density lipoprotein receptor (LDL-R) were observed by RT-PCR and Western blot. Results showed that N-CQCs exhibited a more evident desired effect than chitosan and O-CMCs, indicating that amphiphilicity, solubility, and surface charge of chitosan and its two derivatives played roles in the expression of hepatic lipid metabolism enzymes and LDL-R. Therefore, dietary supplementation of O-CMCs and N-CQCs can alleviate the high fat diet induced aberrations related to NAFLD by their antilipidemic property.

  14. Interest of bone scintigraphy in the care of maxillary osteo-necroses induced by bis-phosphonates

    International Nuclear Information System (INIS)

    Agossa, Kevimy

    2012-01-01

    First cases of bis-phosphonates related osteonecrosis of jaws (BRONJ) have been described in 2003. Since then, this subject is one of the central concerns of several scientific communities, well beyond the oral sphere. The prevalence of BRONJ is evolving. Their etiology is not well established and the results of the treatments are inconstant. So many points that make the care to patients under bis-phosphonates really complex. Early diagnosis is essential in treatment outcome. So nuclear imaging including scintigraphy with technetium 99m seems to be helpful. It may allow detection before the onset of symptoms, facilitate localization of necrosis and it may be useful for the monitoring of such lesions after surgery. These are new applications for oncologist and dentist, in order to improve the management of patients treated by bis-phosphonates. (author) [fr

  15. Formation of phosphonates and pyrophosphates in the reactions of ...

    Indian Academy of Sciences (India)

    Bu-4-Me-C6H2O)2P(O)]2O (8) could be isolated, although the reaction mixture showed several other compounds in the phosphorus NMR. A possible pathway for the formation of phosphonate salts is proposed. The X-ray crystal structures of 4, ...

  16. Lyophilized insulin nanoparticles prepared from quaternized N-aryl derivatives of chitosan as a new strategy for oral delivery of insulin: in vitro, ex vivo and in vivo characterizations.

    Science.gov (United States)

    Mahjub, Reza; Radmehr, Moojan; Dorkoosh, Farid Abedin; Ostad, Seyed Naser; Rafiee-Tehrani, Morteza

    2014-12-01

    The purpose of this research was the development, in vitro, ex vivo and in vivo characterization of lyophilized insulin nanoparticles prepared from quaternized N-aryl derivatives of chitosan. Insulin nanoparticles were prepared from methylated N-(4-N,N-dimethylaminobenzyl), methylated N-(4 pyridinyl) and methylated N-(benzyl). Insulin nanoparticles containing non-modified chitosan and also trimethyl chiotsan (TMC) were also prepared as control. The effects of the freeze-drying process on physico-chemical properties of nanoparticles were investigated. The release of insulin from the nanoparticles was studied in vitro. The mechanism of the release of insulin from different types of nanoparticles was determined using curve fitting. The secondary structure of the insulin released from the nanoparticles was analyzed using circular dichroism and the cell cytotoxicity of nanoparticles on a Caco-2 cell line was determined. Ex vivo studies were performed on excised rat jejunum using Frantz diffusion cells. In vivo studies were performed on diabetic male Wistar rats and blood glucose level and insulin serum concentration were determined. Optimized nanoparticles with proper physico-chemical properties were obtained. The lyophilization process was found to cause a decrease in zeta potential and an increase in PdI as well as and a decrease in entrapment efficiency (EE%) and loading efficiency (LE%) but conservation in size of nanoparticles. Atomic force microscopy (AFM) images showed non-aggregated, stable and spherical to sub-spherical nanoparticles. The in vitro release study revealed higher release rates for lyophilized compared to non-lyophilized nanoparticles. Cytotoxicity studies on Caco-2 cells revealed no significant cytotoxicity for prepared nanoparticles after 3-h post-incubation but did show the concentration-dependent cytotoxicity after 24 h. The percentage of cumulative insulin determined from ex vivo studies was significantly higher in nanoparticles prepared

  17. Development of an injectable chitosan/marine collagen composite gel

    International Nuclear Information System (INIS)

    Wang Wei; Itoh, Soichiro; Aizawa, Tomoyasu; Demura, Makoto; Okawa, Atsushi; Sakai, Katsuyoshi; Ohkuma, Tsuneo

    2010-01-01

    A chitosan/marine-originated collagen composite has been developed. This composite gel was characterized and its biocompatibility, as well as an inflammatory reaction, was observed. The chitosan gel including N-3-carboxypropanoil-6-O-(carboxymethyl) chitosan of 3 mol%, 6-O-(carboxymethyl) chitosan of 62 mol% and 6-O-(carboxymethyl) chitin of 35 mol% was prepared and compounded with the salmon atelocollagen (SA) gel at different mixture ratios. The composite gels were injected subcutaneously in to the back of rats. The specimens were harvested for a histological survey as well as a tumor necrosis factor-alpha (TNF-α) assay by ELISA. The inflammatory cell infiltration and release of TNF-α were successively controlled low with the ratio of SA to chitosan at 10:90 or 20:80. The SA gel first, within 2 weeks, and then chitosan in the composite gel were slowly absorbed after implantation, followed by soft tissue formation. It is expected that this composite gel will be available as a carrier for tissue filler and drug delivery systems.

  18. Physicochemical Characterization of Biopolymer Chitosan Extracted from Shrimp Shells

    Directory of Open Access Journals (Sweden)

    Nezamaddin Mengelizadeh

    2015-02-01

    Full Text Available Chitosan is a deacetylated derivative of chitin, which is a naturally abundant mucopolysaccharide, supporting the matter of crustaceans, insects, and fungi. Because of its unique properties, such as non-toxicity, biodegradability, and biocompatibility, chitosan has a wide range of applications in various fields. The objective of the present work is to extract the polymer chitosan from Persian Gulf shrimp shells. In order to determine the physicochemical characteristics of the extracted chitosan, degree of deacetylation, molecular weight, water and fat binding capacities extraction rate, and apparent viscosity were measured using a variety of techniques including viscometry, weight measurement method and Fourier transform infrared spectroscopy (FTIR. The results of the study of the physicochemical properties, molecular weight (6.7×105 Da, degree of deacetylation (57%, ash content as well as yield (0.5% of the prepared chitosan indicated that shrimp processing wastes (shrimp shells are a good source of chitosan. The water binding capacity (521% and fat binding capacity (327% of the prepared chitosan are in good agreement with the other studies. The elemental analysis showed the C, H and N contents of 35.92%, 7.02%, and 8.66%, respectively. In this study, the antimicrobial activity of chitosan was evaluated against Staphylococcus aureus and Escherichia coli. The results indicated the high potential of chitosan as an antibacterial agent. Moreover, the results of the study indicated that shrimp shells are a rich source of chitin as 25.21% of the shell’s dry weight.

  19. Drug delivery glucantime in PVP/chitosan membranes

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Maria J.A.; Lugao, Ademar B.; Parra, Duclerc F., E-mail: mariajhho@yahoo.com.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Amato, Valdir S. [Universidade de Sao Paulo (DMIP/FM/USP), Sao Paulo, SP (Brazil). Faculdade de Medicina. Departamento de Molestias Infecciosas e Parasitarias

    2015-07-01

    The current study of polymer science considers the area of biomedical application very important to establish developments in new polymeric materials. Examples of that are hydrogels for controlled release of drugs. In this work, hydrogels of poly (N-2-vinil-pyrrolidone) (PVP) containing chitosan and clay nanoparticles were obtained and characterized to investigate chitosan influence on Glucantime drug delivery. The matrixes were crosslinked by gamma irradiation process with doses of 25 kGy. Hydrogels morphologies were observed by X Ray diffraction (DRX). Atomic Force Microscopy (AFM) and swelling kinetic at 22 °C to study the capacity of water retention and, finally, drug delivery tests were performed 'in vitro'. The system showed higher gel fraction for the matrix with 1.0% of clay and 0.5% of chitosan. In this case, besides the interactions of clay ions with PVP, there are interactions of chitosan amine group with PVP amide group. (author)

  20. Drug delivery glucantime in PVP/chitosan membranes

    International Nuclear Information System (INIS)

    Oliveira, Maria J.A.; Lugao, Ademar B.; Parra, Duclerc F.; Amato, Valdir S.

    2015-01-01

    The current study of polymer science considers the area of biomedical application very important to establish developments in new polymeric materials. Examples of that are hydrogels for controlled release of drugs. In this work, hydrogels of poly (N-2-vinil-pyrrolidone) (PVP) containing chitosan and clay nanoparticles were obtained and characterized to investigate chitosan influence on Glucantime drug delivery. The matrixes were crosslinked by gamma irradiation process with doses of 25 kGy. Hydrogels morphologies were observed by X Ray diffraction (DRX). Atomic Force Microscopy (AFM) and swelling kinetic at 22 °C to study the capacity of water retention and, finally, drug delivery tests were performed 'in vitro'. The system showed higher gel fraction for the matrix with 1.0% of clay and 0.5% of chitosan. In this case, besides the interactions of clay ions with PVP, there are interactions of chitosan amine group with PVP amide group. (author)

  1. Radiation degradation of chitosan

    International Nuclear Information System (INIS)

    Norzita Yacob; Maznah Mahmud; Norhashidah Talip; Kamarudin Bahari; Kamaruddin Hashim; Khairul Zaman Dahlan

    2010-01-01

    In order to obtain an oligo chitosan, degradation of chitosan s were carried out in solid state and liquid state. The effects of an irradiation on the molecular weight and viscosity of the chitosan were investigated using Ubbelohde Capillary Viscometer and Brookfield Viscometer respectively. The molecular weight and viscosity of the chitosan s were decreased with an increase in the irradiation dose. In the presence of hydrogen peroxide, the molecular weight of chitosan can be further decreased. (author)

  2. Yield Improvement and Energy Savings Uing Phosphonates as Additives in Kraft pulping

    Energy Technology Data Exchange (ETDEWEB)

    Ulrike W. Tschirner; Timothy Smith

    2007-03-31

    Project Objective: Develop a commercially viable modification to the Kraft process resulting in energy savings, increased yield and improved bleachability. Evaluate the feasibility of this technology across a spectrum of wood species used in North America. Develop detailed fundamental understanding of the mechanism by which phosphonates improve KAPPA number and yield. Evaluate the North American market potential for the use of phosphonates in the Kraft pulping process. Examine determinants of customer perceived value and explore organizational and operational factors influencing attitudes and behaviors. Provide an economic feasibility assessment for the supply chain, both suppliers (chemical supply companies) and buyers (Kraft mills). Provide background to most effectively transfer this new technology to commercial mills.

  3. Design, characterization and ex vivo evaluation of chitosan film integrating of insulin nanoparticles composed of thiolated chitosan derivative for buccal delivery of insulin.

    Science.gov (United States)

    Mortazavian, Elaheh; Dorkoosh, Farid Abedin; Rafiee-Tehrani, Morteza

    2014-05-01

    The purpose of this study is to optimize and characterize of chitosan buccal film for delivery of insulin nanoparticles that were prepared from thiolated dimethyl ethyl chitosan (DMEC-Cys). Insulin nanoparticles composed of chitosan and dimethyl ethyl chitosan (DMEC) were also prepared as control groups. The release of insulin from nanoparticles was studied in vitro in phosphate buffer solution (PBS) pH 7.4. Optimization of chitosan buccal films has been carried out by central composite design (CCD) response surface methodology. Independent variables were different amounts of chitosan and glycerol as mucoadhesive polymer and plasticizer, respectively. Tensile strength and bioadhesion force were considered as dependent variables. Ex vivo study was performed on excised rabbit buccal mucosa. Optimized insulin nanoparticles were obtained with acceptable physicochemical properties. In vitro release profile of insulin nanoparticles revealed that the highest solubility of nanoparticles in aqueous media is related to DMEC-Cys nanoparticles. CCD showed that optimized buccal film containing 4% chitosan and 10% glycerol has 5.81 kg/mm(2) tensile strength and 2.47 N bioadhesion forces. Results of ex vivo study demonstrated that permeation of insulin nanoparticles through rabbit buccal mucosa is 17.1, 67.89 and 97.18% for chitosan, DMEC and DMEC-Cys nanoparticles, respectively. Thus, this study suggests that DMEC-Cys can act as a potential enhancer for buccal delivery of insulin.

  4. Compound list: methylene dianiline [Open TG-GATEs

    Lifescience Database Archive (English)

    Full Text Available methylene dianiline DAPM 00155 ftp://ftp.biosciencedbc.jp/archive/open-tggates/LATEST/Human/in_vitro/methyle...es/LATEST/Rat/in_vivo/Liver/Single/methylene_dianiline.Rat.in_vivo.Liver.Single.zip ftp://ftp.biosciencedbc....jp/archive/open-tggates/LATEST/Rat/in_vivo/Liver/Repeat/methylene_dianiline.Rat.in_vivo.Liver.Repeat.zip ... ...ne_dianiline.Human.in_vitro.Liver.zip ftp://ftp.biosciencedbc.jp/archive/open-tggat

  5. Novel polymeric phosphonate scale inhibitors for improved squeeze treatment lifetimes

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, G.E.; Poynton, N.; McLaughlin, K.; Clark, D.R.

    1996-12-31

    New patented chemistry has provided an exciting discovery which may be used to reduce costs in scale squeeze applications. Phosphomethylated polyamines (PMPAs) have been found to possess outstanding adsorption-desorption properties which generate long squeeze lifetimes. This paper describes the core-flood tests and modelling work, which highlight these properties, plus additional scale inhibition performance studies to demonstrate the all-round capabilities of this chemistry for squeeze treatments. An example of a PMPA is used to show the extremely viable adsorption and desorption isotherms. These illustrate the efficient way in which the desorption occurs to minimise the chemical in the returns with a benefit of reduced chemical content in the discharge. The PMPA also demonstrates that both polymer and phosphonate properties can be embraced in a single product (e.g. dual scale control mechanisms) confirming that this chemistry is a true polymeric phosphonate. 13 refs., 12 figs., 1 tab.

  6. Synthesis of phosphonic acid derivatized bipyridine ligands and their ruthenium complexes.

    Science.gov (United States)

    Norris, Michael R; Concepcion, Javier J; Glasson, Christopher R K; Fang, Zhen; Lapides, Alexander M; Ashford, Dennis L; Templeton, Joseph L; Meyer, Thomas J

    2013-11-04

    Water-stable, surface-bound chromophores, catalysts, and assemblies are an essential element in dye-sensitized photoelectrosynthesis cells for the generation of solar fuels by water splitting and CO2 reduction to CO, other oxygenates, or hydrocarbons. Phosphonic acid derivatives provide a basis for stable chemical binding on metal oxide surfaces. We report here the efficient synthesis of 4,4'-bis(diethylphosphonomethyl)-2,2'-bipyridine and 4,4'-bis(diethylphosphonate)-2,2'-bipyridine, as well as the mono-, bis-, and tris-substituted ruthenium complexes, [Ru(bpy)2(Pbpy)](2+), [Ru(bpy)(Pbpy)2](2+), [Ru(Pbpy)3](2+), [Ru(bpy)2(CPbpy)](2+), [Ru(bpy)(CPbpy)2](2+), and [Ru(CPbpy)3](2+) [bpy = 2,2'-bipyridine; Pbpy = 4,4'-bis(phosphonic acid)-2,2'-bipyridine; CPbpy = 4,4'-bis(methylphosphonic acid)-2,2'-bipyridine].

  7. Gene silencing activity of siRNA polyplexes based on thiolated N,N,N-trimethylated chitosan.

    Science.gov (United States)

    Varkouhi, Amir K; Verheul, Rolf J; Schiffelers, Raymond M; Lammers, Twan; Storm, Gert; Hennink, Wim E

    2010-12-15

    N,N,N-Trimethylated chitosan (TMC) is a biodegradable polymer emerging as a promising nonviral vector for nucleic acid and protein delivery. In the present study, we investigated whether the introduction of thiol groups in TMC enhances the extracellular stability of the complexes based on this polymer and promotes the intracellular release of siRNA. The gene silencing activity and the cellular cytotoxicity of polyplexes based on thiolated TMC were compared with those based on the nonthiolated counterpart and the regularly used lipidic transfection agent Lipofectamine. Incubation of H1299 human lung cancer cells expressing firefly luciferase with siRNA/thiolated TMC polyplexes resulted in 60-80% gene silencing activity, whereas complexes based on nonthiolated TMC showed less silencing (40%). The silencing activity of the complexes based on Lipofectamine 2000 was about 60-70%. Importantly, the TMC-SH polyplexes retained their silencing activity in the presence of hyaluronic acid, while nonthiolated TMC polyplexes hardly showed any silencing activity, demonstrating their stability against competing anionic macromolecules. Under the experimental conditions tested, the cytotoxicity of the thiolated and nonthiolated siRNA complexes was lower than those based on Lipofectamine. Given the good extracellular stability and good silencing activity, it is concluded that polyplexes based on TMC-SH are attractive systems for further in vivo evaluations.

  8. Comparison of cadmium adsorption onto chitosan and epichlorohydrin crosslinked chitosan/eggshell composite

    Science.gov (United States)

    Rahmi; Marlina; Nisfayati

    2018-05-01

    The use of chitosan and epichlorohydrin crosslinked chitosan/eggshell composite for cadmium adsorption from water were investigated. The factors affecting adsorption such as pH and contact time were considered. The results showed that the optimum pH of adsorption was pH = 6.0 and the equilibrium time of adsorption was 40 min. The adsorption isotherm of Cd ions onto chitosan and composite were well fitted to Langmuir equation. The maximum adsorption capacity (fitting by Langmuir model) of chitosan and composite were 1.008 and 11.7647 mg/g, respectively. Adsorption performance of composite after regeneration was better than chitosan.

  9. Bis-phosphonate sequestering agents. Synthesis and preliminary evaluation for in vitro and in vivo uranium(VI) chelation

    Energy Technology Data Exchange (ETDEWEB)

    Sawicki, M.; Lecercle, D.; Taran, F. [CEA Saclay, IBiTecS, Serv Chim Bioorgan et Marquage, F-91191 Gif Sur Yvette (France); Grillon, G.; Le Gall, B.; Serandour, A.L.; Poncy, J.L. [CEA, DSV, DRR, Lab Radiotoxicol, F-91680 Bruyeres Le Chatel (France); Bailly, T.; Burgada, R.; Lecouvey, M.; Challeix, V. [CNRS, Lab Chim Struct Biomol, UMR 7033, F-93017 Bobigny (France); Leydier, A.; Pellet-Rostaing, S. [Univ Lyon 1, ICBMS, UMR 5246, Lab Catalyse et Synth Organ, F-69622 Villeurbanne (France); Ansoborlo, E. [CEA, DEN, DRCP, CETAMA, VRH Marcoule, F-30207 Bagnols Sur Ceze (France)

    2008-07-01

    A library of bis-phosphonate-based ligands was prepared using solution-phase parallel synthesis and tested for its uranium-binding properties. With the help of a screening method, based on a chromo-phoric complex displacement procedure, 23 dipodal and tripodal chelates bearing bis-phosphonate chelating functions were found to display very high affinity for the uranyl ion and were selected for evaluation of their in vivo uranyl-removal efficacy. Among them, 11 ligands induced a huge modification of the uranyl biodistribution by deviating the metal from kidney and bones to liver. Among the other ligands, the most potent was the dipodal bis-phosphonate 3C which reduced the retention of uranyl and increased its excretion by around 10% of the injected metal. (authors)

  10. Photocatalytic enhancement of floating photocatalyst: Layer-by-layer hybrid carbonized chitosan and Fe-N- codoped TiO{sub 2} on fly ash cenospheres

    Energy Technology Data Exchange (ETDEWEB)

    Song, Jingke; Wang, Xuejiang, E-mail: wangxj@tongji.edu.cn; Bu, Yunjie; Wang, Xin; Zhang, Jing; Huang, Jiayu; Ma, RongRong; Zhao, Jianfu

    2017-01-01

    Highlights: • Multifunctional TiO{sub 2} was coated on floating fly ash cenospheres. • TiO{sub 2} was integrated with carbonaceous layer from chitosan and Fe-N co-doping. • Carbonized chitosan improved the adsorption of pollutant and photon absorption ability of TiO{sub 2}. • Modified TiO{sub 2} exhibited superior photocatalytic activity and better recyclability. - Abstract: Due to the advantage of floating on water surface, floating photocatalysts show higher rates of radical formation and collection efficiencies. And they were expected to be used for solar remediation of non-stirred and non-oxygenated reservoirs. In this research, floating fly ash cenospheres (FAC) supported layer-by- layer hybrid carbonized chitosan and Fe-N-codoped TiO{sub 2} was prepared by a simple sol-gel method. The catalysts were characterized by X-ray diffraction(XRD), field emission scanning electron microscopy(FESEM), fourier transform infrared spectroscopy(FTIR), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy(DRS), nitrogen adsorption analyses for Brunauer-Emmett-Teller (BET) specific surface area. It is indicated that Fe-N codoped narrowed the material’s band gap, and the layer of carbonized chitosan (Cts) increased the catalyst’s adsorption capacity and the absorption ability of visible light. Comparing with Fe-N-TiO{sub 2}/FAC and N-TiO{sub 2}/FAC, the composite photocatalyst show excellent performance on the degradation of RhB. Photodegradation rate of RhB by Fe-N-TiO{sub 2}/FAC-Cts was 0.01018 min{sup −1}, which is about 1.5 and 2.09 times higher than Fe-N-TiO{sub 2}/FAC and N-TiO{sub 2}/FAC under visible light irradiation in 240 min, respectively. The dye photosentization, capture of holes and electrons by Fe{sup 3+} ion, and synergistic effect of adsorption and photodegradation were attributed to the results for the improvement of photocatalytic performance. The floating photocatalyst can be reused for at least three consecutive

  11. 29 CFR 1926.1152 - Methylene chloride.

    Science.gov (United States)

    2010-07-01

    ... 29 Labor 8 2010-07-01 2010-07-01 false Methylene chloride. 1926.1152 Section 1926.1152 Labor Regulations Relating to Labor (Continued) OCCUPATIONAL SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR... Methylene chloride. Note: The requirements applicable to construction employment under this section are...

  12. 29 CFR 1915.1052 - Methylene chloride.

    Science.gov (United States)

    2010-07-01

    ... 29 Labor 7 2010-07-01 2010-07-01 false Methylene chloride. 1915.1052 Section 1915.1052 Labor Regulations Relating to Labor (Continued) OCCUPATIONAL SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR... § 1915.1052 Methylene chloride. Note: The requirements applicable to shipyard employment under this...

  13. Preliminary assessment of developmental toxicity of Perfluorinated Phosphonic Acid in mice

    Science.gov (United States)

    Perfluorinated phosphonic acids (PFPAs) are a third member of the perfluoroalkyl acid (PFAA) family, and are structurally similar to the perfluoroalkyl sulfonates and perfluoroalkyl carboxylates. These emerging chemicals have recently been detected in the environment, particularl...

  14. Preparation and Characterization of Facilitated Transport Membranes Composed of Chitosan-Styrene and Chitosan-Acrylonitrile Copolymers Modified by Methylimidazolium Based Ionic Liquids for CO2 Separation from CH4 and N2

    Directory of Open Access Journals (Sweden)

    Ksenia V. Otvagina

    2016-06-01

    Full Text Available CO2 separation was found to be facilitated by transport membranes based on novel chitosan (CS–poly(styrene (PS and chitosan (CS–poly(acrylonitrile (PAN copolymer matrices doped with methylimidazolium based ionic liquids: [bmim][BF4], [bmim][PF6], and [bmim][Tf2N] (IL. CS plays the role of biodegradable film former and selectivity promoter. Copolymers were prepared implementing the latest achievements in radical copolymerization with chosen monomers, which enabled the achievement of outstanding mechanical strength values for the CS-based membranes (75–104 MPa for CS-PAN and 69–75 MPa for CS-PS. Ionic liquid (IL doping affected the surface and mechanical properties of the membranes as well as the gas separation properties. The highest CO2 permeability 400 Barrers belongs to CS-b-PS/[bmim][BF4]. The highest selectivity α (CO2/N2 = 15.5 was achieved for CS-b-PAN/[bmim][BF4]. The operational temperature of the membranes is under 220 °C.

  15. Oxidation-mediated chitosan as additives for creation of chitosan aerogels with diverse three-dimensional interconnected skeletons

    International Nuclear Information System (INIS)

    Zhang, Sizhao; Feng, Jian; Feng, Junzong; Jiang, Yonggang

    2017-01-01

    Highlights: • A new synthetic method for controlling morphology of chitosan aerogels is proposed. • Chitosan aerogels with nanoflake-like and nanofiber-like were prepared. • Textures of chitosan aerogels are strongly dependent upon the oxidation pattern. - Abstract: Naturally occurring polymer-based aerogels have myriad practical utilizations due to environmentally benign and fruitful resources. However, engineering morphology-controllable biomass aerogels still represents a great challenge. Here we present a facile solution to synthesize chitosan aerogels having distinguished textures by reacting oxidized chitosan with formaldehyde and chitosan sol. In more detail, chitosan was chemically oxidized using two types of oxidation agents such as ammonium persulphate (SPD) and sodium periodate (APS) to obtain corresponding oxidized chitosan, subsequently cross-linked with chitosan solution containing formaldehyde to harvest SPD-oxidized chitosan aerogels (SCAs) and APS-SPD-oxidized ones (ASCAs) after aging, solvent exchange and supercritical drying processes. We found that the morphologies of as-prepared chitosan aerogels are strongly dependent upon the oxidation pattern towards chitosan. The structural textures of SCAs and ASCAs appear nanoflake-like and nanofiber-like structures, which may be related to spatial freedom of active groups located in chitosan. Selected area electron diffraction analysis reveals that the crystalline properties of chitosan aerogels generally appear the serious deterioration comparing to raw chitosan owing to their interconnected skeletal structure formation. The occurrence of characteristic groups displays cross-linked chain construction by using chemical state measurements such as FT-IR and XPS. Further, a plausible mechanism for controlling morphology of chitosan aerogels is also established. This new family of method for creation of chitosan aerogels may open up a perspective for biomass aerogels with controllable textures.

  16. Oxidation-mediated chitosan as additives for creation of chitosan aerogels with diverse three-dimensional interconnected skeletons

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Sizhao, E-mail: bule-soul@hotmail.com; Feng, Jian, E-mail: fengj@nudt.edu.cn; Feng, Junzong; Jiang, Yonggang

    2017-02-28

    Highlights: • A new synthetic method for controlling morphology of chitosan aerogels is proposed. • Chitosan aerogels with nanoflake-like and nanofiber-like were prepared. • Textures of chitosan aerogels are strongly dependent upon the oxidation pattern. - Abstract: Naturally occurring polymer-based aerogels have myriad practical utilizations due to environmentally benign and fruitful resources. However, engineering morphology-controllable biomass aerogels still represents a great challenge. Here we present a facile solution to synthesize chitosan aerogels having distinguished textures by reacting oxidized chitosan with formaldehyde and chitosan sol. In more detail, chitosan was chemically oxidized using two types of oxidation agents such as ammonium persulphate (SPD) and sodium periodate (APS) to obtain corresponding oxidized chitosan, subsequently cross-linked with chitosan solution containing formaldehyde to harvest SPD-oxidized chitosan aerogels (SCAs) and APS-SPD-oxidized ones (ASCAs) after aging, solvent exchange and supercritical drying processes. We found that the morphologies of as-prepared chitosan aerogels are strongly dependent upon the oxidation pattern towards chitosan. The structural textures of SCAs and ASCAs appear nanoflake-like and nanofiber-like structures, which may be related to spatial freedom of active groups located in chitosan. Selected area electron diffraction analysis reveals that the crystalline properties of chitosan aerogels generally appear the serious deterioration comparing to raw chitosan owing to their interconnected skeletal structure formation. The occurrence of characteristic groups displays cross-linked chain construction by using chemical state measurements such as FT-IR and XPS. Further, a plausible mechanism for controlling morphology of chitosan aerogels is also established. This new family of method for creation of chitosan aerogels may open up a perspective for biomass aerogels with controllable textures.

  17. Pyrene-Phosphonate Conjugate: Aggregation-Induced Enhanced Emission, and Selective Fe3+ Ions Sensing Properties

    Directory of Open Access Journals (Sweden)

    Sachin D. Padghan

    2017-08-01

    Full Text Available A new pyrene-phosphonate colorimetric receptor 1 has been designed and synthesized in a one-step process via amide bond formation between pyrene butyric acid chloride and phosphonate-appended aniline. The pyrene-phosphonate receptor 1 showed aggregation-induced enhanced emission (AIEE properties in water/acetonitrile (ACN solutions. Dynamic light scattering (DLS characterization revealed that the aggregates of receptor 1 at 80% water fraction have an average size of ≈142 nm. Field emission scanning electron microscopy (FE-SEM analysis confirmed the formation of spherical aggregates upon solvent evaporation. The sensing properties of receptor 1 were investigated by UV-vis, fluorescence emission spectroscopy, and other optical methods. Among the tested metal ions, receptor 1 is capable of recognizing the Fe3+ ion selectively. The changes in spectral measurements were explained on the basis of complex formation. The composition of receptor 1 and Fe3+ ions was determined by using Job’s plot and found to be 1:1. The receptor 1–Fe3+ complex showed a reversible UV-vis response in the presence of EDTA.

  18. 2-N, 6-O-sulfated chitosan-assisted BMP-2 immobilization of PCL scaffolds for enhanced osteoinduction

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Lingyan [Key Laboratory for Ultrafine Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Engineering Research Center for Biomedical Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); CSIRO Manufacturing, Bayview Avenue, Clayton, Victoria 3168 (Australia); Department of Prosthodontics, College of Stomatology, Ninth People' s Hospital, School of Medicine, Shanghai Jiao Tong University, 639 Zhizaoju Road, Shanghai 200011 (China); Yu, Yuanman [Key Laboratory for Ultrafine Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Engineering Research Center for Biomedical Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Wang, Jing, E-mail: biomatwj@163.com [Key Laboratory for Ultrafine Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Engineering Research Center for Biomedical Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Werkmeister, Jerome A [CSIRO Manufacturing, Bayview Avenue, Clayton, Victoria 3168 (Australia); McLean, Keith M, E-mail: Keith.McLean@csiro.au [CSIRO Manufacturing, Bayview Avenue, Clayton, Victoria 3168 (Australia); Liu, Changsheng, E-mail: liucs@ecust.edu.cn [Key Laboratory for Ultrafine Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China); Engineering Research Center for Biomedical Materials of Ministry of Education, East China University of Science and Technology, Shanghai 200237 (China)

    2017-05-01

    The aim of this study was to develop a 2-N, 6-O-sulfated chitosan (26SCS) modified electrospun fibrous PCL scaffold for bone morphogenetic protein-2 (BMP-2) delivery to improve osteoinduction. The PCL scaffold was modified by an aminolysis reaction using ethylenediamine (ED) and 26SCS was immobilized via electrostatic interactions (PCL-N-S). Scaffolds were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and contact angle measurements. In vitro BMP-2 adsorption and release kinetics indicated that modified PCL-N-S scaffolds showed higher levels of binding of BMP-2 (about 30–100 times), moderative burst release (about one third), and prolonged releasing time compared to the unmodified PCL scaffold. The bioactivity of released BMP-2 determined by alkaline phosphatase (ALP) activity assay was maintained and improved 8– 12 times with increasing concentration of immobilized 26SCS on the scaffolds. In vitro studies demonstrated that bone marrow mesenchymal stem cells (BMSCs) attached more readily to the PCL-N-S scaffolds with increased spreading. In conclusion, 26SCS modified PCL scaffolds can be a potent system for the sustained and bioactive delivery of BMP-2. - Graphical abstract: Limited self-regenerating capacity of human body makes the reconstruction of critical size bone defect a significant challenge. Although bone morphogenetic protein-2 (BMP-2) is an important differentiation factor inducing bone regeneration, it's short half-life in vivo and potent side effect at high dosage still show lots of concerns in the clinical use. Herein, modification of electrospun PCL scaffolds was presented through immobilizing of sulfated chitosan (26SCS). The modified scaffolds effectively improve the binding capacity of BMP-2 and exhibited an enhanced bioactivity and sustained release in vitro. Thus, the use of 26SCS modified PCL scaffolds combined with BMP-2 could be a useful scaffold for tissue

  19. Chitosan coated carbon fiber microelectrode for selective in vivo detection of neurotransmitters in live zebrafish embryos

    International Nuclear Information System (INIS)

    Ozel, Rifat Emrah; Wallace, Kenneth N.; Andreescu, Silvana

    2011-01-01

    Graphical abstract: Chitosan coated fiber electrodes are sensitive to serotonin detection while rejecting physiological levels of ascorbic acid interferences. - Abstract: We report the development of a chitosan modified carbon fiber microelectrode for in vivo detection of serotonin. We find that chitosan has the ability to reject physiological levels of ascorbic acid interferences and facilitate selective and sensitive detection of in vivo levels of serotonin, a common catecholamine neurotransmitter. Presence of chitosan on the microelectrode surface was investigated using scanning electron microscopy (SEM) and cyclic voltammetry (CV). The electrode was characterized using differential pulse voltammetry (DPV). A detection limit of 1.6 nM serotonin with a sensitivity of 5.12 nA/μM, a linear range from 2 to 100 nM and a reproducibility of 6.5% for n = 6 electrodes were obtained. Chitosan modified microelectrodes selectively measure serotonin in presence of physiological levels of ascorbic acid. In vivo measurements were performed to measure concentration of serotonin in the live embryonic zebrafish intestine. The sensor quantifies in vivo intestinal levels of serotonin while successfully rejecting ascorbic acid interferences. We demonstrate that chitosan can be used as an effective coating to reject ascorbic acid interferences at carbon fiber microelectrodes, as an alternative to Nafion, and that chitosan modified microelectrodes are reliable tools for in vivo monitoring of changes in neurotransmitter levels.

  20. Chitosan coated carbon fiber microelectrode for selective in vivo detection of neurotransmitters in live zebrafish embryos

    Energy Technology Data Exchange (ETDEWEB)

    Ozel, Rifat Emrah [Department of Chemistry and Biomolecular Science, 8 Clarkson Ave, Potsdam, NY 136995810 (United States); Wallace, Kenneth N. [Department of Biology, Clarkson University, Potsdam, NY 136995810 (United States); Andreescu, Silvana, E-mail: eandrees@clarkson.edu [Department of Chemistry and Biomolecular Science, 8 Clarkson Ave, Potsdam, NY 136995810 (United States)

    2011-06-10

    Graphical abstract: Chitosan coated fiber electrodes are sensitive to serotonin detection while rejecting physiological levels of ascorbic acid interferences. - Abstract: We report the development of a chitosan modified carbon fiber microelectrode for in vivo detection of serotonin. We find that chitosan has the ability to reject physiological levels of ascorbic acid interferences and facilitate selective and sensitive detection of in vivo levels of serotonin, a common catecholamine neurotransmitter. Presence of chitosan on the microelectrode surface was investigated using scanning electron microscopy (SEM) and cyclic voltammetry (CV). The electrode was characterized using differential pulse voltammetry (DPV). A detection limit of 1.6 nM serotonin with a sensitivity of 5.12 nA/{mu}M, a linear range from 2 to 100 nM and a reproducibility of 6.5% for n = 6 electrodes were obtained. Chitosan modified microelectrodes selectively measure serotonin in presence of physiological levels of ascorbic acid. In vivo measurements were performed to measure concentration of serotonin in the live embryonic zebrafish intestine. The sensor quantifies in vivo intestinal levels of serotonin while successfully rejecting ascorbic acid interferences. We demonstrate that chitosan can be used as an effective coating to reject ascorbic acid interferences at carbon fiber microelectrodes, as an alternative to Nafion, and that chitosan modified microelectrodes are reliable tools for in vivo monitoring of changes in neurotransmitter levels.

  1. Impedance spectroscopy study of dehydrated chitosan and chitosan containing LiClO4

    International Nuclear Information System (INIS)

    Costa, M.M.; Terezo, A.J.; Matos, A.L.; Moura, W.A.; Giacometti, Jose A.; Sombra, A.S.B.

    2010-01-01

    Cast films of chitosan and chitosan containing LiClO 4 were characterized using Fourier transform infrared spectroscopy and the thermogravimetric technique. The electric properties of hydrated and dehydrated films were investigated with impedance spectroscopy in the frequency range from 0.1 Hz to 1 MHz, at temperatures varying from 30 to 110 o C. The frequency dependence of the impedance for dehydrated chitosan and chitosan containing LiClO 4 films indicated ionic conduction. Two relaxation peaks were evident on the imaginary curve of the electric modulus, which were assigned to ionic conduction. The peak at higher frequency was found for chitosan and chitosan containing LiClO 4 films. The peak at lower frequency was attributed to Li + conduction since it appeared only for the chitosan containing LiClO 4 . The peak frequency varied with the temperature according to an Arrhenius process with activation energies of circa of 0.6 and 0.45 eV, for H + and Li + conduction, respectively.

  2. Experimental evaluation of photocrosslinkable chitosan as a biologic adhesive with surgical applications.

    Science.gov (United States)

    Ono, K; Ishihara, M; Ozeki, Y; Deguchi, H; Sato, M; Saito, Y; Yura, H; Sato, M; Kikuchi, M; Kurita, A; Maehara, T

    2001-11-01

    In various surgical cases, effective tissue adhesives are required for both hemostasis (eg, intraoperative bleeding) and air sealing (eg, thoracic surgery). We have designed a chitosan molecule (Az-CH-LA) that can be photocrosslinked by ultraviolet (UV) light irradiation, thereby forming a hydrogel. The purpose of this work was to evaluate the effectiveness and safety of the photocrosslinkable chitosan hydrogel as an adhesive with surgical applications. The sealing ability of the chitosan hydrogel, determined as a bursting pressure, was assessed with removed thoracic aorta, trachea, and lung of farm pigs and in a rabbit model. The carotid artery and lung of rabbits were punctured with a needle, and the chitosan hydrogel was applied to, respectively, stop the bleeding and the air leakage. In vivo chitosan degradability and biologic responses were histologically assessed in animal models. The bursting pressure of chitosan hydrogel (30 mg/mL) and fibrin glue, respectively, was 225 +/- 25 mm Hg (mean +/- SD) and 80 +/- 20 mm Hg in the thoracic aorta; 77 +/- 29 mm Hg and 48 +/- 21 mm Hg in the trachea; and in the lung, 51 +/- 11 mm Hg (chitosan hydrogel), 62 +/- 4 mm Hg (fibrin glue, rubbing method), and 12 +/- 2 mm Hg (fibrin glue, layer method). The sealing ability of the chitosan hydrogel was stronger than that of fibrin glue. All rabbits with a carotid artery (n = 8) or lung (n = 8) that was punctured with a needle and then sealed with chitosan hydrogel survived the 1-month observation period without any bleeding or air leakage from the puncture sites. Histologic examinations demonstrated that 30 days after application, a fraction of the chitosan hydrogel was phagocytosed by macrophages, had partially degraded, and had induced the formation of fibrous tissues around the hydrogel. A newly developed photocrosslinkable chitosan has demonstrated strong sealing ability and a great potential for use as an adhesive in surgical operations.

  3. N-Trimethyl chitosan (TMC) nanoparticles loaded with influenza subunit antigen for intranasal vaccination : Biological properties and immunogenicity in a mouse model

    NARCIS (Netherlands)

    Amidi, Maryam; Romeijn, Stefan G.; Verhoef, J. Coos; Junginger, Hans E.; Bungener, Laura; Huckriede, Anke; Crommelin, Daan J. A.; Jiskoot, Wim

    2007-01-01

    In this study, the potential of N-trimethyl chitosan (TMC) nanoparticles as a carrier system for the nasal delivery of a monovalent influenza subunit vaccine was investigated. The antigen-loaded nanoparticles were prepared by mixing a solution containing TMC and monovalent influenza A subunit H3N2

  4. Redox reactions of methylene blue: a pulse radiolysis study

    International Nuclear Information System (INIS)

    Kishore, K.; Guha, S.N.; Mahadevan, J.; Moorthy, P.N.; Mittal, J.P.

    1989-01-01

    One-electron oxidation of methylene blue (MB - has been studied using specific oxidizing radicals such as Cl 2 - , Br 2 - , N 3 and Tl(II) in acidic and neutral aqueous solutions). The transient spectrum showed absorption maxima at 525 nm and 360 nm in the acidic pH region. At neutral pH also the absorption maxima were at 525 and 360 nm but the extinction coefficients were lower by 30%. A pK a of ∼4.3 was observed for the equilibrium MBH 3+ MB 2+ + H + . In the case of N 3 radical as the oxidant, the equilibrium: N 3 + MB = N 3 - + MB 2+ was observed for which an equilibrium constant of 120 was estimated from the experimental data. From this as well as from cyclic voltammetric experiments, the redox potential for the MB 2+ /MB + couple was calculated as 1.25 V vs NHE. The transient species produced by the reaction of OH radicals with methylene blue gave a very different spectrum with λ m = 400nm and a pK a of ∼ 8.6, and hence it is inferred that OH radicals do not bring about one-electron oxidation of the molecule. (author)

  5. Development of silver/titanium dioxide/chitosan adipate nanocomposite as an antibacterial coating for fruit storage

    Science.gov (United States)

    A novel nanocomposite of silver/titanium dioxide/chitosan adipate (Ag/TiO2/CS) was developed through photochemical reduction using a chitosan adipate template. Chitosan served as a reducing agent for the metal ions, and anchored metal ions by forming Ag–N coordination bonds and electrostatic attract...

  6. Rheological and structural studies of carboxymethyl derivatives of chitosan

    Science.gov (United States)

    Winstead, Cherese; Katagumpola, Pushpika

    2014-05-01

    The degrees of substitution of chitosan derivatives were varied and the viscoelastic behavior of these biopolymer solutions was studied using rheology. Chitosan is a cationic copolymer of glucosamine and N-acetylglucosamine obtained by alkaline deacetylation of chitin. Due to its inherent non-toxicity, biocompatibility, and biodegradability, chitosan has gained much interest. However, the poor solubility of the biopolymer in water and most common organic solvents limits its applications. Therefore, the focus of this work is the chemical modification of chitosan via carboxymethylation as well as studying the viscoelastic behavior of these polymer solutions. Varying degrees of substitution (DS) of carboxymethyl chitosan derivatives were synthesized by treating chitosan with monochloroacetic acid under alkylated medium varying the reaction time and temperature. The effect of degree of substitution on the rheology of these polymer solutions was studied as a function of concentration. The viscosity of chitosan derivatives sharply increased with increase in degree of substitution. G' and G" dependence on strain and angular frequency were studied and were found to exhibit predominantly viscous behavior. Additional characterization of the derivatized products were further studied using Fourier transform infrared (FT-IR), 1H Nuclear Magnetic Resonance (1H NMR) spectroscopy, X-ray diffraction (XRD), and thermal gravimetric analysis as well as differential scanning calorimetry (DSC). Degree of substitution (DS) was calculated by titrimetric method.

  7. Rheological and structural studies of carboxymethyl derivatives of chitosan

    International Nuclear Information System (INIS)

    Winstead, Cherese; Katagumpola, Pushpika

    2014-01-01

    The degrees of substitution of chitosan derivatives were varied and the viscoelastic behavior of these biopolymer solutions was studied using rheology. Chitosan is a cationic copolymer of glucosamine and N-acetylglucosamine obtained by alkaline deacetylation of chitin. Due to its inherent non-toxicity, biocompatibility, and biodegradability, chitosan has gained much interest. However, the poor solubility of the biopolymer in water and most common organic solvents limits its applications. Therefore, the focus of this work is the chemical modification of chitosan via carboxymethylation as well as studying the viscoelastic behavior of these polymer solutions. Varying degrees of substitution (DS) of carboxymethyl chitosan derivatives were synthesized by treating chitosan with monochloroacetic acid under alkylated medium varying the reaction time and temperature. The effect of degree of substitution on the rheology of these polymer solutions was studied as a function of concentration. The viscosity of chitosan derivatives sharply increased with increase in degree of substitution. G' and G' dependence on strain and angular frequency were studied and were found to exhibit predominantly viscous behavior. Additional characterization of the derivatized products were further studied using Fourier transform infrared (FT-IR), 1 H Nuclear Magnetic Resonance ( 1 H NMR) spectroscopy, X-ray diffraction (XRD), and thermal gravimetric analysis as well as differential scanning calorimetry (DSC). Degree of substitution (DS) was calculated by titrimetric method

  8. Synthesis and characterization of N-(2-hydroxy)propyl-3-trimethyl ammonium chitosan chloride for potential application in gene delivery.

    Science.gov (United States)

    Xiao, Bo; Wan, Ying; Wang, Xiaoyu; Zha, Qichen; Liu, Haoming; Qiu, Zhiye; Zhang, Shengmin

    2012-03-01

    A series of N-(2-hydroxy)propyl-3-trimethyl ammonium chitosan chloride (HTCC) samples with various degrees of quaternization ranging from 12.4 to 43.7% was synthesized. The structures and properties of HTCC were investigated by FT-IR, (1)H NMR, conductometric titration and XRD analysis. It was found that HTCC had a more amorphous structure than chitosan. HTCC samples showed significantly lower cytotoxicity than polyethyleneimine in HepG2 and HeLa cell lines. The samples spontaneously formed complexes with pGL3 luciferase plasmid. These complexes had desirable particle sizes (160-300 nm) and zeta potentials (10.8-18.7 mV) when the weight ratios of HTCC to plasmid altered in the range of 3:1-20:1. In vitro gene transfection results indicated that HTCC had significantly high transfection efficiency compared with chitosan for delivering pGL3 luciferase plasmid to HeLa cells. The results suggest that HTCC could be a promising non-viral vector for safe and efficient DNA delivery. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Irradiation gamma on chitosan films

    Energy Technology Data Exchange (ETDEWEB)

    Mello, Luana Miranda Lopes de; Souza, Adriana Regia Marques de; Arthur, Valter, E-mail: lumilopes@hotmail.com, E-mail: drilavras@yahoo.com.br, E-mail: arthur@cena.usp.br [Universidade Federal do Tocantins (UFT), Palmas,TO (Brazil). Departmento de Ciencia e Tecnologia de Alimentos; Universidade Federal de Goias (UFGO), Goiania (Brazil). Departmento de Ciencia e Tecnologia de Alimentos; Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil)

    2017-11-01

    Films are preformed structures, independent, that are used to wrap food after processing, increasing their shelf life and enhancing its bright and attractive appearance. They are prepared from biological materials as an alternative to the plastic synthetic containers to improve the quality of the environment. Chitosan is a biodegradable polymer composed of β-(1-4) linked D-glucosamine (deacetylated unit) and N-acetyl-D- glucosamine (acetylated unit). It is produced commercially by deacetylation of chitin, which is a structural component of the exoskeleton of crustaceans. She is able to form films and edible and/or biodegradable coatings. With the objective to evaluate the effect of different doses of gamma radiation (0, 5, 10 and 15 kGy) and chitosan concentrations (1 and 2%) in film properties, it was evaluated its optical, mechanical and morphological properties. The films were produced by casting. Irradiation did not affect the thickness of the films, but influenced its colors, increasing the tone of the film for a stronger yellowish color. This fact can be attributed to the increased concentration of C = O bonds of chitosan due to the breakdown of the chain reaction and the Maillard reaction. Irradiated films showed smoother surface and less rough, due to the degradation of the chitosan molecule and poor mechanical properties, not showing good flexibility and stretching. (author)

  10. Irradiation gamma on chitosan films

    International Nuclear Information System (INIS)

    Mello, Luana Miranda Lopes de; Souza, Adriana Regia Marques de; Arthur, Valter

    2017-01-01

    Films are preformed structures, independent, that are used to wrap food after processing, increasing their shelf life and enhancing its bright and attractive appearance. They are prepared from biological materials as an alternative to the plastic synthetic containers to improve the quality of the environment. Chitosan is a biodegradable polymer composed of β-(1-4) linked D-glucosamine (deacetylated unit) and N-acetyl-D- glucosamine (acetylated unit). It is produced commercially by deacetylation of chitin, which is a structural component of the exoskeleton of crustaceans. She is able to form films and edible and/or biodegradable coatings. With the objective to evaluate the effect of different doses of gamma radiation (0, 5, 10 and 15 kGy) and chitosan concentrations (1 and 2%) in film properties, it was evaluated its optical, mechanical and morphological properties. The films were produced by casting. Irradiation did not affect the thickness of the films, but influenced its colors, increasing the tone of the film for a stronger yellowish color. This fact can be attributed to the increased concentration of C = O bonds of chitosan due to the breakdown of the chain reaction and the Maillard reaction. Irradiated films showed smoother surface and less rough, due to the degradation of the chitosan molecule and poor mechanical properties, not showing good flexibility and stretching. (author)

  11. Evaluation of Hemagglutination Activity of Chitosan Nanoparticles Using Human Erythrocytes

    Directory of Open Access Journals (Sweden)

    Jefferson Muniz de Lima

    2015-01-01

    Full Text Available Chitosan is a polysaccharide composed of randomly distributed chains of β-(1-4 D-glucosamine and N-acetyl-D-glucosamine. This compound is obtained by partial or total deacetylation of chitin in acidic solution. The chitosan-based hemostatic agents have been gaining much attention in the management of bleeding. The aim of this study was to evaluate in vitro hemagglutination activity of chitosan nanoparticles using human erythrocytes. The preparation of nanoparticles was achieved by ionotropic gelification technique followed by neutralization with NaOH 1 mol/L−1. The hemagglutination activity was performed on a solution of 2% erythrocytes (pH 7.4 on PBS collected from five healthy volunteers. The hemolysis determination was made by spectrophotometric analysis. Chitosan nanoparticle solutions without NaOH addition changed the reddish colour of the wells into brown, suggesting an oxidative reaction of hemoglobin and possible cell lysis. All neutralized solutions of chitosan nanoparticles presented positive haemagglutination, without any change in reaction color. Chitosan nanoparticles presented hemolytic activity ranging from 186.20 to 223.12%, while neutralized solutions ranged from 2.56 to 72.54%, comparing to distilled water. Results highlight the need for development of new routes of synthesis of chitosan nanoparticles within human physiologic pH.

  12. Influence of Chitosan Treatment on Surrogate Serum Markers of Cholesterol Metabolism in Obese Subjects

    Directory of Open Access Journals (Sweden)

    Dieter Lütjohann

    2018-01-01

    Full Text Available Chitosan treatment results in significantly lower serum low density lipoprotein (LDL cholesterol concentrations. To assess the working mechanisms of chitosan, we measured serum surrogate markers of cholesterol absorption (campesterol, sitosterol, cholestanol, synthesis (lathosterol, lanosterol, desmosterol, and degradation to bile acids (7α-hydroxy-cholesterol, 27-hydroxy-cholesterol, corrected for cholesterol concentration (R_sterols. Over 12 weeks, 116 obese subjects (Body Mass Index, BMI 31.7, range 28.1–38.9 kg/m2 were studied under chitosan (n = 61 and placebo treatments (n = 55. The participants were briefly educated regarding improvement of nutrition quality and energy expenditure. Daily chitosan intake was 3200 mg. Serum LDL cholesterol concentration decreased significantly more (p = 0.0252 under chitosan (−8.67 ± 18.18 mg/dL, 5.6% than under placebo treatment (−1.00 ± 24.22 mg/dL, 0.9%. This reduction was not associated with the expected greater decreases in markers of cholesterol absorption under chitosan treatment. Also, increases in markers of cholesterol synthesis and bile acid synthesis under chitosan treatment were not any greater than under placebo treatment. In conclusion, a significant selective reduction of serum LDL cholesterol under chitosan treatment is neither associated with a reduction of serum surrogate markers of cholesterol absorption, nor with increases of markers for cholesterol and bile acid synthesis.

  13. Influence of chitosan concentration on mechanical and barrier properties of corn starch/chitosan films.

    Science.gov (United States)

    Ren, Lili; Yan, Xiaoxia; Zhou, Jiang; Tong, Jin; Su, Xingguang

    2017-12-01

    The active packaging films based on corn starch and chitosan were prepared through mixing the starch solution and the chitosan solution (1:1) by casting. The aim of this work was to characterize and analyze the effects of the chitosan concentrations (0, 21, 41, 61 and 81wt% of starch) on physicochemical, mechanical and water vapor barrier properties as well as morphological characteristics of the corn starch/chitosan (CS/CH) films. Starch molecules and chitosan could interact through hydrogen bonding as confirmed from the shift of the main peaks to higher wavenumbers in FTIR and the reduction of crystallinity in XRD. Results showed that the incorporation of chitosan resulted in an increase in film solubility, total color differences, tensile strength and elongation at break and a decrease in Young's modulus and water vapor permeability (WVP). Elongation at break of the CS/CH films increased with increasing of chitosan concentration, and reached a maximum at 41 wt%, then declined at higher chitosan concentration. The WVP of CS/CH films increased with an increase of chitosan concentration and the same tendency observed for the moisture content. The results suggest that this biodegradable CS/CH films could potentially be used as active packaging films for food and pharmaceutical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Model for the mechanism and regulation of chitosan synthesis in Mucor rouxii

    International Nuclear Information System (INIS)

    Davis, L.L.; Bartnicki-Garcia, S.

    1984-01-01

    The cell walls of mucoraceous fungi are characterized by the joint occurrence of chitosan and chitin, the β-1,4-linked polysaccharides of G1cN and G1cNAc, respectively. It has been proposed that chitosan is made from chitin by enzymatic deacetylation, but the evidence is inconclusive since the deacetylase isolated from Mucor rouxii is effective against glycol chitin, but not against genuine chitin; consequently, chitosan synthesis in vitro was not achieved. The authors discovered that the same deacetylase can deacetylate chitin efficiently if it is allowed to act on chitin chains as they are being formed; i.e. the simultaneous presence and operation of chitin synthetase and chitin deacetylase is required for chitosan synthesis. Subsequent studies on the effect of digitonin on chitosan synthesis were the basis for a model the authors have developed for the regulation of chitosan and chitin syntheses in vivo

  15. Scanning electron microscopy and swelling test of shrimp shell chitosan and chitosan-RGD scaffolds

    Science.gov (United States)

    Mandacan, M. C.; Yuniastuti, M.; Amir, L. R.; Idrus, E.; Suniarti, D. F.

    2017-08-01

    Shrimp shell chitosan and chitosan-RGD scaffold membranes are produced to be biocompatible with tissue engineering. Nonetheless, their architectural properties have not yet been studied. Analyze the architectural properties of chitosan and chitosan-RGD scaffolds. Analyze pore count and size, interpore distance, and porosity (using SEM testing and ImageJ analysis) and water absorption (using a swelling test). The properties of the chitosan and chitosan-RGD scaffolds were as follows, respectively. The pore counts were 225 and 153; pore size, 171.4 μam and 180.2 μam interpore distance, 105.7 μam and 101.4 μam porosity, 22% and 10.2%; and water absorption, 9.1 mgH2O/mgScaffold and 19.3 mgH2O/mgScaffold. The shrimp shell chitosan-RGD membrane scaffold was found to have architectural properties that make it more conducive to use in tissue engineering.

  16. Transfection efficiency of chitosan and thiolated chitosan in retinal pigment epithelium cells: A comparative study

    Directory of Open Access Journals (Sweden)

    Ana V Oliveira

    2013-01-01

    Full Text Available Objective: Gene therapy relies on efficient vector for a therapeutic effect. Efficient non-viral vectors are sought as an alternative to viral vectors. Chitosan, a cationic polymer, has been studied for its gene delivery potential. In this work, disulfide bond containing groups were covalently added to chitosan to improve the transfection efficiency. These bonds can be cleaved by cytoplasmic glutathione, thus, releasing the DNA load more efficiently. Materials and Methods: Chitosan and thiolated chitosan nanoparticles (NPs were prepared in order to obtain a NH3 + :PO4− ratio of 5:1 and characterized for plasmid DNA complexation and release efficiency. Cytotoxicity and gene delivery studies were carried out on retinal pigment epithelial cells. Results: In this work, we show that chitosan was effectively modified to incorporate a disulfide bond. The transfection efficiency of chitosan and thiolated chitosan varied according to the cell line used, however, thiolation did not seem to significantly improve transfection efficiency. Conclusion: The apparent lack of improvement in transfection efficiency of the thiolated chitosan NPs is most likely due to its size increase and charge inversion relatively to chitosan. Therefore, for retinal cells, thiolated chitosan does not seem to constitute an efficient strategy for gene delivery.

  17. Preparation of polyvinyl alcohol graphene oxide phosphonate film and research of thermal stability and mechanical properties.

    Science.gov (United States)

    Li, Jihui; Song, Yunna; Ma, Zheng; Li, Ning; Niu, Shuai; Li, Yongshen

    2018-05-01

    In this article, flake graphite, nitric acid, peroxyacetic acid and phosphoric acid are used to prepare graphene oxide phosphonic and phosphinic acids (GOPAs), and GOPAs and polyvinyl alcohol (PVA) are used to synthesize polyvinyl alcohol graphene oxide phosphonate and phosphinate (PVAGOPs) in the case of faint acidity and ultrasound irradiation, and PVAGOPs are used to fabricate PVAGOPs film, and the structure and morphology of GOPAs, PVAGOPs and PVAGOPs film are characterized, and the thermal stability and mechanical properties of PVAGOPs film are investigated. Based on these, it has been proved that GOPAs consist of graphene oxide phosphonic acid and graphene oxide phosphinic acid, and there are CP covalent bonds between them, and PVAGOPs are composed of GOPAs and PVA, and there are six-member lactone rings between GOPAs and PVA, and the thermal stability and mechanical properties of PVAGOPs film are improved effectively. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. The dispersion of fine chitosan particles by beads-milling

    Science.gov (United States)

    Rochima, Emma; Utami, Safira; Hamdani, Herman; Azhary, Sundoro Yoga; Praseptiangga, Danar; Joni, I. Made; Panatarani, Camellia

    2018-02-01

    This research aimed to produce fine chitosan particles from a crab shell waste by beads-milling method by two different concentration of PEG as dispersing agent (150 and 300 wt. %). The characterization was performed to obtain the size and size distribution, the characteristics of functional groups and the degree of deacetylation. The results showed that the chitosan fine particles was obtained with a milling time 120 minutes with the best concentration of PEG 400 150 wt. %. The average particle size of the as-prepared suspension is 584 nm after addition of acetic acid solution (1%, v/v). Beads milling process did not change the glucosamine and N-acetylglucosamine content on chitosan structure which is indicated by degree of deacetylation higher than 70%. It was concluded that beads milling process can be applied to prepare chitosan fineparticles by proper adjustment in the milling time, pH and dosage of dispersing agent.

  19. Antiretrovirus activity of a novel class of acyclic pyrimidine nucleoside phosphonates

    Czech Academy of Sciences Publication Activity Database

    Balzarini, J.; Pannecouque, C.; De Clercq, E.; Aquaro, S.; Perno, C. F.; Egberink, H.; Holý, Antonín

    2002-01-01

    Roč. 46, č. 7 (2002), s. 2185-2193 ISSN 0066-4804 R&D Projects: GA ČR GV203/96/K001 Institutional research plan: CEZ:AV0Z4055905 Keywords : nucleoside phosphonates Subject RIV: CC - Organic Chemistry Impact factor: 4.215, year: 2002

  20. Thermoresponsive behavior of chitosan-g-N-isopropylacrylamide copolymer solutions.

    Science.gov (United States)

    Recillas, Maricarmen; Silva, Luisa L; Peniche, Carlos; Goycoolea, Francisco M; Rinaudo, Marguerite; Argüelles-Monal, Waldo M

    2009-06-08

    Chitosan-g-N-isopropylacrylamide (NIPAm) water-soluble copolymers were synthesized and characterized by FTIR and (1)H NMR spectroscopies combined with conductometric and potentiometric titrations. Their thermoresponsive, fully reversible, behavior in aqueous solutions was characterized by means of microcalorimetry and rheology. During heating of copolymer solutions there is a well-known endothermic effect, which coincides with a marked increase in G' and a moderate decrement in G'' due to the formation of a hydrophobic network at the expense of the net amount of sol fraction. It was also found that a straight dependence between the values of G' above the LCST and the enthalpies associated with the transition reflecting that the connectivity in the gel network is governed by the net number of formed enthalpic-hydrophobic driven-junctions. Both the LCST and the enthalpy change vary with the ionic strength of copolymer solutions, but no dependence was found with the neutralization of the polyelectrolyte chain.

  1. O emprego de quitosana quimicamente modificada com anidrido succínico na adsorção de azul de metileno The use of chemical modified chitosam with succinic anhydride in the methylene blue adsorption

    Directory of Open Access Journals (Sweden)

    Ilauro S. Lima

    2006-06-01

    Full Text Available The adsorption capacity of alpha-chitosan and its modified form with succinic anhydride was compared with the traditional adsorbent active carbon by using the dye methylene blue, employed in the textile industry. The isotherms for both biopolymers were classified as SSA systems in the Giles model, more specifically in L class and subgroup 3. The dye concentration in the supernatant in the adsorption assay was determined through electronic spectroscopy. By calorimetric titration thermodynamic data of the interaction between methyene blue and the chemically modified chitosan at the solid/liquid interface were obtained. The enthalpy of the dye/chitosan interaction gave 2.47 ± 0.02 kJ mol-1 with an equilibrium constant of 7350 ± 10 and for the carbon/dye interaction this constant gave 5951 ± 8. The spontaneity of these adsorptions are reflected by the free Gibbs energies of -22.1 ± 0.4 and -21.5 ± 0.2 kJ mol-1, respectively, found for these systems. This new adsorbent derived from a natural polysaccharide is as efficient as activated carbon. However 97% of the bonded dye can be eluted by sodium chloride solution, while this same operation elutes only 42% from carbon. Chitosan is efficient in dye removal with the additional advantage of being cheap, non-toxic, biocompatible and biodegradable.

  2. Preparation and characterisation of irradiated crab chitosan and New Zealand Arrow squid pen chitosan

    International Nuclear Information System (INIS)

    Shavandi, Amin; Bekhit, Adnan A.; Bekhit, Alaa El-Din A.; Sun, Zhifa; Ali, M. Azam

    2015-01-01

    The properties of chitosan from Arrow squid (Nototodarus sloanii) pen (CHS) and commercial crab shell (CHC) were investigated using FTIR, DSC, SEM and XRD before and after irradiation at the dose of 28 kGy in the presence or absence of 5% water. Also, the viscosity, deacetylation degree, water and oil holding capacities, colour and antimicrobial activities of the chitosan samples were determined. Irradiation decreased (P < 0.05) the viscosity of CHC from 0.21 to 0.03 Pa s and of CHS from 1.71 to 0.23 Pa s. The inclusion of water had no effect on the viscosity of irradiated chitosan. Irradiation did not affect the degree of deacetylation of CHC, but increased the deacetylation degree of CHS from 72.78 to 82.29% in samples with 5% water. Water and oil holding capacities of CHS (1197.30% and 873.3%, respectively) were higher (P < 0.05) than those found in CHC (340.70% and 264.40%, respectively). The water and oil holding capacities were decreased for both types of chitosan irradiation, but were not affected by the addition of water. Squid pen chitosan was whiter in colour (White Index = 90.06%) compared to CHC (White Index = 83.70%). Generally, the CHC samples (control and irradiated) exhibited better antibacterial activity compared to CHS, but the opposite was observed with antifungal activity. - Highlights: • Chitosan prepared from Arrow squid pens (Nototodarus sloanii). • Chitosan samples were gamma irradiated at 28 kGy. • Squid pen chitosan showed high fat and water uptake capacities compared to crab shell chitosan. • Gamma irradiation enhanced the DDA of squid pen chitosan but not crab shell chitosan.

  3. N-PEG´ylation of chitosan via "click chemistry" reactions

    Czech Academy of Sciences Publication Activity Database

    Kulbokaite, R.; Ciuta, G.; Netopilík, Miloš; Makuška, R.

    2009-01-01

    Roč. 69, č. 10 (2009), s. 771-778 ISSN 1381-5148 R&D Projects: GA ČR GA203/07/0659 Institutional research plan: CEZ:AV0Z40500505 Keywords : chitosan * poly(ethylene glycol) * click chemistry Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.461, year: 2009

  4. Two-Ply Composite Membranes with Separation Layers from Chitosan and Sulfoethylcellulose on a Microporous Support Based on Poly(diphenylsulfone-N-phenylphthalimide

    Directory of Open Access Journals (Sweden)

    Svetlana V. Kononova

    2017-12-01

    Full Text Available Two-ply composite membranes with separation layers from chitosan and sulfoethylcellulose were developed on a microporous support based on poly(diphenylsulfone-N-phenylphthalimide and investigated by use of X-ray diffraction and scanning electron microscopy methods. The pervaporation properties of the membranes were studied for the separation of aqueous alcohol (ethanol, propan-2-ol mixtures of different compositions. When the mixtures to be separated consist of less than 15 wt % water in propan-2-ol, the membranes composed of polyelectrolytes with the same molar fraction of ionogenic groups (-NH3+ for chitosan and -SO3− for sulfoethylcellulose show high permselectivity (the water content in the permeate was 100%. Factors affecting the structure of a non-porous layer of the polyelectrolyte complex formed on the substrate surface and the contribution of that complex to changes in the transport properties of membranes are discussed. The results indicate significant prospects for the use of chitosan and sulfoethylcellulose for the formation of highly selective pervaporation membranes.

  5. Synthesis, crystal structures, and luminescent properties of two series' of new lanthanide (III) amino-carboxylate-phosphonates.

    Science.gov (United States)

    Zhou, Tian-Hua; Yi, Fei-Yan; Li, Pei-Xin; Mao, Jiang-Gao

    2010-02-01

    Hydrothermal reactions of lanthanide(III) chlorides with 4-HOOC-C(6)H(4)-CH(2)NHCH(2)PO(3)H(2) (H(3)L) at different ligand-to-metal (L/M) ratios afforded nine new lanthanide(III) carboxylate-phosphonates with two types of 3D network structures, namely, LnCl(HL)(H(2)O)(2) (Ln = Sm, 1; Eu, 2; Gd, 3; Tb, 4; Dy, 5; Er, 6) and [Ln(2)(HL)(H(2)L)(L)(H(2)O)(2)].4H(2)O (Ln = Nd, 7; Sm, 8; Eu, 9). Compounds 1-6 are isostructural and feature a 3D network in which the LnO(7)Cl polyhedra are interconnected by bridging CPO(3) tetrahedra into 2D inorganic layers parallel to the bc plane. These layers are further cross-linked by organic groups of the carboxylate-phosphonate ligands via the coordination of the carboxylate groups into a pillared-layered architecture. Compounds 7-9 are also isostructural and feature a 3D open-framework composed of 1D lanthanide(III) phosphonate inorganic slabs which are further bridged by organic groups of the carboxylate-phosphonate liagnds via the coordination of the carboxylate groups, forming large 1D tunnels along the b-axis which are filled by lattice water molecules. Luminescent measurements indicate that compounds 2, 4, and 5 show strong emission bands in red, green, and yellow light region, respectively. Magnetic properties of 2, 3, 5, and 7 have also been studied.

  6. Gelatin/chitosan biofilm: preparation and characterization

    International Nuclear Information System (INIS)

    Trindade, Luciane da C.; Nunes, Raquel A.; Diniz, Nadie K.S.; Braga, Carla R.C.; Silva, Suedina M. de Lima

    2011-01-01

    In this study, gelatin, chitosan and gelatin/chitosan bio films using the ratio of gelatin/chitosan (50/50) were prepared by casting method. The bio films prepared were characterized by X-ray diffraction, scanning electron microscopy and dissolution ratio. According to the results, the incorporation of chitosan into gelatin indicate the decrease of crystallinity of chitosan, a compact structure without large pores and that the dissolution of gelatin/chitosan film is little influenced by hot water than gelatin films. (author)

  7. Fabrication of chitosan microparticles loaded in chitosan and poly

    Indian Academy of Sciences (India)

    In recent decades, the use of microparticle-mediated drug delivery is widely applied in the field of biomedicalapplication. Here, we report the new dressing material with ciprofloxacin-loaded chitosan microparticle (CMP) impregnatedin chitosan (CH) and poly(vinyl alcohol) (PVA) scaffold for effective delivery of drug in a ...

  8. Non-isothermal kinetics of thermal degradation of chitosan

    Directory of Open Access Journals (Sweden)

    Georgieva Velyana

    2012-08-01

    Full Text Available Abstract Background Chitosan is the second most abundant nitrogen containing biopolymer in nature, obtained from the shells of crustaceans, particularly crabs, shrimp and lobsters, which are waste products of seafood processing industries. It has great potential application in the areas of biotechnology, biomedicine, food industries, and cosmetics. Chitosan is also capable of adsorbing a number of metal ions as its amino groups can serve as chelation sites. Grafted functional groups such as hydroxyl, carboxyl, sulfate, phosphate, and amino groups on the chitosan have been reported to be responsible for metal binding and sorption of dyes and pigments. The knowledge of their thermal stability and pyrolysis may help to better understand and plan their industrial processing. Results Thermogravimetric studies of chitosan in air atmosphere were carried out at six rates of linear increasing of the temperature. The kinetics and mechanism of the thermal decomposition reaction were evaluated from the TG data using recommended from ICTAC kinetics committee iso-conversional calculation procedure of Kissinger-Akahira-Sunose, as well as 27 mechanism functions. The comparison of the obtained results showed that they strongly depend on the selection of proper mechanism function for the process. Therefore, it is very important to determine the most probable mechanism function. In this respect the iso-conversional calculation procedure turned out to be the most appropriate. Conclusion Chitosan have excellent properties such as hydrophilicity, biocompatibility, biodegradability, antibacterial, non-toxicity, adsorption application. The thermal degradation of chitosan occurs in two stages. The most probable mechanism function for both stages is determined and it was best described by kinetic equations of n-th order (Fn mechanism. For the first stage, it was established that n is equal to 3.0 and for the second stage – to 1.0 respectively. The values of the

  9. Covalent modification of calcium hydroxyapatite surface by grafting phenyl phosphonate moieties

    International Nuclear Information System (INIS)

    Aissa, Abdallah; Debbabi, Mongi; Gruselle, Michel; Thouvenot, Rene; Gredin, Patrick; Traksmaa, Rainer; Tonsuaadu, Kaia

    2007-01-01

    The reaction between phenyl phosphonic dichloride (C 6 H 5 P(O)Cl 2 ) and synthetic calcium hydroxy- and fluorapatite has been investigated. The presence of mono- or polymeric (C 6 H 5 PO) fragment bound to hydroxyapatite was evidenced by IR, and solid-state 31 P NMR spectroscopy. X-ray powder analysis has shown that the apatitic structure remains unchanged during the reaction. In contrast, no reaction was found using fluorapatite. According to the results found for these two different apatites a mechanism was proposed for the formation of covalent P-O-P bonds as the result of a reaction between the C 6 H 5 P(O)Cl 2 organic reagent and (HPO 4 ) - and/or OH - ions of the hydroxyapatite. - Graphical abstract: Representation of the first step of the reaction between the phenyl phosphonic dichloride and the hydroxyl groups on the surface of the apatite, leading to covalent P-O-P bond with elimination of HCl

  10. Use of new phosphonylating and coupling agents in the synthesis of oligodeoxyribonucleotides via the H-phosphonate approach.

    OpenAIRE

    Sakatsume, O; Yamane, H; Takaku, H; Yamamoto, N

    1990-01-01

    New phosphonylating and coupling agents for the synthesis of oligodeoxyribonucleotides via H-phosphonate approach have been developed. Tris(1,1,1,3,3,3-hexafluoro-2-propyl) phosphite, prepared by the reaction of lithium salt of 1,1,1,3,3,3-hexafluoro-2-propoxide with PCl3, reacts with deoxyribonucleosides in the presence of a catalytic amount of triethylamine to produce in the high yield the corresponding deoxyribonucleoside 3'-H-phosphonate units. The use of a new coupling reagent, 1,3-dimet...

  11. Proton conducting graft copolymers with tunable length and density of phosphonated side chains for fuel cell membranes

    DEFF Research Database (Denmark)

    Dimitrov, Ivaylo; Takamuku, Shogo; Jankova Atanasova, Katja

    2014-01-01

    Polysulfones functionalized with highly phosphonated poly(pentafluorostyrene) side chains of different lengths were synthesized applying controlled polymerization and modification methods. The graft copolymers' thermal properties were evaluated by differential scanning calorimetry and thermal...... gravimetrical analyses. The proton conductivity of membrane prepared from the graft copolymer with the shortest phosphonated side chains was 134 mS cm(-1) at 100 degrees C under fully immersed conditions. The graft copolymer TEM image shows a nanophase separation of ion-rich segments within the polysulfone...

  12. Characterization and obtainment of thin films based on N,N,N-trimethyl chitosan and heparin through the technical layer-by-layer

    International Nuclear Information System (INIS)

    Martins, Alessandro F.; Follmann, Heveline D.M.; Rubira, Adley F.; Muniz, Edvani C.

    2011-01-01

    Thin films of Heparin (HP) and N,N,N-trimethyl chitosan (TMC) with a high degree of quaternization (DQ) were obtained at pH 7.4 through the layer-by-layer (LbL) technique. Polystyrene (PS) was oxidized with aqueous solution of sodium persulfate and subsequently employed as substrate. The characterization of TMC and the respective determination of DQ were performed through 1 H NMR spectroscopy. The thin films de TMC/HP were characterized by FTIR-ATR and AFM. Both techniques confirmed the adsorption of TMC and HP in surface of the PS. The increasing of the bilayers provides a decrease of the projections and/or roughness, further of minimizing the depressions at the surface of the films. Studies of thin films the base of TMC/HP prepared from the LbL technique has not been reported in the literature. It is expected that the thin films of TMC/HP present anti-adhesive and antimicrobial properties. (author)

  13. Encapsulation of testosterone by chitosan nanoparticles.

    Science.gov (United States)

    Chanphai, P; Tajmir-Riahi, H A

    2017-05-01

    The loading of testosterone by chitosan nanoparticles was investigated, using multiple spectroscopic methods, thermodynamic analysis, TEM images and modeling. Thermodynamic parameters showed testosterone-chitosan bindings occur mainly via H-bonding and van der Waals contacts. As polymer size increased more stable steroid-chitosan conjugates formed and hydrophobic contact was also observed. The loading efficacy of testosterone-nanocarrier was 40-55% and increased as chitosan size increased. Testosterone encapsulation markedly alters chitosan morphology. Chitosan nanoparticles are capable of transporting testosterone in vitro. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Antimicrobial activity of chitosan coatings and films against Listeria monocytogenes on black radish.

    Science.gov (United States)

    Jovanović, Gordana D; Klaus, Anita S; Nikšić, Miomir P

    2016-01-01

    The antibacterial activity of chitosan coatings prepared with acetic or lactic acid, as well as of composite chitosan-gelatin films prepared with essential oils, was evaluated in fresh shredded black radish samples inoculated with Listeria monocytogenes ATCC 19115 and L. monocytogenes ATCC 19112 during seven days of storage at 4°C. The chitosan coating prepared with acetic acid showed the most effective antibacterial activity. All tested formulations of chitosan films exhibited strong antimicrobial activity on the growth of L. monocytogenes on black radish, although a higher inhibition of pathogens was achieved at higher concentrations of chitosan. The antimicrobial effect of chitosan films was even more pronounced with the addition of essential oils. Chitosan-gelatin films with thyme essential oils showed the most effective antimicrobial activity. A reduction of 2.4log10CFU/g for L. monocytogenes ATCC 19115 and 2.1log10CFU/g for L. monocytogenes ATCC 19112 was achieved in the presence of 1% chitosan film containing 0.2% of thyme essential oil after 24h of storage. Copyright © 2016 Asociación Argentina de Microbiología. Publicado por Elsevier España, S.L.U. All rights reserved.

  15. Synthesis of a novel amphiphilic quaternized chitosan and its distribution in rats.

    Science.gov (United States)

    Liu, Xiaofei; Zeng, Anrong; Li, Lin; Yang, Fan; Wang, Qi; Sun, Zhong; Shen, Jun

    2011-01-01

    A novel amphiphilic chitosan derivative, N-[(2-hydroxy-3-N,N-dimethylhexadecyl ammonium)propyl]chitosan chloride (N-CQCs), was prepared with a degree of substitution (DS) of 15.58%. N-CQCs was positively charged and its zeta potential was +28.4 mV. The introduction of a long carbon chain with a quaternary ammonium salt group into the chitosan backbone enabled N-CQCs to be lipotropic and hydrophilic. According to the hypothesis of the hypocholesterolemic effect of N-CQCs, its organ distribution in rats was investigated 48 h after administration via gavage using fluorescein isothiocyanate labeling. N-CQCs showed lower cytotoxicity. The plasma half-life of N-CQCs in rats was 48 h and the plasma AUC0-48 h (P) was 371.70 μg/ml per h, suggesting that N-CQCs remained in body for a long time. The results also showed that the accumulation in adipose tissue and gastrointestinal tract was higher than in thymus, kidney, liver and spleen at 48 h after administration. It could be presumed that N-CQCs play an important part in the metabolic process of body fat. Adipose tissue and gastrointestinal tract were the probable interaction sites of N-CQCs and body fat.

  16. A versatile characterization of poly(N-isopropylacrylamide-co-N,N'-methylene-bis-acrylamide hydrogels for composition, mechanical strength, and rheology

    Directory of Open Access Journals (Sweden)

    J. Kovacs

    2013-01-01

    Full Text Available Poly(N-isopropylacrylamide-co-N,N'-methylene-bisacrylamide (P(NIPAAm-co-MBA hydrogels were prepared in water using redox initiator. The copolymer composition at high conversion (> 95% was determined indirectly by HPLC (high performance liquid chromatography analysis of the leaching water and directly by solid state 13C CP MAS NMR (cross polarization magic angle spinning nuclear magnetic resonance spectroscopy of the dried gels, and was found to be close to that of the feed. The effect of cross-linker (MBA content in the copolymer was investigated in the concentration range of 1.1–9.1 mol% (R:90–10; R = mol NIPAAm/mol MBA on the rheological behaviour and mechanical strength of the hydrogels. Both storage and loss modulus decreased with decreasing cross-linker content as revealed by dynamic rheometry. Gels R70 and R90 with very low cross-linker content (1.2–1.5 mol% MBA have a very loose network structure, which is significantly different from those with higher cross-linker content manifesting in higher difference in storage modulus. The temperature dependence of the damping factor served the most accurate determination of the volume phase transition temperature, which was not affected by the cross-link density in the investigated range of MBA concentration. Gel R10 with highest cross-linker content (9.1 mol% MBA behaves anomalously due to heterogeneity and the hindered conformation of the side chains of PNIPAAm.

  17. Functionalized and graft copolymers of chitosan and its pharmaceutical applications.

    Science.gov (United States)

    Bhavsar, Chintan; Momin, Munira; Gharat, Sankalp; Omri, Abdelwahab

    2017-10-01

    Chitosan is the second most abundant natural polysaccharide. It belongs a family of polycationic polymers comprised of repetitive units of glucosamine and N-acetylglucosamine. Its biodegradability, nontoxicity, non-immunogenicity and biocompatibility along with properties like mucoadhesion, fungistatic and bacteriogenic have made chitosan an appreciated polymer with numerous applications in the pharmaceutical, comestics and food industry. However, the limited solubility of chitosan at alkaline and neutral pH limits its widespread commercial use. This can be circumvented by fabrication of chitosan by graft copolymerization with acyl, alkyl, monomeric and polymeric moieties. Areas covered: Modifications like quarterization, thiolation, acylation and grafting result in copolymers with higher mucoadhesion strength, increased hydrophobic interactions (advantageous in hydrophobic drug entrapment), and increased solubility in alkaline pH, the ability for adsorption of metal ions, protein and peptide delivery and nutrient delivery. Insights on methods of polymerization, including atomic transfer radical polymerization and click chemistry are discussed. Applications of such modified chitosan copolymers in medical and surgical, and drug delivery, including nasal, oral and buccal delivery have also been covered. Expert opinion: Despite a number of successful investigations, commercialization of chitosan copolymers still remains a challenge. Further advancements in polymerization techniques may address the unmet needs of the healthcare industry.

  18. Chitosan-Coated Magnetic Nanoparticles with Low Chitosan Content Prepared in One-Step

    Directory of Open Access Journals (Sweden)

    Yolanda Osuna

    2012-01-01

    Full Text Available Chitosan-coated magnetic nanoparticles (CMNP were obtained at 50°C in a one-step method comprising coprecipitation in the presence of low chitosan content. CMNP showed high magnetization and superparamagnetism. They were composed of a core of 9.5 nm in average diameter and a very thin chitosan layer in accordance with electron microscopy measurements. The results from Fourier transform infrared spectrometry demonstrated that CMNP were obtained and those from thermogravimetric analysis allowed to determine that they were composed of 95 wt% of magnetic nanoparticles and 5 wt% of chitosan. 67% efficacy in the Pb+2 removal test indicated that only 60% of amino groups on CMNP surface bound to Pb, probably due to some degree of nanoparticle flocculation during the redispersion. The very low weight ratio chitosan to magnetic nanoparticles obtained in this study, 0.053, and the high yield of the precipitation reactions (≈97% are noticeable.

  19. Structure and properties of microcrystalline chitosan

    International Nuclear Information System (INIS)

    Pighinelli, Luciano; Guimaraes, Fernando Machado; Paz, Luan Rios; Zanin, Gabrielle Brehm; Kmiec, Marzena; Tedesco, Felipe Melleu; Reis, Victoria Oliva dos; Silva, Matheus Machado; Becker, Cristiane Miotto; Zehetmeyer, Gislene; Rasia, Gisele

    2016-01-01

    Full text: The microcrystalline chitosan is a modified form of chitosan; it has been elaborated from obtaining method of chitosan salts. It is characterized by special properties of the initial chitosan such as biocompatibility, bioactivity, non-toxic, biodegradability [1]. The objective of this study is to develop a different method to obtain the microcrystalline chitosan and the following characterization of the initial chitosan and MCCh. The material was characterized by FTIR, scanning of electron microscopy, SEM, nuclear magnetic resonance, NMR, and x-ray diffraction. The results indicate that the process to obtain MCCh, did not change the structure of the initial chitosan. The MCCh shows the same functional groups of the initial chitosan. The NMR results shows the acetylated and deacetylated groups. The morphology shows a homogeneous structure of surface. The X-ray diffraction shows the reduction of the crystallinity in the MCCh, indicating a bigger amorphous structure of the MCCh. The chitosan and its derivatives are polymers with excellent properties to be used in regenerative medicine because of ensure efficiency in healing process. This polysaccharide has a great potential to develop a new generation of biomaterials that can be used in regenerative medicine and tissue engineering [2]. References: [1]. LI, Q. et al. Applications and properties of chitosan. In: GOOSEN, M. F. A. (Ed.). Applications of chitin and chitosan. Basel: Technomic, 1997. p. 3-29; [2]. Luciano Pighinelli, Magdalena Kucharska, Dariuz Wawro. Preparation of Microcrystalline chitosan: (MCCh0/tricalcium phosphate complex with Hydroxyapatite in sponge and fibre from for hard tissue regeneration. (author)

  20. Structure and properties of microcrystalline chitosan

    Energy Technology Data Exchange (ETDEWEB)

    Pighinelli, Luciano; Guimaraes, Fernando Machado; Paz, Luan Rios; Zanin, Gabrielle Brehm; Kmiec, Marzena; Tedesco, Felipe Melleu; Reis, Victoria Oliva dos; Silva, Matheus Machado, E-mail: lpighinelli@hotmail.com [Universidade Luterana, Sao Paulo, SP (Brazil); Becker, Cristiane Miotto; Zehetmeyer, Gislene; Rasia, Gisele [Centro Universitario SENAI CIMATEC, Salvador, BA (Brazil). Instituto de Engenharia de Materiais Polimericos

    2016-07-01

    Full text: The microcrystalline chitosan is a modified form of chitosan; it has been elaborated from obtaining method of chitosan salts. It is characterized by special properties of the initial chitosan such as biocompatibility, bioactivity, non-toxic, biodegradability [1]. The objective of this study is to develop a different method to obtain the microcrystalline chitosan and the following characterization of the initial chitosan and MCCh. The material was characterized by FTIR, scanning of electron microscopy, SEM, nuclear magnetic resonance, NMR, and x-ray diffraction. The results indicate that the process to obtain MCCh, did not change the structure of the initial chitosan. The MCCh shows the same functional groups of the initial chitosan. The NMR results shows the acetylated and deacetylated groups. The morphology shows a homogeneous structure of surface. The X-ray diffraction shows the reduction of the crystallinity in the MCCh, indicating a bigger amorphous structure of the MCCh. The chitosan and its derivatives are polymers with excellent properties to be used in regenerative medicine because of ensure efficiency in healing process. This polysaccharide has a great potential to develop a new generation of biomaterials that can be used in regenerative medicine and tissue engineering [2]. References: [1]. LI, Q. et al. Applications and properties of chitosan. In: GOOSEN, M. F. A. (Ed.). Applications of chitin and chitosan. Basel: Technomic, 1997. p. 3-29; [2]. Luciano Pighinelli, Magdalena Kucharska, Dariuz Wawro. Preparation of Microcrystalline chitosan: (MCCh0/tricalcium phosphate complex with Hydroxyapatite in sponge and fibre from for hard tissue regeneration. (author)

  1. The effect of hydroxylation on CNT to form Chitosan-CNT composites: A DFT study

    International Nuclear Information System (INIS)

    Yu, Rui; Ran, Maofei; Wen, Jie; Sun, Wenjing; Chu, Wei; Jiang, Chengfa; He, Zhiwei

    2015-01-01

    Graphical abstract: - Highlights: • The effect of hydroxylation on CNT to form Chitosan-CNT composites was studied. • The adsorption of Chitosan on CNTs is very weak by electrostatic interactions. • Chitosan loads onto CNT-OH_n via hydrogen-bond interactions. • Chitosan transfers electron to CNT-OH_n and thus improves the reactivity of CNT. - Abstract: The effect of types of CNTs (pristine and hydroxylated) on the synthesis of Chitosan-CNT (CS-CNT) composites was investigated theoretically. The adsorption energy (E_a_d_s) of CS on the pristine CNT and hydroxylated CNTs (CNT-OH_n, n = 1–6) as well as the structural and electronic properties of said composites have been investigated. Results show that the adsorption of CS on CNT and CNT-OH_n is thermodynamically favored. The E_a_d_s of CS on CNTs was calculated to be −20.387 kcal/mol from electrostatic interactions. For CS adsorbed into CNT-OH_n, E_a_d_s ranges from −20.612 to −37.567 kcal/mol. Hydroxyl groups on CNT are the main adsorption sites for CS loading onto CNT-OH_n via hydrogen-bond interactions. The CS-CNT-OH_3 is the most sable composite among tested complexes. The energy gap (ΔE_g_a_p) of CS-CNT-OH_3 was calculated less than pristine CNT and CNT-OH_3, indicative of the composites being more reactive than that of pristine CNTs and CNT-OH_3. It was proved that CS can transfer electron to the hydroxylated CNTs, thus overcoming the drawbacks of CNTs being chemically inert.

  2. The effect of hydroxylation on CNT to form Chitosan-CNT composites: A DFT study

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Rui [China-America Cancer Research Institute, Key Laboratory for Medical Molecular Diagnostics of Guangdong Province, Guangdong Medical University, Dongguan, Guangdong 523808 (China); Department of Chemical Engineering, Sichuan University, Chengdu 610065 (China); Ran, Maofei [College of Chemistry & Environment Protection Engineering, Southwest University for Nationalities, Chengdu 610041, Sichuan (China); Wen, Jie [College of Chemistry and Chemical Engineering, Southwest Petroleum University, Chengdu 610500, Sichuan (China); Sun, Wenjing, E-mail: swj_gdmc@163.com [China-America Cancer Research Institute, Key Laboratory for Medical Molecular Diagnostics of Guangdong Province, Guangdong Medical University, Dongguan, Guangdong 523808 (China); Chu, Wei; Jiang, Chengfa [Department of Chemical Engineering, Sichuan University, Chengdu 610065 (China); He, Zhiwei, E-mail: zhiweihe688@yahoo.com [China-America Cancer Research Institute, Key Laboratory for Medical Molecular Diagnostics of Guangdong Province, Guangdong Medical University, Dongguan, Guangdong 523808 (China)

    2015-12-30

    Graphical abstract: - Highlights: • The effect of hydroxylation on CNT to form Chitosan-CNT composites was studied. • The adsorption of Chitosan on CNTs is very weak by electrostatic interactions. • Chitosan loads onto CNT-OH{sub n} via hydrogen-bond interactions. • Chitosan transfers electron to CNT-OH{sub n} and thus improves the reactivity of CNT. - Abstract: The effect of types of CNTs (pristine and hydroxylated) on the synthesis of Chitosan-CNT (CS-CNT) composites was investigated theoretically. The adsorption energy (E{sub ads}) of CS on the pristine CNT and hydroxylated CNTs (CNT-OH{sub n}, n = 1–6) as well as the structural and electronic properties of said composites have been investigated. Results show that the adsorption of CS on CNT and CNT-OH{sub n} is thermodynamically favored. The E{sub ads} of CS on CNTs was calculated to be −20.387 kcal/mol from electrostatic interactions. For CS adsorbed into CNT-OH{sub n}, E{sub ads} ranges from −20.612 to −37.567 kcal/mol. Hydroxyl groups on CNT are the main adsorption sites for CS loading onto CNT-OH{sub n} via hydrogen-bond interactions. The CS-CNT-OH{sub 3} is the most sable composite among tested complexes. The energy gap (ΔE{sub gap}) of CS-CNT-OH{sub 3} was calculated less than pristine CNT and CNT-OH{sub 3}, indicative of the composites being more reactive than that of pristine CNTs and CNT-OH{sub 3}. It was proved that CS can transfer electron to the hydroxylated CNTs, thus overcoming the drawbacks of CNTs being chemically inert.

  3. Visible light driven photocatalytic degradation of methylene blue using novel camphor sulfonic acid doped polycarbazole/g-C3N4 nanocomposite

    Science.gov (United States)

    Praveena, P.; Dhanavel, S.; Sangamithirai, D.; Narayanan, V.; Stephen, A.

    2018-04-01

    A novel polycabazole(PCz)/graphitic carbon nitride(g-C3N4) nanocomposite was synthesized via chemical oxidative polymerization method. In the present work, camphor sulfonic acid (CSA) was used as a dopantand ammonium peroxydisulphate (APS) was used as an oxidizing agent. The PCz/g-C3N4 nanocompositewas characterizedusing X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and UV-Visible spectroscopy (UV-Vis). The obtained results confirm the successful formation of PCz/g-C3N4 nanocomposite. Visible light induced photocatalytic activity of the novel catalyst was demonstrated using methylene blue as a target pollutant. The results suggestthat PCz/g-C3N4 nanocomposite can be used as an effective catalyst for the degradation of organic pollutants from waste water.

  4. Pseudo-thermosetting chitosan hydrogels for biomedical application.

    Science.gov (United States)

    Berger, J; Reist, M; Chenite, A; Felt-Baeyens, O; Mayer, J M; Gurny, R

    2005-01-06

    To prepare transparent chitosan/beta-glycerophosphate (betaGP) pseudo-thermosetting hydrogels, the deacetylation degree (DD) of chitosan has been modified by reacetylation with acetic anhydride. Two methods (I and II) of reacetylation have been compared and have shown that the use of previously filtered chitosan, dilution of acetic anhydride and reduction of temperature in method II improves efficiency and reproducibility. Chitosans with DD ranging from 35.0 to 83.2% have been prepared according to method II under homogeneous and non-homogeneous reacetylation conditions and the turbidity of chitosan/betaGP hydrogels containing homogeneously or non-homogeneously reacetylated chitosan has been investigated. Turbidity is shown to be modulated by the DD of chitosan and by the homogeneity of the medium during reacetylation, which influences the distribution mode of the chitosan monomers. The preparation of transparent chitosan/betaGP hydrogels requires a homogeneously reacetylated chitosan with a DD between 35 and 50%.

  5. Halloysite and chitosan oligosaccharide nanocomposite for wound healing.

    Science.gov (United States)

    Sandri, Giuseppina; Aguzzi, Carola; Rossi, Silvia; Bonferoni, Maria Cristina; Bruni, Giovanna; Boselli, Cinzia; Cornaglia, Antonia Icaro; Riva, Federica; Viseras, Cesar; Caramella, Carla; Ferrari, Franca

    2017-07-15

    Halloysite is a natural nanotubular clay mineral (HNTs, Halloysite Nano Tubes) chemically identical to kaolinite and, due to its good biocompatibility, is an attractive nanomaterial for a vast range of biological applications. Chitosan oligosaccharides are homo- or heterooligomers of N-acetylglucosamine and D-glucosamine, that accelerate wound healing by enhancing the functions of inflammatory and repairing cells. The aim of the work was the development of a nanocomposite based on HNTs and chitosan oligosaccharides, to be used as pour powder to enhance healing in the treatment of chronic wounds. A 1:0.05 wt ratio HTNs/chitosan oligosaccharide nanocomposite was obtained by simply stirring the HTNs powder in a 1% w/w aqueous chitosan oligosaccharide solution and was formed by spontaneous ionic interaction resulting in 98.6% w/w HTNs and 1.4% w/w chitosan oligosaccharide composition. Advanced electron microscopy techniques were considered to confirm the structure of the hybrid nanotubes. Both HTNs and HTNs/chitosan oligosaccharide nanocomposite showed good in vitro biocompatibility with normal human dermal fibroblasts up to 300μg/ml concentration and enhanced in vitro fibroblast motility, promoting both proliferation and migration. The HTNs/chitosan oligosaccharide nanocomposite and the two components separately were tested for healing capacity in a murine (rat) model. HTNs/chitosan oligosaccharide allowed better skin reepithelization and reorganization than HNTs or chitosan oligosaccharide separately. The results suggest to develop the nanocomposite as a medical device for wound healing. The present work is focused on the development of halloysite and chitosan oligosaccharide nanocomposite for wound healing. It considers a therapeutic option for difficult to heal skin lesions and burns. The significance of the research considers two fundamental aspects: the first one is related to the development of a self-assembled nanocomposite, formed by spontaneous ionic

  6. Oxygen and nitrogen plasma etching of three-dimensional hydroxyapatite/chitosan scaffolds fabricated by additive manufacturing

    Science.gov (United States)

    Myung, Sung-Woon; Kim, Byung-Hoon

    2016-01-01

    Three-dimensional (3D) chitosan and hydroxyapatite (HAp)/chitosan (CH) scaffolds were fabricated by additive manufacturing, then their surfaces were etched with oxygen (O2) and nitrogen (N2) plasma. O2 and N2 plasma etching was performed to increase surface properties such as hydrophilicity, roughness, and surface chemistry on the scaffolds. After etching, hydroxyapatite was exposed on the surface of 3D HAp/CH scaffolds. The surface morphology and chemical properties were characterized by contact angle measurement, scanning electron microscopy, X-ray diffraction, and attenuated total reflection Fourier infrared spectroscopy. The cell viability of 3D chitosan scaffolds was examined by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. The differentiation of preosteoblast cells was evaluated by alkaline phosphatase assay. The cell viability was improved by O2 and N2 plasma etching of 3D chitosan scaffolds. The present fabrication process for 3D scaffolds might be applied to a potential tool for preparing biocompatible scaffolds.

  7. Synthesis and Optimization of Chitosan Nanoparticles of Shrimp shell as Adsorbent of Pb2+ Ions

    Directory of Open Access Journals (Sweden)

    Sulistyani Sulistyani

    2017-11-01

    Full Text Available Synthesis and optimization of chitosan nanoparticles from shrimp shell as an adsorbent of Pb2+ ions has been done. Chitosan is obtained through several stages, namely deproteinase, demineralization and deacetylation. Deproteinase by using 2 N NaOH solution (a ratio of 1:6 w/v while stirring at 90 °C for 1 hour. Demineralization by using 1 N HCl solution (a ratio of 1:12 w/v while stirring at room temperature for 1 hour. Deacetylation by using 50% NaOH solution (a ratio of 1:10 w/v at 120 °C for 3 hours. Chitosan nanoparticles are obtained by adding a solution of 1% CH3COOH and a few drops of NH3 concentrated at 90 °C to form a white gel is then washed to pH neutral and dried. Characterization of chitosan include analysis of degree of deacetylation by using FTIR and analysis of particle size by using Particle Size Analyzer (PSA. Chitosan nanoparticles was then applied as an adsorbent of lead. Optimization of chitosan as an adsorbent include contact time and pH. Concentration of lead is determined using Atomic Absorption Spectroscopy (AAS. The results showed chitosan synthesis product has a size of ~600 nm, so that it can be expressed as nanoparticles with a degree of deacetylation of 62.69%. Chitosan nanoparticles as adsorbent optimum at pH 3 and a contact time of 2 hours with an adsorption capacity of 13,25 mg/g .

  8. Novel sulfonated poly (ether ether ketone)/phosphonic acid-functionalized titania nanohybrid membrane by an in situ method for direct methanol fuel cells

    Science.gov (United States)

    Wu, Hong; Cao, Ying; Li, Zhen; He, Guangwei; Jiang, Zhongyi

    2015-01-01

    Sulfonated poly (ether ether ketone)/phosphonic acid-functionalized titania nanohybrid membranes are prepared by an in situ method using titanium tetrachloride (TiCl4) as inorganic precursor and amino trimethylene phosphonic acid (ATMP) as modifier. Phosphonic acid-functionalized titania nanoparticles with a uniform particle size of ∼50 nm are formed and dispersed homogeneously in the SPEEK matrix with good interfacial compatibility. Accordingly, the nanohybrid membranes display remarkably enhanced proton conduction property due to the incorporation of additional sites for proton transport and the formation of well-connected channels by bridging the hydrophilic domains in SPEEK matrix. The nanohybrid membrane with 6 wt. % of phosphonic acid-functionalized titania nanoparticles exhibits the highest proton conductivity of 0.334 S cm-1 at 65 °C and 100% RH, which is 63.7% higher than that of pristine SPEEK membrane. Furthermore, the as-prepared nanohybrid membranes also show elevated thermal and mechanical stabilities as well as decreased methanol permeability.

  9. Effects of Paclitaxel-conjugated N-Succinyl-Hydroxyethyl Chitosan Film for Proliferative Cholangitis in Rabbit Biliary Stricture Model.

    Science.gov (United States)

    Wang, Tao; Zou, Hao; Liu, Yun-Xia; Zhang, Xiao-Wen

    2018-03-20

    Paclitaxel (PTX) could inhibit the growth of fibroblasts, which occurs in proliferative cholangitis and leads to biliary stricture. However, its use has been limited due to poor bioavailability and local administration for short time. This study designed and synthesized a new PTX-conjugated chitosan film (N-succinyl-hydroxyethyl chitosan containing PTX [PTX-SHEC]) and evaluated its safety and efficiency using in vivo and in vitro experiments. The SHEC conjugated with PTX was confirmed by nuclear magnetic resonance (NMR) and Fourier-transform infrared spectroscopy (FT-IR) measurements. Drug releases in vitro and in vivo were determined using high-performance liquid chromatography. Cell viability in vitro was measured using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide. Rabbit biliary stricture model was constructed. All rabbits randomly divided into five groups (n = 8 in each group): the sham-operated rabbits were used as control (Group A), Groups B received laparotomies and suture, Group C received laparotomies and covered SHEC suture without the PTX coating, Group D received laparotomies and covered PTX-SHEC suture, and Group E received laparotomies and 1000 μmol/L PTX administration. Liver function tests and residual dosage of PTX from each group were measured by enzyme-linked immunosorbent assay. Histological data and α-smooth muscle actin (SMA) immunohistochemical staining of common bile duct were examined. NMR and FT-IR indicated that PTX was successfully introduced, based on the appearance of signals at 7.41-7.99 ppm, 1.50 ppm, and 1.03 ppm, due to the presence of aromatic protons, methylene protons, and methyl protons of PTX, respectively. No bile leak was observed. The PTX-conjugated film could slowly release PTX for 4 weeks (8.89 ± 0.03 μg at day 30). The in vitro cell viability test revealed significantly different levels of toxicity between films with and without PTX (111.7 ± 4.0% vs. 68.1 ± 6.0%, P films (67.7 ± 5.4%, 67.2 ± 3

  10. The effect of chitosan and whey proteins-chitosan films on the growth of Penicillium expansum in apples.

    Science.gov (United States)

    Simonaitiene, Dovile; Brink, Ieva; Sipailiene, Ausra; Leskauskaite, Daiva

    2015-05-01

    Penicillium expansum causes a major post-harvest disease of apples. The aim of this study was to investigate the inhibition effect of chitosan and whey proteins-chitosan films containing different amounts of quince and cranberry juice against P. expansum on the simulation medium and on apples. The mechanical properties of films were also evaluated. The presence of cranberry and quince juice in the composition of chitosan and whey proteins-chitosan films caused a significant (P ≤ 0.05) increase in elasticity and decrease in tensile strength of films. Chitosan and whey proteins-chitosan films with quince and cranberry juice demonstrated a significant (P ≤ 0.05) inhibition effect against P. expansum growth on the simulated medium and apples. The presence of cranberry juice in the composition of chitosan and whey proteins-chitosan films resulted in a longer lag phase and a lower P. expansum growth rate on the simulation medium in comparison with films made with the addition of quince juice. These differences were not evident when experiment was conducted with apples. Addition of quince and cranberry juice to the chitosan and whey proteins-chitosan films as natural antifungal agents has some potential for prolonging the shelf life of apples. © 2014 Society of Chemical Industry.

  11. A functionalized phosphonate-rich organosilica layered hybrid material (PSLM) fabricated through a mild process for heavy metal uptake

    Energy Technology Data Exchange (ETDEWEB)

    Daikopoulos, Chris [Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110 (Greece); Bourlinos, Athanasios B. [Institute of Materials Science, NCSR “Demokritos”, Ag. Paraskevi Attikis, Athens 15310 (Greece); Georgiou, Yiannis [Laboratory of Physical Chemistry, Department of Environmental and Natural Resources Management, University of Patras, Seferi 2, Agrinio 30100 (Greece); Deligiannakis, Yiannis, E-mail: ideligia@cc.uoi.gr [Laboratory of Physical Chemistry, Department of Environmental and Natural Resources Management, University of Patras, Seferi 2, Agrinio 30100 (Greece); Zboril, Radek [Regional Centre of Advanced Technologies and Materials, Faculty of Science, Department of Physical Chemistry and Experimental Physics, Palacky University, Olomouc 77146 (Czech Republic); Karakassides, Michael A. [Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110 (Greece)

    2014-04-01

    Highlights: • Novel phosphonate-rich organosilica layered hybrid material (PSLM) fabricated through a mild xerogel process. • Surface Complexation Modeling reveals that PSLM bears 2 types of functional groups able to bind heavy metal. • Maximum metal uptake capacities were found 2.72 mmol g{sup −1} for Cu{sup 2+}, 1.67 mmol g{sup −1} for Pb{sup 2+} and 1.00 mmol g{sup −1} for Cd{sup 2+} at pH 7. • EPR spectroscopy reveals local coordination environment for Cu{sup 2+} ions. - Abstract: A phosphonate-rich organosilica layered hybrid material (PSLM) made of 3-(trihydroxysilyl)propyl methylphosphonate, monosodium salt, as the single silica source, has been obtained from its aqueous solution through a xerogel process and mild thermal aging. The method is simple, affording bulk quantities of powdered PSLM in a single-step. The hybrid is stable in water and possesses a high content of phosphonate groups fixed on the solid matrix. In addition, PSLM shows good thermal stability, which exceeds 300 °C in air. The material was characterized using SEM, TEM, XRD, FT-IR and TGA techniques. Potentiometric titrations show that PSLM bears high-surface density of phosphonate groups (3 mmol g{sup −1}). As a result, the material displays high metal uptake capacity for heavy metal ions such as Cu{sup 2+} (2.72 mmol g{sup −1}), Pb{sup 2+} (1.67 mmol g{sup −1}) and Cd{sup 2+} (1.00 mmol g{sup −1}) at neutral pH values e.g. the pH of natural waters. Detailed theoretical modeling using a Surface Complexation Model combined with Electron Paramagnetic Resonance (EPR) spectroscopy shows that the surface distribution of surface bound Cu{sup 2+} ions is rather homogeneous e.g. copper-binding phosphonate sites are arranged in average distances 5–8 Å.

  12. Development and Evaluation of Diclofenac Sodium Loaded-N-Trimethyl Chitosan Nanoparticles for Ophthalmic Use.

    Science.gov (United States)

    Asasutjarit, Rathapon; Theerachayanan, Thitaree; Kewsuwan, Prartana; Veeranodha, Sukitaya; Fuongfuchat, Asira; Ritthidej, Garnpimol C

    2015-10-01

    The ophthalmic preparation of diclofenac sodium (DC) for relieving ocular inflammation is presently available in the market only as an eye drop solution. Due to its low occular bioavailability, it requires frequent application leading to low patients' compliance and quality of life. This study was conducted to develop formulations of DC loaded-N-trimethyl chitosan nanoparticles (DC-TMCNs) for ophthalmic use to improve ocular biavailabiltiy of DC. DC-TMCNs varied in formulation compositions were prepared using ionic gelation technique and evaluated for their physicochemical properties, drug release, eye irritation potential, and ophthalmic absorption of diclofenac sodium. N-Trimethyl chitosan (TMC) with a 49.8% degree of quaternization was synthesized and used for DC-TMCNs production. The obtained DC-TMCNs had particle size in a range of 130-190 nm with zeta potential values of +4 to +9 mV and drug entrapment efficiencies of more than 70% depending on the content of TMC and sodium tripolyphosphate (TPP). The optimized DC-TMCNs formulation contained TMC, DC, and TPP at a weight ratio of TMC/DC/TPP = 3:1:1. Their lyophilized product reconstituted with phosphate buffer solution pH 5.5 possessed a drug release pattern that fitted within the zero-order model. The eye irritation tests showed that DC-TMCNs were safe for ophthalmic use. The in vivo ophthalmic drug absorption study performed on rabbits indicated that DC-TMCNs could improve ophthalmic bioavailability of DC. Results of this study suggested that DC-TMCNs had potential for use as an alternative to conventional DC eye drops for ophthalmic inflammation treatment.

  13. Polysulfone Functionalized With Phosphonated Poly(pentafluorostyrene) Grafts for Potential Fuel Cell Applications

    DEFF Research Database (Denmark)

    Dimitrov, Ivaylo; Takamuku, Shogo; Jankova Atanasova, Katja

    2012-01-01

    A multi‐step synthetic strategy to polysulfone (PSU) grafted with phosphonated poly(pentafluorostyrene) (PFS) is developed. It involves controlled radical polymerization resulting in alkyne‐end functional PFS. The next step is the modification of PSU with a number of azide side groups. The grafting...

  14. Application of chitosan and its N-heterocyclic derivatives for preconcentration of noble metal ions and their determination using atomic absorption spectrometry.

    Science.gov (United States)

    Azarova, Yu A; Pestov, A V; Ustinov, A Yu; Bratskaya, S Yu

    2015-12-10

    Chitosan and its N-heterocyclic derivatives N-2-(2-pyridyl)ethylchitosan (2-PEC), N-2-(4-pyridyl) ethylchitosan (4-PEC), and N-(5-methyl-4-imidazolyl) methylchitosan (IMC) have been applied in group preconcentration of gold, platinum, and palladium for subsequent determination by atomic absorption spectroscopy (AAS) in solutions with high background concentrations of iron and sodium ions. It has been shown that the sorption mechanism, which was elucidated by XPS, significantly influences the sorption capacity of materials, the efficiency of metal ions elution after preconcentration, and, as a result, the accuracy of metal determination by AAS. We have shown that native chitosan was not suitable for preconcentration of Au(III), if the elution step was used as a part of the analysis scheme. The group preconcentration of Au(III), Pd(II), and Pt(IV) with subsequent quantitative elution using 0.1M HCl/1M thiourea solution was possible only on IMC and 4-PEC. Application of IMC for analysis of the national standard quartz ore sample proved that gold could be accurately determined after preconcentration/elution with the recovery above 80%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Preparation and characterization of chitosan/genipin/poly(N-vinyl-2-pyrrolidone) films for controlled release drugs

    Energy Technology Data Exchange (ETDEWEB)

    Aldana, Ana Agustina, E-mail: aaldana@fcq.unc.edu.ar [Departamento de Quimica Organica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba (UNC), Edificio de Ciencias II, Medina Allende y Haya de la Torre, Ciudad Universitaria, Cordoba 5000 (Argentina); Gonzalez, Agustin, E-mail: agustingonzalez@fcq.unc.edu.ar [Departamento de Quimica Organica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba (UNC), Edificio de Ciencias II, Medina Allende y Haya de la Torre, Ciudad Universitaria, Cordoba 5000 (Argentina); Strumia, Miriam C., E-mail: mcs@fcq.unc.edu.ar [Departamento de Quimica Organica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba (UNC), Edificio de Ciencias II, Medina Allende y Haya de la Torre, Ciudad Universitaria, Cordoba 5000 (Argentina); Martinelli, Marisa, E-mail: mmartinelli@fcq.unc.edu.ar [Departamento de Quimica Organica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba (UNC), Edificio de Ciencias II, Medina Allende y Haya de la Torre, Ciudad Universitaria, Cordoba 5000 (Argentina)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Cross-linked chitosan films using genipin and/or PVP. Black-Right-Pointing-Pointer Propranolol hydrochloride was used like a model drug to release studies. Black-Right-Pointing-Pointer Incorporating PVP improves mechanical and diffusion properties. Black-Right-Pointing-Pointer Ch-Gen 0.10% and Ch-Gen 0.10%-PVP have optimal behavior. - Abstract: The study of the physicochemical and functional properties of chitosan films cross-linked with genipin and poly(N-vinyl-2-pyrrolidone) (PVP) was performed in this work. Cross-linked films were prepared by casting method from acetic acid solutions. The structure and physical properties of the films were analyzed by infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy ({sup 13}C NMR), differential scanning calorimetry (DSC) and mechanical testings. Propranolol hydrochloride was used like a model drug to determine the behavior of drug release from films. The drug release capacity was measured and compared with the degree of cross-linking, mechanical properties and swelling index. There was an appropriate balance of hydrophilicity, mechanical properties and diffusion by the incorporation of PVP into the networks cross-linked with genipin. The combination of both cross-linkers allows obtaining a soft and tough material potentially applicable as a controlled release. This research represents the first report where both cross-linkers, chemical and ionic agents, are used for obtaining films. These studies suggest that the chitosan films prepared here are promising drug delivery systems for buccal application, with thermal stability and acceptable mechanical properties. Buccal films may be preferred in terms of flexibility and comfort.

  16. Preparation and characterization of chitosan/genipin/poly(N-vinyl-2-pyrrolidone) films for controlled release drugs

    International Nuclear Information System (INIS)

    Aldana, Ana Agustina; González, Agustín; Strumia, Miriam C.; Martinelli, Marisa

    2012-01-01

    Highlights: ► Cross-linked chitosan films using genipin and/or PVP. ► Propranolol hydrochloride was used like a model drug to release studies. ► Incorporating PVP improves mechanical and diffusion properties. ► Ch–Gen 0.10% and Ch–Gen 0.10%–PVP have optimal behavior. - Abstract: The study of the physicochemical and functional properties of chitosan films cross-linked with genipin and poly(N-vinyl-2-pyrrolidone) (PVP) was performed in this work. Cross-linked films were prepared by casting method from acetic acid solutions. The structure and physical properties of the films were analyzed by infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy ( 13 C NMR), differential scanning calorimetry (DSC) and mechanical testings. Propranolol hydrochloride was used like a model drug to determine the behavior of drug release from films. The drug release capacity was measured and compared with the degree of cross-linking, mechanical properties and swelling index. There was an appropriate balance of hydrophilicity, mechanical properties and diffusion by the incorporation of PVP into the networks cross-linked with genipin. The combination of both cross-linkers allows obtaining a soft and tough material potentially applicable as a controlled release. This research represents the first report where both cross-linkers, chemical and ionic agents, are used for obtaining films. These studies suggest that the chitosan films prepared here are promising drug delivery systems for buccal application, with thermal stability and acceptable mechanical properties. Buccal films may be preferred in terms of flexibility and comfort.

  17. Development and evaluation of N-naphthyl-N,O-succinyl chitosan micelles containing clotrimazole for oral candidiasis treatment.

    Science.gov (United States)

    Tonglairoum, Prasopchai; Woraphatphadung, Thisirak; Ngawhirunpat, Tanasait; Rojanarata, Theerasak; Akkaramongkolporn, Prasert; Sajomsang, Warayuth; Opanasopit, Praneet

    2017-03-01

    Clotrimazole (CZ)-loaded N-naphthyl-N,O-succinyl chitosan (NSCS) micelles have been developed as an alternative for oral candidiasis treatment. NSCS was synthesized by reductive N-amination and N,O-succinylation. CZ was incorporated into the micelles using various methods, including the dropping method, the dialysis method, and the O/W emulsion method. The size and morphology of the CZ-loaded micelles were characterized using dynamic light scattering measurements (DLS) and a transmission electron microscope (TEM), respectively. The drug entrapment efficiency, loading capacity, release characteristics, and antifungal activity against Candida albicans were also evaluated. The CZ-loaded micelles prepared using different methods differed in the size of micelles. The micelles ranged in size from 120 nm to 173 nm. The micelles prepared via the O/W emulsion method offered the highest percentage entrapment efficiency and loading capacity. The CZ released from the CZ-loaded micelles at much faster rate compared to CZ powder. The CZ-loaded NSCS micelles can significantly hinder the growth of Candida cells after contact. These CZ-loaded NSCS micelles offer great antifungal activity and might be further developed to be a promising candidate for oral candidiasis treatment.

  18. A sulfuric-lactic acid process for efficient purification of fungal chitosan with intact molecular weight.

    Science.gov (United States)

    Naghdi, Mitra; Zamani, Akram; Karimi, Keikhosro

    2014-02-01

    The most recent method of fungal chitosan purification, i.e., two steps of dilute sulfuric acid treatment, pretreatment of cell wall at room temperature for phosphate removal and extraction of chitosan from the phosphate free cell wall at high temperature, significantly reduces the chitosan molecular weight. This study was aimed at improvement of this method. In the pretreatment step, to choose the best conditions, cell wall of Rhizopus oryzae, containing 9% phosphate, 10% glucosamine, and 21% N-acetyl glucosamine, was treated with sulfuric, lactic, acetic, nitric, or hydrochloric acid, at room temperature. Sulfuric acid showed the best performance in phosphate removal (90%) and cell wall recovery (89%). To avoid depolymerisation of chitosan, hot sulfuric acid extraction was replaced with lactic acid treatment at room temperature, and a pure fungal chitosan was obtained (0.12 g/g cell wall). Similar pretreatment and extraction processes were conducted on pure shrimp chitosan and resulted in a chitosan recovery of higher than 87% while the reduction of chitosan viscosity was less than 15%. Therefore, the sulfuric-lactic acid method purified the fungal chitosan without significant molecular weight manipulation. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Radiation processing of chitosan derivative and its characteristics

    International Nuclear Information System (INIS)

    Kamarudin Bahari; Kamarolzaman Hussein; Kamaruddin Hashim; Khairul Zaman Mohd Dahlan

    2002-01-01

    Chitosan is natural polymer derived from chitin, a polysaccharide found in the exoskeleton of shrimps, crabs, fungi and others. Chitosan is a naturally occurring substance that is chemically similar to cellulose. Chitosan possesses a positive ionic charge give ability to chemically bond with negatively charged fats. Chitosan is soluble in organic acid but insoluble in water. Carboxymethyl-chitosan (cm-chitosan) is a derivative of chitosan which is water-soluble was then prepared by a carboxymethylation process of chitosan produced from local shrimp shell. A simple method for synthesis of cm-chitosan has been developed at 55 degree C in aqueous sodium hydroxide / propanol with chloroacetic acid (CAA) or sodium chloroacetate salt (SCA). The modification of chitosan to water-soluble chitosan can be used in hydrogel as anti-bacterial agent and it overcome the problem of bad smell using acetic acid. (Author)

  20. Synthesis, characterization and radiation processing of carboxymethyl-chitosan

    International Nuclear Information System (INIS)

    Kamarudin Bahari; Kamarolzaman Hussein; Kamaruddin Hashim; Khairul Zaman Mohd Dahlan

    2002-01-01

    Chitosan is natural polymer derived from chitin, a polysaccharide found in the exoskeleton of shrimps, crabs, fungi and others. Chitosan is a naturally occurring substance that is chemically similar to cellulose. Chitosan possesses a positive ionic charge give ability to chemically bond with negatively charged fats. Chitosan is soluble in organic acid but insoluble in water. Carboxymethyl-chitosan (cm-chitosan) is a derivative of chitosan which is water-soluble was then prepared by carboxymethylation process of chitosan produced from local shrimp shell. A simple method for synthesis of cm-chitosan has been developed at 55 degree C in aqueous sodium hydroxide / propanol with chloroacetic acid (CAA) or sodium chloroacetate salt (SCA). The modification of chitosan to water-soluble chitosan can be used in hydrogel as anti-bacterial and anti-fungal agent, and it overcome the problem of bad smell using organic acid. (Author)

  1. Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

    Energy Technology Data Exchange (ETDEWEB)

    Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

  2. Phosphorus sorption on marine carbonate sediment: phosphonate as model organic compounds.

    Science.gov (United States)

    Huang, Xiao-Lan; Zhang, Jia-Zhong

    2011-11-01

    Organophosphonate, characterized by the presence of a stable, covalent, carbon to phosphorus (C-P) bond, is a group of synthetic or biogenic organophosphorus compounds. The fate of these organic phosphorus compounds in the environment is not well studied. This study presents the first investigation on the sorption of phosphorus (P) in the presence of two model phosphonate compounds, 2-aminothylphosphonoic acid (2-AEP) and phosphonoformic acid (PFA), on marine carbonate sediments. In contrast to other organic P compounds, no significant inorganic phosphate exchange was observed in seawater. P was found to adsorb on the sediment only in the presence of PFA, not 2-AEP. This indicated that sorption of P from phosphonate on marine sediment was compound specific. Compared with inorganic phosphate sorption on the same sediments, P sorption from organic phosphorus is much less in the marine environment. Further study is needed to understand the potential role of the organophosphonate compounds in biogeochemical cycle of phosphorus in the environment. Copyright © 2011 Elsevier Ltd. All rights reserved.

  3. Cu-Catalyzed Asymmetric Allylic Alkylation of Phosphonates and Phosphine Oxides with Grignard Reagents

    NARCIS (Netherlands)

    Hornillos, Valentin; Perez, Manuel; Fananas-Mastral, Martin; Feringa, Ben L.

    An efficient and highly enantioselective copper-catalyzed allylic alkylation of phosphonates and phosphine oxides with Grignard reagents and Taniaphos or phosphoramidites as chiral ligands is reported. Transformation of these products leads to a variety of new phosphorus-containing chiral

  4. Radiation Synthesis and Application of Carboxymethylated Chitosan Hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Noh, Young Chang

    2007-08-15

    This research proposal is to investigate radiation effect of carboxymethylated chitosan in order to obtain the crosslinked carboxymethylated chitosan. The application studies on CM-chitosan- based intelligent hydrogels will be tried too. Chitin is the most abundant natural amino polysaccharide and estimated to be produced annually almost as much as cellulose. Chitosan is the deacetylated product of chitin showing the enhanced solubility in dilute acids, further, carboxymethylated chitosan (CM-chitosan) can solve in both acidic and basic physiological media, which might be good candidates as a kind of biomedical materials. Radiation technique is an important method for modification of chitin derivatives. It includes radiation-induced degradation, grafting, and crosslinking. It was found that CM-chitosan degraded in solid state or dilute aqueous solution under irradiation, but crosslinked at paste-like sate when the concentration of CM-chitosan is more than 10%. Both degraded and crosslinked CM-chitosan have antibacterial activity, so it is essential to investigate in detail the radiation effect of CM-chitosan. Study on radiation effect of CM-chitosan in different condition is beneficial to modification of CM-chitosan by irradiation technique. However, little study was reported on radiation crosslinking and application of CM-chitosan. The radiation-closslinked CM-chitosan synthesized from chitosan was characterized by a Fourier transform infrared spectroscopy (FT-IR) analysis. A kinetic swelling in water and the mechanical properties such as a gelation, water absorptivity, and gel strength were also investigated. For the preparation of crosslinked CM-chitosan by using gamma irradiation, the concentration of an aqueous CM-chitosan is above 10wt%. We confirmed that the gel contents was in the range of 15-63%, and when the irradiation dose was increased, the degree of gelation was decreased by disintegration of the CM-chitosan. In conclusion, we developed a new

  5. Radiation Synthesis and Application of Carboxymethylated Chitosan Hydrogels

    International Nuclear Information System (INIS)

    Noh, Young Chang

    2007-08-01

    This research proposal is to investigate radiation effect of carboxymethylated chitosan in order to obtain the crosslinked carboxymethylated chitosan. The application studies on CM-chitosan- based intelligent hydrogels will be tried too. Chitin is the most abundant natural amino polysaccharide and estimated to be produced annually almost as much as cellulose. Chitosan is the deacetylated product of chitin showing the enhanced solubility in dilute acids, further, carboxymethylated chitosan (CM-chitosan) can solve in both acidic and basic physiological media, which might be good candidates as a kind of biomedical materials. Radiation technique is an important method for modification of chitin derivatives. It includes radiation-induced degradation, grafting, and crosslinking. It was found that CM-chitosan degraded in solid state or dilute aqueous solution under irradiation, but crosslinked at paste-like sate when the concentration of CM-chitosan is more than 10%. Both degraded and crosslinked CM-chitosan have antibacterial activity, so it is essential to investigate in detail the radiation effect of CM-chitosan. Study on radiation effect of CM-chitosan in different condition is beneficial to modification of CM-chitosan by irradiation technique. However, little study was reported on radiation crosslinking and application of CM-chitosan. The radiation-closslinked CM-chitosan synthesized from chitosan was characterized by a Fourier transform infrared spectroscopy (FT-IR) analysis. A kinetic swelling in water and the mechanical properties such as a gelation, water absorptivity, and gel strength were also investigated. For the preparation of crosslinked CM-chitosan by using gamma irradiation, the concentration of an aqueous CM-chitosan is above 10wt%. We confirmed that the gel contents was in the range of 15-63%, and when the irradiation dose was increased, the degree of gelation was decreased by disintegration of the CM-chitosan. In conclusion, we developed a new

  6. Chitosan Modification and Pharmaceutical/Biomedical Applications

    Directory of Open Access Journals (Sweden)

    Jiali Zhang

    2010-06-01

    Full Text Available Chitosan has received much attention as a functional biopolymer for diverse applications, especially in pharmaceutics and medicine. Our recent efforts focused on the chemical and biological modification of chitosan in order to increase its solubility in aqueous solutions and absorbability in the in vivo system, thus for a better use of chitosan. This review summarizes chitosan modification and its pharmaceutical/biomedical applications based on our achievements as well as the domestic and overseas developments: (1 enzymatic preparation of low molecular weight chitosans/chitooligosaccharides with their hypocholesterolemic and immuno-modulating effects; (2 the effects of chitin, chitosan and their derivatives on blood hemostasis; and (3 synthesis of a non-toxic ion ligand—D-Glucosaminic acid from Oxidation of D-Glucosamine for cancer and diabetes therapy.

  7. Disinfection of water with new chitosan-modified hybrid clay composite adsorbent

    Directory of Open Access Journals (Sweden)

    Emmanuel I. Unuabonah

    2017-08-01

    Full Text Available Hybrid clay composites were prepared from Kaolinite clay and Carica papaya seeds via modification with chitosan, Alum, NaOH, and ZnCl2 in different ratios, using solvothermal and surface modification techniques. Several composite adsorbents were prepared, and the most efficient of them for the removal of gram negative enteric bacteria was the hybrid clay composite that was surface-modified with chitosan, Ch-nHYCA1:5 (Chitosan: nHYCA = 1:5. This composite adsorbent had a maximum adsorption removal value of 4.07 × 106 cfu/mL for V. cholerae after 120 min, 1.95 × 106 cfu/mL for E. coli after ∼180 min and 3.25 × 106 cfu/mL for S. typhi after 270 min. The Brouers-Sotolongo model was found to better predict the maximum adsorption capacity (qmax of Ch-nHYCA1:5 composite adsorbent for the removal of E. coli with a qmax of 103.07 mg/g (7.93 × 107 cfu/mL and V. cholerae with a qmax of 154.18 mg/g (1.19 × 108 cfu/mL while the Sips model best described S. typhi adsorption by Ch-nHYCA1:5 composite with an estimated qmax of 83.65 mg/g (6.43 × 107 cfu/mL. These efficiencies do far exceed the alert/action levels of ca. 500 cfu/mL in drinking water for these bacteria. The simplicity of the composite preparation process and the availability of raw materials used for its preparation underscore the potential of this low-cost chitosan-modified composite adsorbent (Ch-nHYCA1:5 for water treatment.

  8. Hydrophosphorylation of substituted alkynes by phosphonic acids

    International Nuclear Information System (INIS)

    Nifant'ev, E.F.; Solovetskaya, L.A.; Maslennikova, V.I.; Sergeev, N.M.

    1987-01-01

    Hydrophosphorylation of functionally substituted alkynes by phosphonic acids can be a convenient method for synthesis of functionally substituted mono- and diphosphine oxides. The ease of hydrophosphorylation is determined by the strength of the negative inductive effect of the substituents on the triple bond and the steric factor. The structure of the bis-adducts was confirmed by elementary analysis and the 31 P and 13 C NMR spectra. The 31 P NMR spectrum is an AB two-spin system. The values of the chemical shifts and spin-spin interaction constants 3 J/sub PP/ are in agreement with the data in the literature for similar compounds

  9. Capillary gas chromatography of alkylbenzenes II. Correlations between the structures and methylene group increments and differences in retention indices of isomers

    NARCIS (Netherlands)

    Sojak, L.; Janak, J.; Rijks, J.A.

    1977-01-01

    The contribution to gas chromatographic retention behaviour of methylene group increments and differences in the retention indices (dI) of isomers of alkylbenzenes up to C16 on squalane and acetyltri-n-butyl citrate was studied. The methylene group increments appear to vary over a wide range (60–100

  10. Synthesis and characterization of Ag2S decorated chitosan nanocomposites and chitosan nanofibers for removal of lincosamides antibiotic.

    Science.gov (United States)

    Gupta, Vinod Kumar; Fakhri, Ali; Agarwal, Shilpi; Azad, Mona

    2017-10-01

    We report the synthesis of Ag 2 S-Chitosan nanocomposites and Ag 2 S-chitosan nanohybrids as performance adsorbents for Lincosamides such as Clindamycin antibiotic removal. Isotherms and kinetic studies were determined to understand the adsorption behavior both two adsorbent. At low adsorbent dose, removals are increased in the adsorption process, and performance is better with Ag 2 S-chitosan nanohybrids due to the special surface area increased. The average sizes and surface area of Ag 2 S-Chitosan nanocomposites and Ag 2 S-chitosan nanohybrids were found as 50nm, 70nm and 180.18, 238.24m 2 g -1 , respectively. In particular, Ag 2 S-Chitosan nanocomposites and Ag 2 S-chitosan nanohybrids show high maximum Clindamycin adsorption capacity (q max ) of 153.21, and 181.28mgg -1 , respectively. More strikingly, Ag 2 S-Chitosan nanocomposites and Ag 2 S-chitosan nanohybrids are also demonstrated to nearly completely remove Clindamycin from drinking water. The excellent adsorption performance along with their cost effective, convenient synthesis makes this range of adsorbents highly promising for commercial applications in drinking water and wastewater treatment. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Fragmentation of the radiation degraded chitosan by centrifugal filter and application of the fragmented chitosan in cotton fabrics finishing

    International Nuclear Information System (INIS)

    Luu Thi Tho; Nguyen Van Thong; Vu Thi Hong Khanh; Tran Minh Quynh

    2014-01-01

    Three kind of Vietnamese chitosans with the same deacetylation degrees of about 75% and viscosity average molecular weights are 69.000, 187.000 and 345.000 Da, respectively, were produced from shrimp shells and cuttle-bone at the MTV chitosan company (Kien Giang). These chitosans were irradiated at 25, 50, 75, 100, 200 and 500 kGy under Cobalt-60 gamma source at Hanoi Irradiation Center in order to prepare a series of chitosan segments with wide distribution of molecular weights. Different chitosan samples of the predetermined average molecular weight from 3,000 to 50,000 Da were separated from the irradiated chitosans by ultrafiltration with series of filter membranes (Centriprep devices). Molecular properties of the fragmented chitosans were analysed with gel permeation chromatography, Fourier transfer infra red spectrometry, and the results suggested that principal characteristics of chitosan were not affected by gamma irradiation, even its deacetylation degrees was increased. Solubility of the fragmented chitosans were much improved by radiation processing, and the chitosans having molecular weights below 5.000 Da were water-soluble polymers, which can easily apply as the auxiliary agent in textile. (author)

  12. Application of Spectroscopic Methods for Structural Analysis of Chitin and Chitosan

    Directory of Open Access Journals (Sweden)

    Jolanta Kumirska

    2010-04-01

    Full Text Available Chitin, the second most important natural polymer in the world, and its N-deacetylated derivative chitosan, have been identified as versatile biopolymers for a broad range of applications in medicine, agriculture and the food industry. Two of the main reasons for this are firstly the unique chemical, physicochemical and biological properties of chitin and chitosan, and secondly the unlimited supply of raw materials for their production. These polymers exhibit widely differing physicochemical properties depending on the chitin source and the conditions of chitosan production. The presence of reactive functional groups as well as the polysaccharide nature of these biopolymers enables them to undergo diverse chemical modifications. A complete chemical and physicochemical characterization of chitin, chitosan and their derivatives is not possible without using spectroscopic techniques. This review focuses on the application of spectroscopic methods for the structural analysis of these compounds.

  13. Phosphonate self-assembled monolayers on aluminum surfaces

    International Nuclear Information System (INIS)

    Hoque, E.; DeRose, J.A.; Hoffmann, P.; Mathieu, H.J.; Bhushan, B.; Cichomski, M.

    2006-01-01

    Substrates of aluminum (Al) deposited by physical vapor deposition onto Si substrates and then chemically reacted with perfluorodecylphosphonic acid (PFDP/Al/Si), decylphosphonic acid (DP/Al/Si), and octadecylphosphonic acid (ODP/Al/Si) were studied by x-ray photoelectron spectroscopy (XPS), contact angle measurements, atomic force microscopy (AFM), and friction force microscopy, a derivative of AFM, to characterize their surface chemical composition, roughness, and micro-/nanotribological properties. XPS analysis confirmed the presence of perfluorinated and nonperfluorinated alkylphosphonate molecules on the PFDP/Al/Si, DP/Al/Si, and ODP/Al/Si. The sessile drop static contact angle of pure water on PFDP/Al/Si was typically more than 130 deg. and on DP/Al/Si and ODP/Al/Si typically more than 125 deg. indicating that all phosphonic acid reacted Al/Si samples were very hydrophobic. The surface roughness for PFDP/Al/Si, DP/Al/Si, ODP/Al/Si, and bare Al/Si was approximately 35 nm as determined by AFM. The surface energy for PFDP/Al/Si was determined to be approximately 11 mN/m by the Zisman plot method compared to 21 and 20 mN/m for DP/Al/Si and ODP/Al/Si, respectively. Tribology involves the measure of lateral forces due to friction and adhesion between two surfaces. Friction, adhesion, and wear play important roles in the performance of micro-/nanoelectromechanical systems. PFDP/Al/Si gave the lowest adhesion and coefficient of friction values while bare Al/Si gave the highest. The adhesion and coefficient of friction values for DP/Al/Si and ODP/Al/Si were comparable

  14. Metal phosphonate coordination networks and frameworks as precursors of electrocatalysts for the hydrogen and oxygen evolution reactions

    Science.gov (United States)

    Zhang, Rui; El-Refaei, Sayed M.; Russo, Patrícia A.; Pinna, Nicola

    2018-05-01

    The hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER) play key roles in the conversion of energy derived from renewable energy sources into chemical energy. Efficient, robust, and inexpensive electrocatalysts are necessary for driving these reactions at high rates at low overpotentials and minimize energetic losses. Recently, electrocatalysts derived from hybrid metal phosphonate compounds have shown high activity for the HER or OER. We review here the utilization of metal phosphonate coordination networks and metal-organic frameworks as precursors/templates for transition-metal phosphides, phosphates, or oxyhydroxides generated in situ in alkaline solutions, and their electrocatalytic performance in HER or OER.

  15. Adsorption of methylene blue onto treated activated carbon

    International Nuclear Information System (INIS)

    Yamin Yasin; Mohd Zobir Hussein; Faujan Ahmad

    2007-01-01

    The potential feasibility of treated and untreated activated carbon for removal of methylene blue from aqueous solution was investigated. The effects of various experimental parameters such as contact time, solution pH and adsorbent dosage were investigated. The extent of methylene blue removal increased with the increased in contact time, solution pH and amount of adsorbent used. Adsorption data was better fitted to the Langmuir isotherm. The results in this study indicated that the treated activated carbon was an attractive candidate for removing organic dye of methylene blue which shows great reduction of colour while reducing the time contact to achieve equilibrium. (author)

  16. Secretion of antiretroviral chemokines by human cells cultured with acyclic nucleoside phosphonates

    Czech Academy of Sciences Publication Activity Database

    Zídek, Zdeněk; Kmoníčková, Eva; Holý, Antonín

    2007-01-01

    Roč. 574, - (2007), s. 77-84 ISSN 0014-2999 R&D Projects: GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z50390512; CEZ:AV0Z40550506 Keywords : Acyclic nucleoside phosphonate * Chemokine * Cytokine Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.376, year: 2007

  17. Extraction studies of actinides by diamylbutyl phosphonate

    International Nuclear Information System (INIS)

    Brahmananda Rao, C.V.S.; Jayalakshmi, S.; Subramaniam, S.; Sabharwal, K.N.; Sivaraman, N.; Vasudeva Rao, P.R.

    2014-01-01

    The extraction ability of a monodentate organophosphorus extractant depends on the basicity of the phosphoryl oxygen atom and the nature of the substituents attached to the phosphorus atom. The basicity on the phosphoryl oxygen in the neutral organophosphorus extractant series increases in the order, phosphates 1 H, 13 C and 31 P NMR spectra. Extraction of U(VI) by 1.1 M DABP/n-dodecane as a function of nitric acid was studied using 233 U tracer. Th(IV) extraction behaviour as a function of nitric acid was studied using Arsenazo-III as chromogenic agent. 5 mL of the 1.1 M DABP solution in the diluent (n-dodecane) was equilibrated with 5mL of saturated thorium nitrate in an equilibration tube using a magnetic stirring bar. The organic and aqueous phases were analysed by complexometry using DTPA as titrant and xylenol orange as indicator. The LOC values were determined as a function of nitric acid concentration. The extraction of U(VI) and Th(IV) by 1.1M DABP along with TBP in n-dodecane at 303 K as a function of equilibrium nitric acid concentration are shown. The DABP shows higher distribution ratios for U(VI) and Th(IV) in the entire range of nitric acid concentrations studied compared to TBP. The steep rise in the distribution ratio is attributed to the higher basicity of phosphoryl group in phosphonates compared to the less basic nature of phosphates. The third phase formation of thorium as function of nitric acid concentration with 1.1 M DABP at 303 K are given. The LOC values for DABP system were higher throughout the nitric acid concentration compared to the TBP system. (author)

  18. Preparation and properties of hydrogels of PVA/PVP/chitosan by radiation

    International Nuclear Information System (INIS)

    Nho, Y. C.; Park, K. R.

    2001-01-01

    The radiation can induce chemical reaction to modify polymer under even the solid condition or in the low temperature. The radiation crosslinking can be easily adjusted and is easily reproducible by controlling the radiation dose. The finished product contains no residuals of substances required to initiate the chemical crosslinking which can restrict the application possibilities. In these studies, hydrogels from a mixture of chitosan and polyvinyl alcohol(PVA)/Poly-N-vinylpyrrolidone(PVP) were made by 'freezing and thawing', or gamma-ray irradiation or two steps of 'freezing and thawing', and gamma-ray irradiation or two steps of 'freezing and thawing' and gamma-ray irradiation for wound dressing. The mechanical properties such as gelation, water absorptivity, and gel strength were examined to evaluate the hydrogels for wound dressing. The composition of PVA:PVP was 60:40, PVA/PVP: chitosan ratio was in the range of 9:1 -7:3, and the solid concentration of PVA/PVP/chitosan solution was 15wt%. Gamma irradiation doses of 25, 35, 50, 60 and 70kGy, respectively were exposed to a mixture of PVA/PVP/chitosan to evaluate the effect of irradiation dose on the mechanical properties of hydrogels. Water-soluble chitosan was used to in this experiment. The mechanical properties of hydrogels such as gelation and gel strength was higher when two steps of 'freezing and thawing' and irradiation were used than only 'freezing and thawing' was utilized. Gel content was influenced slightly by PVA/PVP:chitosan composition and irradiation dose, but swelling was done greatly by them. Swelling percent was much increased as the composition of chitosan in PVA/PVP/chitosan increased

  19. Efficient gene delivery using chitosan-polyethylenimine hybrid systems

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Hu-Lin; Kim, Tae-Hee; Kim, You-Kyoung; Park, In-Young; Cho, Chong-Su [Department of Agricultural Bioechnology, Seoul National University, Seoul 151-921 (Korea, Republic of); Cho, Myung-Haing [Laboratory of Toxicology, College of Veterinary Medicine, Seoul National University, Seoul 151-742 (Korea, Republic of)], E-mail: chocs@plaza.snu.ac.kr

    2008-06-01

    Chitosan and chitosan derivatives have been investigated as non-viral vectors because they have several advantages, such as biocompatibility, biodegradability, low cytotoxicity and low immunogenicity. However, low transfection efficiency and low cell specificity must be solved for their use in clinical trials. In this paper, chitosan-polyethylenimine (PEI) hybrid systems such as chitosan/PEI blend and chitosan-graft-PEI are described for efficient gene delivery because the PEI has high transfection efficiency owing to a proton sponge effect and chitosan has biocompatibility. Also, hepatocyte specificity of the galactosylated chitosan is explained after combination with PEI.

  20. Efficient gene delivery using chitosan-polyethylenimine hybrid systems

    International Nuclear Information System (INIS)

    Jiang, Hu-Lin; Kim, Tae-Hee; Kim, You-Kyoung; Park, In-Young; Cho, Chong-Su; Cho, Myung-Haing

    2008-01-01

    Chitosan and chitosan derivatives have been investigated as non-viral vectors because they have several advantages, such as biocompatibility, biodegradability, low cytotoxicity and low immunogenicity. However, low transfection efficiency and low cell specificity must be solved for their use in clinical trials. In this paper, chitosan-polyethylenimine (PEI) hybrid systems such as chitosan/PEI blend and chitosan-graft-PEI are described for efficient gene delivery because the PEI has high transfection efficiency owing to a proton sponge effect and chitosan has biocompatibility. Also, hepatocyte specificity of the galactosylated chitosan is explained after combination with PEI

  1. Application of irradiated chitosan for fruit preservation

    Energy Technology Data Exchange (ETDEWEB)

    Kieu N. Lan [Post Harvest Technology Inst. of Vietnam (Viet Nam)

    2000-09-01

    Application of irradiated chitosan has been investigated for coating of fruit preservation. Anti-fungal activity of chitosan was induced by {gamma}-ray irradiation in dry condition at 25 kGy. The irradiated chitosan can suppress the growth of Aspergillus. spp. and Fusarium. spp. isolated from Vietnam mango. Fusarium. spp. was sensitive for irradiated chitosan than the other strains. The coating from irradiated chitosan solution at dose 31 kGy has prolonged the storage life of mango from 7 to 15 days. At the 15th day mango keeps good colour, natural ripening, without spoilage, weight loss 10%, whereas the control is spoiled completely and the sample of fruit with unirradiated chitosan coating could not ripe. The effect is due to the anti-fungal activity and change in physico-chemical properties of chitosan by irradiation. Radiation causes the decrease in viscosity affecting the gas permeability of coating film. The irradiated chitosan coating has positive effect on mango that is susceptible to chilling injury at low storage temperature. (author)

  2. Plasticized chitosan/polyolefin films produced by extrusion.

    Science.gov (United States)

    Matet, Marie; Heuzey, Marie-Claude; Ajji, Abdellah; Sarazin, Pierre

    2015-03-06

    Plasticized chitosan and polyethylene blends were produced through a single-pass extrusion process. Using a twin-screw extruder, chitosan plasticization was achieved in the presence of an acetic acid solution and glycerol, and directly mixed with metallocene polyethylene, mPE, to produce a masterbatch. Different dilutions of the masterbatch (2, 5 and 10 wt% of plasticized chitosan), in the presence of ethylene vinyl acetate, EVA, were subsequently achieved in single screw film extrusion. Very small plasticized chitosan domains (number average diameter <5 μm) were visible in the polymeric matrix. The resulting films presented a brown color and increasing haze with chitosan plasticized content. Mechanical properties of the mPE films were affected by the presence of plasticized chitosan, but improvement was observed as a result of some compatibility between mPE and chitosan in the presence of EVA. Finally the incorporation of plasticized chitosan affected mPE water vapor permeability while oxygen permeability remained constant. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Application of irradiated chitosan for fruit preservation

    International Nuclear Information System (INIS)

    Kieu N, Lan; Nguyen D, Lam; Yoshii, Fumio; Kume, Tamikazu

    2000-01-01

    Application of irradiated chitosan has been investigated for coating of fruit preservation. Anti-fungal activity of chitosan was induced by γ-ray irradiation in dry condition at 25 kGy. The irradiated chitosan can suppress the growth of Aspergillus. spp. and Fusarium. spp. isolated from Vietnam mango. Fusarium. spp. was sensitive for irradiated chitosan than the other strains. The coating from irradiated chitosan solution at dose 31 kGy has prolonged the storage life of mango from 7 to 15 days. At the 15th day mango keeps good colour, natural ripening, without spoilage, weight loss 10%, whereas the control is spoiled completely and the sample of fruit with unirradiated chitosan coating could not ripe. The effect is due to the anti-fungal activity and change in physico-chemical properties of chitosan by irradiation. Radiation causes the decrease in viscosity affecting the gas permeability of coating film. The irradiated chitosan coating has positive effect on mango that is susceptible to chilling injury at low storage temperature. (author)

  4. Functional elastic hydrogel as recyclable membrane for the adsorption and degradation of methylene blue.

    Directory of Open Access Journals (Sweden)

    Song Bao

    Full Text Available Developing the application of high-strength hydrogels has gained much attention in the fields of medical, pharmacy, and pollutant removal due to their versatility and stimulus-responsive properties. In this presentation, a high-strength freestanding elastic hydrogel membrane was constructed by clay nanosheets, N, N-dimethylacrylamide and 2-acrylamide-2-methylpropanesulfonic acid for adsorption of methylene blue and heavy metal ions. The maximum values of elongation and Young's modulus for 0.5% AMPSNa hydrogel were 1901% and 949.4 kPa, respectively, much higher than those of traditional hydrogels. The adsorptions were confirmed to follow pseudo-second kinetic equation and Langmuir isotherm model fits the data well. The maximum adsorption capacity of hydrogel towards methylene blue was 434.8 mg g(-1. The hydrogel also exhibited higher separation selectivity to Pb(2+ than Cu(2+. The methylene blue adsorbed onto the hydrogel membrane can be photocatalytically degraded by Fenton agent and the hydrogel membrane could be recycled at least five times without obvious loss in mechanical properties. In conclusion, this presentation demonstrates a convenient strategy to prepare tough and elastic clay nanocomposite hydrogel, which can not only be applied as recyclable membrane for the photocatalytic degradation of organic dye, but also for the recovery of valuables.

  5. A mediator-free glucose biosensor based on glucose oxidase/chitosan/α-zirconium phosphate ternary biocomposite.

    Science.gov (United States)

    Liu, Li-Min; Wen, Jiwu; Liu, Lijun; He, Deyong; Kuang, Ren-yun; Shi, Taqing

    2014-01-15

    A novel glucose oxidase/chitosan/α-zirconium phosphate (GOD/chitosan/α-ZrP) ternary biocomposite was prepared by co-intercalating glucose oxidase (GOD) and chitosan into the interlayers of α-zirconium phosphate (α-ZrP) via a delamination-reassembly procedure. The results of X-ray diffraction, infrared spectroscopy, circular dichroism, and ultraviolet spectrum characterizations indicated not only the layered and hybrid structure of the GOD/chitosan/α-ZrP ternary biocomposite but also the recovered activity of the intercalated GOD improved by the co-intercalated chitosan. By depositing the GOD/chitosan/α-ZrP biocomposite film onto a glassy carbon electrode, the direct electrochemistry of the intercalated GOD was achieved with a fast electron transfer rate constant, k(s), of 7.48±3.52 s(-1). Moreover, this GOD/chitosan/α-ZrP biocomposite modified electrode exhibited a sensitive response to glucose in the linear range of 0.25-8.0 mM (R=0.9994, n=14), with a determination limit of 0.076 mM. Copyright © 2013 Elsevier Inc. All rights reserved.

  6. Effects of Chitosan Alkali Pretreatment on the Preparation of Electrospun PCL/Chitosan Blend Nanofibrous Scaffolds for Tissue Engineering Application

    Directory of Open Access Journals (Sweden)

    Fatemeh Roozbahani

    2013-01-01

    Full Text Available Recently, nanofibrous scaffolds have been used in the field of biomedical engineering as wound dressings, tissue engineering scaffolds, and drug delivery applications. The electrospun nanofibrous scaffolds can be used as carriers for several types of drugs, genes, and growth factors. PCL is one of the most commonly applied synthetic polymers for medical use because of its biocompatibility and slow biodegradability. PCL is hydrophobic and has no cell recognition sites on its structure. Electrospinning of chitosan and PCL blend was investigated in formic acid/acetic acid as the solvent with different PCL/chitosan ratios. High viscosity of chitosan solutions makes difficulties in the electrospinning process. Strong hydrogen bonds in a 3D network in acidic condition prevent the movement of polymeric chains exposed to the electrical field. Consequently, the amount of chitosan in PCL/chitosan blend was limited and more challenging when the concentration of PCL increases. The treatment of chitosan in alkali condition under high temperature reduced its molecular weight. Longer treatment time further decreased the molecular weight of chitosan and hence its viscosity. Electrospinning of PCL/chitosan blend was possible at higher chitosan ratio, and SEM images showed a decrease in fiber diameter and narrower distribution with increase in the chitosan ratio.

  7. UV-crosslinkable and thermo-responsive chitosan hybrid hydrogel for NIR-triggered localized on-demand drug delivery.

    Science.gov (United States)

    Wang, Lei; Li, Baoqiang; Xu, Feng; Xu, Zheheng; Wei, Daqing; Feng, Yujie; Wang, Yaming; Jia, Dechang; Zhou, Yu

    2017-10-15

    Innovative drug delivery technologies based on smart hydrogels for localized on-demand drug delivery had aroused great interest. To acquire smart UV-crosslinkable chitosan hydrogel for NIR-triggered localized on-demanded drug release, a novel UV-crosslinkable and thermo-responsive chitosan was first designed and synthesized by grafting with poly N-isopropylacrylamide, acetylation of methacryloyl groups and embedding with photothermal carbon. The UV-crosslinkable unit (methacryloyl groups) endowed chitosan with gelation via UV irradiation. The thermo-responsive unit (poly N-isopropylacrylamide) endowed chitosan hydrogel with temperature-triggered volume shrinkage and reversible swelling/de-swelling behavior. The chitosan hybrid hydrogel embedded with photothermal carbon exhibited distinct NIR-triggered volume shrinkage (∼42% shrinkage) in response to temperature elevation as induced by NIR laser irradiation. As a demonstration, doxorubicin release rate was accelerated and approximately 40 times higher than that from non-irradiated hydrogels. The UV-crosslinkable and thermal-responsive hybrid hydrogel served as in situ forming hydrogel-based drug depot is developed for NIR-triggered localized on-demand release. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Chitosan and chitosan chlorhydrate based various approaches for enhancement of dissolution rate of carvedilol

    Directory of Open Access Journals (Sweden)

    Shete Amol S

    2012-12-01

    Full Text Available Abstract Background and the purpose of the study Carvedilol nonselective β-adrenoreceptor blocker, chemically (±-1-(Carbazol-4-yloxy-3-[[2-(o-methoxypHenoxy ethyl] amino]-2-propanol, slightly soluble in ethyl ether; and practically insoluble in water, gastric fluid (simulated, TS, pH 1.1, and intestinal fluid (simulated, TS without pancreatin, pH 7.5 Compounds with aqueous solubility less than 1% W/V often represents dissolution rate limited absorption. There is need to enhance the dissolution rate of carvedilol. The objective of our present investigation was to compare chitosan and chitosan chlorhydrate based various approaches for enhancement of dissolution rate of carvedilol. Methods The different formulations were prepared by different methods like solvent change approach to prepare hydrosols, solvent evaporation technique to form solid dispersions and cogrind mixtures. The prepared formulations were characterized in terms of saturation solubility, drug content, infrared spectroscopy (FTIR, differential scanning calorimetry (DSC, powder X-ray diffraction (PXRD, electron microscopy, in vitro dissolution studies and stability studies. Results The practical yield in case of hydrosols was ranged from 59.76 to 92.32%. The drug content was found to uniform among the different batches of hydrosols, cogrind mixture and solid dispersions ranged from 98.24 to 99.89%. There was significant improvement in dissolution rate of carvedilol with chitosan chlorhdyrate as compare to chitosan and explanation to this behavior was found in the differences in the wetting, solubilities and swelling capacity of the chitosan and chitosan salts, chitosan chlorhydrate rapidly wet and dissolve upon its incorporation into the dissolution medium, whereas the chitosan base, less water soluble, would take more time to dissolve. Conclusion This technique is scalable and valuable in manufacturing process in future for enhancement of dissolution of poorly water soluble

  9. STIFFNESS MODIFICATION OF COTTON IN CHITOSAN TREATMENT

    Directory of Open Access Journals (Sweden)

    CAMPOS Juan

    2017-05-01

    Full Text Available Chitosan is a biopolymer obtained from chitin, and among their most important aspects highlights its applications in a lot of industrial sectors due to its intrinsic properties, especially in the textile sector. In the last years, chitosan is widely used in the cotton and wool finishing processes due to its bond between them and its properties as an antifungical and antimicrobial properties. In this paper three different molecular weight chitosan are used in the finishing process of cotton to evaluate its influence in the surface properties modification. In order to evaluate the effect of the treatment with chitosan, flexural stiffness test is performed in warp and weft direction, and then the total value is calculated. The cotton fabric is treated with 5 g/L of different types of chitosan in an impregnation bath. This study shows the extent of surface properties modification of the cotton provided by three types of chitosan treatment. The results show that all types of chitosan modify the cotton flexural rigidity properties but the one which modifies it in a relevant manner is chitosan originated from shrimps. Chitosan, textile, flexural stiffnes, chitin, cotton.

  10. Development of Cy5.5-Labeled Hydrophobically Modified Glycol Chitosan Nanoparticles for Protein Delivery

    Science.gov (United States)

    Chin, Amanda

    Therapeutic proteins are often highly susceptible to enzymatic degradation, thus restricting their in vivo stability. To overcome this limitation, delivery systems designed to promote uptake and reduce degradation kinetics have undergone a rapid shift from macro-scale systems to nanomaterial based carriers. Many of these nanomaterials, however, elicit immune responses and may have cytotoxic effects both in vitro and in vivo. The naturally derived polysaccharide chitosan has emerged as a promising biodegradable material and has been utilized for many biomedical applications; nevertheless, its function is often constrained by poor solubility. Glycol chitosan, a derivative of chitosan, can be hydrophobically modified to impart amphiphilic properties that enable the self-assembly into nanoparticles in aqueous media at neutral pH. This nanoparticle system has shown initial success as a therapeutic agent in several model cell culture systems, but little is known about its stability against enzymatic degradation. Therefore, the goal of this research was to investigate the resistance of hydrophobically modified glycol chitosan against enzyme-catalyzed degradation using an in vivo simulated system containing lysozyme. To synthesize the nanoparticles, hydrophobic cholanic acid was first covalently conjugated to glycol chitosan using of N-(3-Dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS). Conjugates were purified by dialysis, lyophilized, and ultra-sonicated to form nanoparticles. Fourier transform infrared (FT-IR) spectroscopy confirmed the binding of 5beta-cholanic acid to the glycol chitosan. Particle size and stability over time were determined with dynamic light scattering (DLS), and particle morphology was evaluated by transmission electron microscopy (TEM). The average diameter of the nanoparticles was approximately 200 nm, which remained stable at 4°C for up to 10 days. Additionally, a near infrared fluorescent (NIRF) dye

  11. Effect of Chitosan Properties on Immunoreactivity

    Science.gov (United States)

    Ravindranathan, Sruthi; Koppolu, Bhanu prasanth; Smith, Sean G.; Zaharoff, David A.

    2016-01-01

    Chitosan is a widely investigated biopolymer in drug and gene delivery, tissue engineering and vaccine development. However, the immune response to chitosan is not clearly understood due to contradicting results in literature regarding its immunoreactivity. Thus, in this study, we analyzed effects of various biochemical properties, namely degree of deacetylation (DDA), viscosity/polymer length and endotoxin levels, on immune responses by antigen presenting cells (APCs). Chitosan solutions from various sources were treated with mouse and human APCs (macrophages and/or dendritic cells) and the amount of tumor necrosis factor-α (TNF-α) released by the cells was used as an indicator of immunoreactivity. Our results indicate that only endotoxin content and not DDA or viscosity influenced chitosan-induced immune responses. Our data also indicate that low endotoxin chitosan (chitosan in preclinical studies in order for this valuable biomaterial to achieve widespread clinical application. PMID:27187416

  12. Characteristic of ascorbic acid in crosslinked chitosan edible film as drug delivery system membrane

    Directory of Open Access Journals (Sweden)

    Kistriyani Lilis

    2018-01-01

    Full Text Available Chitosan is a polysaccharide compound in the form of a linear polysaccharide consisting of N-acetyl glucosamine (GlcNAc and D-glucosamine (GlcN monomer, which is a derivative of deacetylization of chitin polymer. Chitin is one of common type of polysaccharide on earth after the excess cellulose from inveterbrata skeletons. Chitosan has anti-microbial properties. Based on this properties, chitosan is potentially used to be an edible film as drug delivery system membrane. Edible film was made by dissolving chitosan in 100 mL acetic acid 1%, then the plasticizer and crosslinker was added while heated at 60° C. It was molded and dried in oven at 50°C for 48 hours. Drug loading in the edible film could be controlled by remodeling membrane characteristics in the presence of crosslinker additions. The purpose of this study was to estimate the mass transfer coefficient (kCa of drug loading in various concentrations of ascorbic acid in the edible film. The characteristics of ascorbic acid in chitosan edible film could be seen from the number of drugs that could be loaded through the uv-vis spectrophotometric analysis. The higher concentration of ascorbic acid was added, the drug would be loaded more into edible film.

  13. Synthesis, kinetic evaluation, and utilization of a biotinylated dipeptide proline diphenyl phosphonate for the disclosure of dipeptidyl peptidase IV-like serine proteases.

    Science.gov (United States)

    Gilmore, Brendan F; Carson, Louise; McShane, Laura L; Quinn, Derek; Coulter, Wilson A; Walker, Brian

    2006-08-18

    In this study, we report on the synthesis, kinetic characterisation, and application of a novel biotinylated and active site-directed inactivator of dipeptidyl peptidase IV (DPP-IV). Thus, the dipeptide-derived proline diphenyl phosphonate NH(2)-Glu(biotinyl-PEG)-Pro(P)(OPh)(2) has been prepared by a combination of classical solution- and solid-phase methodologies and has been shown to be an irreversible inhibitor of porcine DPP-IV, exhibiting an over all second-order rate constant (k(i)/K(i)) for inhibition of 1.57 x 10(3) M(-1) min(-1). This value compares favourably with previously reported rates of inactivation of DPP-IV by dipeptides containing a P(1) proline diphenyl phosphonate grouping [B. Boduszek, J. Oleksyszyn, C.M. Kam, J. Selzler, R.E. Smith, J.C. Powers, Dipeptide phophonates as inhibitors of dipeptidyl peptidase IV, J. Med. Chem. 37 (1994) 3969-3976; B.F. Gilmore, J.F. Lynas, C.J. Scott, C. McGoohan, L. Martin, B. Walker, Dipeptide proline diphenyl phosphonates are potent, irreversible inhibitors of seprase (FAPalpha), Biochem, Biophys. Res. Commun. 346 (2006) 436-446.], thus demonstrating that the incorporation of the side-chain modified (N-biotinyl-3-(2-(2-(3-aminopropyloxy)-ethoxy)-ethoxy)-propyl) glutamic acid residue at the P(2) position is compatible with inhibitor efficacy. The utilisation of this probe for the detection of both purified dipeptidyl peptidase IV and the disclosure of a dipeptidyl peptidase IV-like activity from a clinical isolate of Porphyromonas gingivalis, using established electrophoretic and Western blotting techniques previously developed by our group, is also demonstrated.

  14. Effectiveness of chitosan against wine-related microorganisms.

    Science.gov (United States)

    Bağder Elmaci, Simel; Gülgör, Gökşen; Tokatli, Mehmet; Erten, Hüseyin; İşci, Asli; Özçelik, Filiz

    2015-03-01

    The antimicrobial action of chitosan against wine related microorganisms, including Lactobacillus plantarum, Saccharomyces cerevisiae, Oeonococcus oeni, Lactobacillus hilgardii, Brettanomyces bruxellensis, Hanseniaspora uvarum and Zygosaccharomyces bailii was examined in laboratory media. In order to assess the potential applicability of chitosan as a microbial control agent for wine, the effect of chitosan, applied individually and/or in combination with sulphur dioxide (SO2), on the growth of microorganisms involved in various stages of winemaking and on the fermentative performance of S. cerevisiae was investigated. Of the seven wine-related microorganisms studied, S. cerevisiae exhibited the strongest resistance to antimicrobial action of chitosan in laboratory media with a minimum inhibitory concentration (MIC) greater than 2 g/L. L. hilgardii, O. oeni and B. bruxellensis were the most susceptible to chitosan since they were completely inactivated by chitosan at 0.2 g/L. The MIC of chitosan for L. plantarum, H. uvarum and Z. bailii was 2, 0.4 and 0.4 g/L, respectively. In wine experiments, it was found that chitosan had a retarding effect on alcoholic fermentation without significantly altering the viability and the fermentative performance of S. cerevisiae. With regard to non-Saccharomyces yeasts (H. uvarum and Z. bailii) involved in winemaking, the early deaths of these yeasts in mixed cultures with S. cerevisiae were not probably due to the antimicrobial action of chitosan but rather due to ethanol produced by the yeasts. The complex interactions between chitosan and wine ingredients as well as microbial interactions during wine fermentation considerably affect the efficacy of chitosan. It was concluded that chitosan was worthy of further investigation as an alternative or complementary preservative to SO2 in wine industry.

  15. Alkyl chitosan film-high strength, functional biomaterials.

    Science.gov (United States)

    Lu, Li; Xing, Cao; Xin, Shen; Shitao, Yu; Feng, Su; Shiwei, Liu; Fusheng, Liu; Congxia, Xie

    2017-11-01

    Biofilm with strong tensile strength is a topic item in the area of tissue engineering, medicine engineering, and so forth. Here we introduced an alkyl chitosan film with strong tensile strength and its possibility for an absorbable anticoagulation material in vivo was tested in the series of blood test, such as dynamic coagulation time, plasma recalcification time and hemolysis. Alkyl chitosan film was a better biomaterial than traditional chitosan film in the anticoagulation, tissue compatibility and cell compatibility. The unique trait of alkyl chitosan film may be for its greater contact angle and hydrophobicity ability to reduce the adsorption capacity for the blood component and the activity of fibrinolytic enzymes, enhance the antibacterial capacity than chitosan film. Moreover, none of chitosan film or butyl chitosan film exhibited quick inflammation or other disadvantage and degraded quickly by implanted test. Therefore, Alkyl chitosan film is of prospective properties as an implantable, absorbable agent for tissue heals, and this material need further research. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 3034-3041, 2017. © 2017 Wiley Periodicals, Inc.

  16. Removal of Arsenic (V) from Aqueous Solutions Using Chitosan-Red Scoria and Chitosan-Pumice Blends.

    Science.gov (United States)

    Asere, Tsegaye Girma; Mincke, Stein; De Clercq, Jeriffa; Verbeken, Kim; Tessema, Dejene A; Fufa, Fekadu; Stevens, Christian V; Du Laing, Gijs

    2017-08-09

    In different regions across the globe, elevated arsenic contents in the groundwater constitute a major health problem. In this work, a biopolymer chitosan has been blended with volcanic rocks (red scoria and pumice) for arsenic (V) removal. The effect of three blending ratios of chitosan and volcanic rocks (1:2, 1:5 and 1:10) on arsenic removal has been studied. The optimal blending ratio was 1:5 (chitosan: volcanic rocks) with maximum adsorption capacity of 0.72 mg/g and 0.71 mg/g for chitosan: red scoria (Ch-Rs) and chitosan: pumice (Ch-Pu), respectively. The experimental adsorption data fitted well a Langmuir isotherm ( R ² > 0.99) and followed pseudo-second-order kinetics. The high stability of the materials and their high arsenic (V) removal efficiency (~93%) in a wide pH range (4 to 10) are useful for real field applications. Moreover, the blends could be regenerated using 0.05 M NaOH and used for several cycles without losing their original arsenic removal efficiency. The results of the study demonstrate that chitosan-volcanic rock blends should be further explored as a potential sustainable solution for removal of arsenic (V) from water.

  17. Microencapsulation of norfloxacin in chitosan/chitosan oligosaccharides and its application in shrimp culture.

    Science.gov (United States)

    Lian, Ziru; Pan, Rong; Wang, Jiangtao

    2016-11-01

    Norfloxacin chitosan/chitosan oligosaccharide microcapsules (NCCM) were prepared by emulsion-chemical crosslinking method. The characteristics of obtained microcapsules were evaluated by scanning electron microscopy, Fourier transform infrared spectroscopy and release experiments. Cumulative release profile of norfloxacin from the chitosan microcapsules in natural seawater was measured and the controlled release of drugs was at a uniform rate in 48h. The chitosan microcapsules were applied onto the antibacterial study of the shrimp culture in natural seawater. It is observed that the seawater in the NCCM added groups was relatively clear and the biomass of Vibrio increased slowly in contrast to the control and norfloxacin groups. The inhibition rate of Vibrio in norfloxacin groups obvioursly decreased after the 5 th day, whereas, it remained high and stable during experiment period in NCCM groups. The results showed that the chitosan microcapsules as release materials have excellent antibacterial effects on Vibrio in the farming of Penaeus vannamei Boone. The controlled release could obviously reduce dosage of antibiotics and delivery times, and effectively improve the utilization rate of norfloxacin drugs for shrimps. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Surface grafted chitosan gels. Part I. Molecular insight into the formation of chitosan and poly(acrylic acid) multilayers

    DEFF Research Database (Denmark)

    Liu, Chao; Thormann, Esben; Claesson, Per M.

    2014-01-01

    Composite polyelectrolyte multilayers of chitosan and low molecular weight poly(acrylic acid) (PAA) have been assembled by sequential adsorption as a first step toward building a surface anchored chitosan gel. Silane chemistry was used to graft the first chitosan layer to prevent film detachment...... and decomposition. The assembly process is characterized by nonlinear growth behavior, with different adsorption kinetics for chitosan and PAA. In situ analysis of the multilayer by means of surface sensitive total internal reflection Raman (TIRR) spectroscopy, combined with target factor analysis of the spectra...... molecular weight chitosan shows a similar behavior, although to a much lower extent. Our data demonstrate that the charged monomeric units of chitosan are mainly compensated by carboxylate ions from PAA. Furthermore, the morphology and mechanical properties of the multilayers were investigated in situ using...

  19. Chitosan Dermal Substitute and Chitosan Skin Substitute Contribute to Accelerated Full-Thickness Wound Healing in Irradiated Rats

    Directory of Open Access Journals (Sweden)

    Abu Bakar Mohd Hilmi

    2013-01-01

    Full Text Available Wounds with full-thickness skin loss are commonly managed by skin grafting. In the absence of a graft, reepithelialization is imperfect and leads to increased scar formation. Biomaterials can alter wound healing so that it produces more regenerative tissue and fewer scars. This current study use the new chitosan based biomaterial in full-thickness wound with impaired healing on rat model. Wounds were evaluated after being treated with a chitosan dermal substitute, a chitosan skin substitute, or duoderm CGF. Wounds treated with the chitosan skin substitute showed the most re-epithelialization (33.2 ± 2.8%, longest epithelial tongue (1.62 ± 0.13 mm, and shortest migratory tongue distance (7.11 ± 0.25 mm. The scar size of wounds treated with the chitosan dermal substitute (0.13 ± 0.02 cm and chitosan skin substitute (0.16 ± 0.05 cm were significantly decreased (P<0.05 compared with duoderm (0.45 ± 0.11 cm. Human leukocyte antigen (HLA expression on days 7, 14, and 21 revealed the presence of human hair follicle stem cells and fibroblasts that were incorporated into and surviving in the irradiated wound. We have proven that a chitosan dermal substitute and chitosan skin substitute are suitable for wound healing in full-thickness wounds that are impaired due to radiation.

  20. Physical Properties and Antibacterial Efficacy of Biodegradable Chitosan Films

    OpenAIRE

    中島, 照夫

    2009-01-01

    [Synopsis] Chitin, chitosan and quaternary chitosan films were prepared, and the physical properties and the antibacterial activities of chitosan and quaternary chitosan films were evaluated. The tensile strength of chitin films was 30~40% lower than that of chitosan films, but the crystallinity of chitin film was much higher than that of chitosan films. The crystallinity and orientation of crystallites were hardly affected by the four kinds of solvent chosen to cast chitosan films, but a de...

  1. New prodrugs of two pyrimidine acyclic nucleoside phosphonates: Synthesis and antiviral activity

    Czech Academy of Sciences Publication Activity Database

    Krečmerová, Marcela; Dračínský, Martin; Snoeck, R.; Balzarini, J.; Pomeisl, Karel; Andrei, G.

    2017-01-01

    Roč. 25, č. 17 (2017), s. 4637-4648 ISSN 0968-0896 R&D Projects: GA ČR(CZ) GA14-00522S Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonates * open-ring * PMEO-DAPy * 5-azacytosine * PME-azaC * HPMP-5-azaC Subject RIV: CC - Organic Chemistry OBOR OECD: Organic chemistry Impact factor: 2.930, year: 2016

  2. Emerging Biomedical Applications of Nano-Chitins and Nano-Chitosans Obtained via Advanced Eco-Friendly Technologies from Marine Resources

    Science.gov (United States)

    Muzzarelli, Riccardo A. A.; El Mehtedi, Mohamad; Mattioli-Belmonte, Monica

    2014-01-01

    The present review article is intended to direct attention to the technological advances made in the 2010–2014 quinquennium for the isolation and manufacture of nanofibrillar chitin and chitosan. Otherwise called nanocrystals or whiskers, n-chitin and n-chitosan are obtained either by mechanical chitin disassembly and fibrillation optionally assisted by sonication, or by e-spinning of solutions of polysaccharides often accompanied by poly(ethylene oxide) or poly(caprolactone). The biomedical areas where n-chitin may find applications include hemostasis and wound healing, regeneration of tissues such as joints and bones, cell culture, antimicrobial agents, and dermal protection. The biomedical applications of n-chitosan include epithelial tissue regeneration, bone and dental tissue regeneration, as well as protection against bacteria, fungi and viruses. It has been found that the nano size enhances the performances of chitins and chitosans in all cases considered, with no exceptions. Biotechnological approaches will boost the applications of the said safe, eco-friendly and benign nanomaterials not only in these fields, but also for biosensors and in targeted drug delivery areas. PMID:25415349

  3. Animal experiments and clinical trials of 166Ho-Chitosan for various cancers

    International Nuclear Information System (INIS)

    Lim, S.M.; Choi, C.W.; Park, S.Y.; Lee, S.H.; Lee, B.H.; Park, K.B.

    1998-01-01

    166 Ho-Chitosan is a complex of 166 Ho and N-glucosamine with 400 to 500 kD MW, which chelates metal ions and degrades slowly in vivo. In mice, 166 H-Chitosan administered intraperitoneally was uniformly bound to the peritoneal wall (94%), and the surface dose calculated by Monte Carlo simulation (EGS 4 code) was 81 Gy/uCi/cm 2 . 166 Ho-Chitosan was administered intraperitoneally as an adjunct in the treatment of ovarian cancer with diffuse spread of malignant cells in the peritoneal surfaces including the diaphragm. 97-99% of 166 Ho-Chitosan was localized within the peritoneal cavity, and more than 90% of 166 Ho-Chitosan was attached to the peritoneal wall. Partial response were observed in 4 among 5 patients with ovarian cancer without severe toxicity. Intracavitary radiation therapy with 166 Ho-Chitosan in the cystic brain tumor, 5 or 8 cysts were shrunken in size with thinning of the wall, 2 out of 8 showed growth retardation. For large or multiple primary liver cancers, which were inoperable and resistent to chemotherapy. 166 Ho-Chitosan was used for intraarterial injection, because this solution became gel with neutral pH. In the primary liver cancer, radioactivity was distributed in the territory of selected hepatic arterial branch, and partial responses were observed in 2 cases. For the large solitary liver tumor, which was not operable due to its location, direct intratumoral injection of the radioisotope had a limited response. 18 FDG PET was a useful tool to follow up those radionuclide therapy, and guide to plan the next therapy. In one case of the large single metastatic stomach cancer in the liver, 18 FDG PET was done two weeks after intratumoral injection of 166 Ho-Chitosan, which showed cold defects matched with distribution of 166 Ho-Chitosan, and second injection was guided by PET image. Various methods of the administration of 166 Ho-Chitosan could be used for the treatment of the cancers. (author)

  4. Multicomponent reactions: A simple and efficient route to heterocyclic phosphonates

    Science.gov (United States)

    2016-01-01

    Summary Multicomponent reactions (MCRs) are one of the most important processes for the preparation of highly functionalized organic compounds in modern synthetic chemistry. As shown in this review, they play an important role in organophosphorus chemistry where phosphorus reagents are used as substrates for the synthesis of a wide range of phosphorylated heterocycles. In this article, an overview about multicomponent reactions used for the synthesis of heterocyclic compounds bearing a phosphonate group on the ring is given. PMID:27559377

  5. Immobilization of catalase on chitosan and amino acid- modified chitosan beads.

    Science.gov (United States)

    Başak, Esra; Aydemir, Tülin

    2013-08-01

    Bovine liver catalase was covalently immobilized onto amino acid-modified chitosan beads. The beads were characterized with SEM, FTIR, TGA and the effects of immobilization on optimum pH and temperature, thermostability, reusability were evaluated. Immobilized catalase showed the maximal enzyme activity at pH 7.0 at 30°C. The kinetic parameters, Km and Vmax, for immobilized catalase on alanine-chitosan beads and lysine-chitosan beads were estimated to be 25.67 mM, 27 mM and 201.39 μmol H2O2/min, 197.50 μmol H2O2/min, respectively. The activity of the immobilized catalase on Ala-CB and Lys-CB retained 40% of its high initial activity after 100 times of reuse.

  6. Degradation of chitosan for rice crops application

    International Nuclear Information System (INIS)

    Norzita Yacob; Maznah Mahmud; Norhashidah Talip; Kamaruddin Hashim; Abdul Rahim Harun; Khairul Zaman; Hj Dahlan

    2013-01-01

    A variety of techniques including chemical and enzymatic hydrolysis, and radiation degradation processes can be used to prepare low molecular weight chitosan. Degradation of chitosan by radiation can be carried out in solid state and liquid state. Radiation degraded polysaccharides has been reported to exhibit growth-stimulating activity like phytohormones that induce the promotion in germination, shoot and root elongation in variety of plants. In this study, the chitosan was irradiated in solid state (powder form) by gamma rays within the dose range of 25-75 kGy. And the irradiated chitosan was then irradiated in solution form in the presence of hydrogen peroxide. The effects of irradiation on the molecular weight and viscosity of the chitosan were investigated using Ubbelohde Capillary Viscometer. The molecular weight and viscosity of the chitosan decreased with increment of absorbed doses. In the presence of hydrogen peroxide, the molecular weight of chitosan could be further decreased. The effect of radiation degraded chitosan on the growth promotion of rice was investigated and it was shown during seedling period of 15 days for transplanting whereby the growth is 15%-20% faster than using chemicals growth promoters. (authors)

  7. Development of chitosan-pullulan composite nanoparticles for nasal delivery of vaccines: in vivo studies.

    Science.gov (United States)

    Cevher, Erdal; Salomon, Stefan K; Somavarapu, Satyanarayana; Brocchini, Steve; Alpar, H Oya

    2015-01-01

    Here, we aimed at developing chitosan/pullulan composite nanoparticles and testing their potential as novel systems for the nasal delivery of diphtheria toxoid (DT). All the chitosan derivatives [N-trimethyl (TMC), chloride and glutamate] and carboxymethyl pullulan (CMP) were synthesised and antigen-loaded composites were prepared by polyion complexation of chitosan and pullulan derivatives (particle size: 239-405 nm; surface charge: +18 and +27 mV). Their immunological effects after intranasal administration to mice were compared to intramuscular route. Composite nanoparticles induced higher levels of IgG responses than particles formed with chitosan derivative and antigen. Nasally administered TMC-pullulan composites showed higher DT serum IgG titre when compared with the other composites. Co-encapsulation of CpG ODN within TMC-CMP-DT nanoparticles resulted in a balanced Th1/Th2 response. TMC/pullulan composite nanoparticles also induced highest cytokine levels compared to those of chitosan salts. These findings demonstrated that TMC-CMP-DT composite nanoparticles are promising delivery system for nasal vaccination.

  8. Methylene blue adsorption by algal biomass based materials: biosorbents characterization and process behaviour.

    Science.gov (United States)

    Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

    2007-08-17

    Dead algal biomass is a natural material that serves as a basis for developing a new family of sorbent materials potentially suitable for many industrial applications. In this work an algal industrial waste from agar extraction process, algae Gelidium and a composite material obtained by immobilization of the algal waste with polyacrylonitrile (PAN) were physical characterized and used as biosorbents for dyes removal using methylene blue as model. The apparent and real densities and the porosity of biosorbents particles were determined by mercury porosimetry and helium picnometry. The methylene blue adsorption in the liquid phase was the method chosen to calculate the specific surface area of biosorbent particles as it seems to reproduce better the surface area accessible to metal ions in the biosorption process than the N2 adsorption-desorption dry method. The porous texture of the biosorbents particles was also studied. Equilibrium isotherms are well described by the Langmuir equation, giving maximum uptake capacities of 171, 104 and 74 mg g(-1), respectively for algae, algal waste and composite material. Kinetic experiments at different initial methylene blue concentrations were performed to evaluate the equilibrium time and the importance of the driving force to overcome mass transfer resistances. The pseudo-first-order and pseudo-second-order kinetic models adequately describe the kinetic data. The biosorbents used in this work proved to be promising materials for removing methylene blue from aqueous solutions.

  9. Versatile nature of hetero-chitosan based derivatives as biodegradable adsorbent for heavy metal ions; a review.

    Science.gov (United States)

    Ahmad, Mudasir; Manzoor, Kaiser; Ikram, Saiqa

    2017-12-01

    The polyfunctional chitosan can act as the biological macromolecule ligand not only for the adsorption and the recovery of metal ions from an aqueous media, but also for the fabrication of novel adsorbents which shows selectivity and better adsorption properties. The unmodified chitosan itself, a single cationic polysaccharide, has hydroxyl and amine groups carrying complex properties with the metal ions. In addition, the selectivity of metal ions, the adsorption efficiency and adsorption capacity of the adsorbent can be modified chemically. This review covers the synthetic strategies of chitosan towards the synthesis of hetero-chitosan based adsorbents via chemical modifications in past two decades. It also includes how chemical modification influences the metal adsorption with N, O, S and P containing chitosan derivatives. Hope this review article provides an opportunity for researchers in the future to explore the potential of chitosan as an adsorbent for removal of metal ions from wastewater. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Effect of water-soluble P-chitosan and S-chitosan on human primary osteoblasts and giant cell tumor of bone stromal cells

    Energy Technology Data Exchange (ETDEWEB)

    Tang, T; Zhang, G; PY Lau, Carol; Zheng, L Z; Xie, X H; Wang, X L; Patrick, Y; Qin, L; Kumta, Shekhar M [Department of Orthopaedics and Traumatology, Chinese University of Hong Kong (Hong Kong); Wang, X H; He, K, E-mail: kumta@cuhk.edu.hk [Department of Mechanical Engineering, Institute of Bio-manufacturing Engineering, Tsinghua University, Beijing (China)

    2011-02-15

    Water-soluble phosphorylated chitosan (P-chitosan) and disodium (1 {yields} 4)-2-deoxy-2-sulfoamino-{beta}-D-glucopyranuronan (S-chitosan) are two chemically modified chitosans. In this study, we found that P-chitosan significantly promotes cell proliferation of both human primary osteoblasts (OBs) and the OB like stromal cell component of the giant cell tumor of bone (GCTB) cells at the concentration from 125 to 1000 {mu}g ml{sup -1} at all time points of 1, 3, 5 and 7 days after treatment. Further investigation of the osteogenic effect of the P-chitosan suggested that it regulates the levels of osteoclastogenic factors, receptor activator of nuclear factor kappa B ligand and osteoprotegerin expression. An interesting finding is that S-chitosan at lower concentration (100 {mu}g ml{sup -1}) stimulates cell proliferation while a higher dose (1000 {mu}g ml{sup -1}) of S-chitosan inhibits it. The inhibitory effect of S-chitosan on human primary GCT stromal cells was greater than that of OBs (p < 0.05). Taken together, our findings elucidated the osteogenic effect of P-chitosan and the varying effects of S-chitosan on the proliferation of human primary OBs and GCT stromal cells and provided us the rationale for the construction of novel bone repair biomaterials with the dual properties of bone induction and bone tumor inhibition.

  11. Oral Vaccination Based on DNA-Chitosan Nanoparticles against Schistosoma mansoni Infection

    Directory of Open Access Journals (Sweden)

    Carolina R. Oliveira

    2012-01-01

    Full Text Available The development of a vaccine would be essential for the control of schistosomiasis, which is recognized as the most important human helminth infection in terms of morbidity and mortality. A new approach of oral vaccination with DNA-chitosan nanoparticles appears interesting because of their great stability and the ease of target accessibility, besides chitosan immunostimulatory properties. Here we described that chitosan nanoparticles loaded with plasmid DNA encoding Rho1-GTPase protein of Schistosoma mansoni, prepared at different molar ratios of primary amines to DNA phosphate anion (N/P, were able to complex electrostatically with DNA and condense it into positively charged nanostructures. Nanoparticles were able to maintain zeta potential and size characteristics in media that simulate gastric (SGF and intestinal fluids (SIF. Further in vivo studies showed that oral immunization was not able to induce high levels of specific antibodies but induced high levels of the modulatory cytokine IL-10. This resulted in a significative reduce of liver pathology, although it could not protect mice of infection challenge with S. mansoni worms. Mice immunized only with chitosan nanoparticles presented 47% of protection against parasite infection, suggesting an important role of chitosan in inducing a protective immune response against schistosomiasis, which will be more explored in further studies.

  12. Entirely S-protected chitosan: A promising mucoadhesive excipient for metronidazole vaginal tablets.

    Science.gov (United States)

    Lupo, Noemi; Fodor, Benjamin; Muhammad, Ijaz; Yaqoob, Muhammad; Matuszczak, Barbara; Bernkop-Schnürch, Andreas

    2017-12-01

    Synthesis and evaluation of an entirely S-protected chitosan as mucoadhesive excipient for vaginal drug delivery. N-acetyl-cysteine was linked to 6-mercaptonicotinamide via disulphide exchange reaction. The obtained ligand, NAC-6-MNA, was subsequently attached to chitosan by carbodiimide mediated amide bond formation in two concentrations. The synthesized S-protected chitosan was chemically characterized and mucoadhesive properties and stability against oxidation were investigated. Moreover, metronidazole tablets comprising the S-protected chitosan were evaluated regarding water uptake capacity, disintegration behaviour, residence time on vaginal mucosa, release of the encapsulated drug and antimicrobial activity. S-protected chitosan displayed 160±19 (CS-MNA-160) and 320±38 (CS-MNA-320)µmol of ligand per gram of polymer. At pH 4.2, CS-MNA-160 and CS-MNA-320 showed 5.2-fold and 6.2-fold increase in mucus viscosity in comparison to unmodified chitosan (One-way ANOVA, pchitosan remained stable against oxidation in presence of 0.5%v/v hydrogen peroxide. Metronidazole tablets consisting in S-protected chitosan showed prolonged residence time on vaginal mucosa and improved water uptake capacity and disintegration time in comparison to tablets consisting of unmodified chitosan. Moreover, CS-MNA-320 metronidazole tablets displayed prolonged drug release and antimicrobial activity. On the basis of the achieved results, entirely S-protected chitosan represents a promising excipient for the development of metronidazole vaginal tablets. S-protected thiomers are polymers modified with thiol groups protected by aromatic ligands and characterized by strong mucoadhesive properties and high stability against oxidation. Up to date, the entirely S-protection of thiol groups was achieved via the synthesis of the ligand 2-((2-amino-2-carboxyethyl)disulfanyl)nicotinic acid) which can be directly bound to the backbone of polymers bearing carboxylic moieties as pectin. However, this

  13. Effect of Chitosan Properties on Immunoreactivity

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    Sruthi Ravindranathan

    2016-05-01

    Full Text Available Chitosan is a widely investigated biopolymer in drug and gene delivery, tissue engineering and vaccine development. However, the immune response to chitosan is not clearly understood due to contradicting results in literature regarding its immunoreactivity. Thus, in this study, we analyzed effects of various biochemical properties, namely degree of deacetylation (DDA, viscosity/polymer length and endotoxin levels, on immune responses by antigen presenting cells (APCs. Chitosan solutions from various sources were treated with mouse and human APCs (macrophages and/or dendritic cells and the amount of tumor necrosis factor-α (TNF-α released by the cells was used as an indicator of immunoreactivity. Our results indicate that only endotoxin content and not DDA or viscosity influenced chitosan-induced immune responses. Our data also indicate that low endotoxin chitosan (<0.01 EU/mg ranging from 20 to 600 cP and 80% to 97% DDA is essentially inert. This study emphasizes the need for more complete characterization and purification of chitosan in preclinical studies in order for this valuable biomaterial to achieve widespread clinical application.

  14. Effect of chitosan-carvacrol coating on the quality of Pacific white shrimp during iced storage as affected by caprylic acid.

    Science.gov (United States)

    Wang, Qianyun; Lei, Jun; Ma, Junjie; Yuan, Gaofeng; Sun, Haiyan

    2018-01-01

    This study aimed to investigate the effect of chitosan-carvacrol coating with or without caprylic acid (CAP) on the quality of Pacific white shrimp (Litopenaeus vannamei) during 10days of iced storage. The result showed that chitosan-carvacrol coating significantly inhibited the increase in total aerobic plate count (TPC), pH and total volatile basic nitrogen content (TVB-N) of shrimp in comparison with the control. Chitosan-carvacrol coating also delayed the melanosis formation and changes of ΔE values, and improved the texture and sensory properties of shrimp. Moreover, incorporation of CAP potentiated the efficacy of chitosan-carvacrol coating in retarding the increase of TPC and TVB-N. Incorporation of CAP into chitosan-carvacrol coating also enabled the texture characteristics of shrimp to be retained greater degrees. These results suggested that chitosan-carvacrol coating may be promising to be used as active packaging for extending the shelf life, and incorporation of CAP may enhance the efficacy of the coating. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. The effect of andiroba oil and chitosan concentration on the physical properties of chitosan emulsion film

    Directory of Open Access Journals (Sweden)

    Vanessa Tiemi Kimura

    Full Text Available Abstract Chitosan film is used as a dressing to heal burns. The physical and biological properties of the film can be modified by the addition of phytotherapic compounds. This work used the casting -solvent evaporation technique to prepare chitosan film containing andiroba oil (Carapa guianensis which has anti-inflammatory, antibiotic, and healing properties. The objective of this study was to determine the effect of the concentrations of chitosan and andiroba oil on the physical properties of chitosan films. The emulsion films were evaluated concerning the mechanical properties and fluid handling capacity. Additionally, scanning electron microscopy and thermal analysis were performed. The results showed that the barrier and mechanical properties were affected by the addition of andiroba oil, and these may be modulated as a function of the concentration of oil added to the film. The thermal analysis showed no evidence of chemical interactions between the oil and chitosan.

  16. Enhancement of antimicrobial activity of chitosan by irradiation

    International Nuclear Information System (INIS)

    Matsuhashi, S.; Kume, T.

    1997-01-01

    Antimicrobial activity of irradiated chitosan was studied against Escherichia coli B/r. Irradiation of chitosan at 100 kGy under dry conditions was effective in increasing the activity, and inhibited the growth of E. coli completely. The molecular weight of chitosan significantly decreased with the increase in irradiation dose, whereas the relative surface charge of chitosan was decreased only 3% by 100 kGy irradiation. Antimicrobial activity assay of chitosan fractionated according to molecular weight showed that 1 x 10 5 -3 x 10 5 fraction was most effective in suppressing the growth of E coli. This fraction comprised only 8% of the 100 kGy irradiated chitosan. On the other hand, chitosan whose molecular weight was less than 1 x 10 5 had no activity. The results show that low dose irradiation, specifically 100 kGy, of chitosan gives enough degradation to increase its antimicrobial activity as a result of a change in molecular weight. (Author)

  17. Study on the inclusion interaction of p-sulfonated calix[n]arenes with Vitamin K3 using methylene blue as a spectral probe.

    Science.gov (United States)

    Lu, Qin; Gu, Jiashan; Yu, Huapeng; Liu, Chun; Wang, Lun; Zhou, Yunyou

    2007-09-01

    The characteristics of host-guest complexation between p-sulfonated calix[n]arene (SCnA, n = 4, 6) and Vitamin K(3) (VK(3)) were investigated by fluorescence spectrometry and absorption spectrometry using methylene blue (MB) as a probe. Interaction with MB and SCnA led to an obvious decrease in fluorescence intensity of MB, accompanying with shifts of emission peaks. Absorption peaks also showed interesting changes; however, when VK(3) was added, fluorescence intensity and absorbance recovered and a slight and slow red shift was observed. The obtained results showed that the inclusion ability of p-sulphonated calix[n]arenes towards VK(3) was the order: p-sulphonated calix[6]arene (SC6A) >p-sulphonated calix[4]arene (SC4A). Relative mechanism was proposed to explain the inclusion process.

  18. Chitosan and Its Derivatives for Application in Mucoadhesive Drug Delivery Systems

    Directory of Open Access Journals (Sweden)

    Twana Mohammed M. Ways

    2018-03-01

    Full Text Available Mucoadhesive drug delivery systems are desirable as they can increase the residence time of drugs at the site of absorption/action, provide sustained drug release and minimize the degradation of drugs in various body sites. Chitosan is a cationic polysaccharide that exhibits mucoadhesive properties and it has been widely used in the design of mucoadhesive dosage forms. However, its limited mucoadhesive strength and limited water-solubility at neutral and basic pHs are considered as two major drawbacks of its use. Chemical modification of chitosan has been exploited to tackle these two issues. In this review, we highlight the up-to-date studies involving the synthetic approaches and description of mucoadhesive properties of chitosan and chitosan derivatives. These derivatives include trimethyl chitosan, carboxymethyl chitosan, thiolated chitosan, chitosan-enzyme inhibitors, chitosan-ethylenediaminetetraacetic acid (chitosan-EDTA, half-acetylated chitosan, acrylated chitosan, glycol chitosan, chitosan-catechol, methyl pyrrolidinone-chitosan, cyclodextrin-chitosan and oleoyl-quaternised chitosan. We have particularly focused on the effect of chemical derivatization on the mucoadhesive properties of chitosan. Additionally, other important properties including water-solubility, stability, controlled release, permeation enhancing effect, and in vivo performance are also described.

  19. Radiation depolymerization of chitosan to prepare oligomers

    International Nuclear Information System (INIS)

    Hai, Le; Bang Diep, Tran; Nagasawa, Naotsugu; Yoshii, Fumio; Kume, Tamikazu

    2003-01-01

    Radiation depolymerization of chitosan was carried out by gamma irradiation in the solid state. The radiation-chemical depolymerization yield of chitosan in the solid state, Gd, determined by gel permeation chromatography, is 0.9 for chitosan 10B and 1.8 for chitosan 8B. Low molecular weight chitosan/or oligochitosans were separated from a chitosan depolymerized by gamma radiation, using mixtures of methanol-water and acetone as the solvents. Due to the differences in solubility revealed upon radiolysis, extracts became subdivided into precipitates and soluble fractions. The biological effect of oligochitosan in each fraction was evaluated; the preliminary results indicated that the oligochitosan with M w -bar=2x10 4 inhibited the growth of fungi at 100 ppm and that with M w -bar=800 only enhanced the growth of the same typical fungi

  20. Synthesis, characterization, and biocompatible properties of alanine-grafted chitosan copolymers.

    Science.gov (United States)

    Park, Gyu Han; Kang, Min-Sil; Knowles, Jonathan C; Gong, Myoung-Seon

    2016-04-01

    In order to overcome major problems regarding the lack of affinity to solvents and limited reactivity of the free amines of chitosan, introduction of appropriate spacer arms having terminal amine function is considered of interest. L-Alanine-N-carboxyanhydride was grafted onto chitosan via anionic ring-opening polymerization. The chemical and structural characterizations of L-alanine-grafted chitosan (Ala-g-Cts) were confirmed through Fourier transform infrared spectroscopy and proton nuclear magnetic resonance spectroscopy ((1)H NMR). In addition, the viscoelastic properties of Ala-g-Cts were examined by means of a rotational viscometer, and thermal analysis was carried out with a thermogravimetric analyzer and differential scanning calorimetry. Morphological changes in the chitosan L-alanine moiety were determined by x-ray diffraction. To determine the feasibility of using these films as biomedical materials, we investigated the effects of their L-alanine content on physical and mechanical properties. The biodegradation results of crosslinked Ala-g-Cts films were evaluated in phosphate-buffered solution containing lysozyme at 37℃. Proliferation of MC3T3-E1 cells on crosslinked Ala-g-Cts films was also investigated with use of the CCK-8 assay. © The Author(s) 2016.

  1. Extraction and Characterization of Chitin and Chitosan from Blue Crab and Synthesis of Chitosan Cryogel Scaffolds

    Directory of Open Access Journals (Sweden)

    Nimet Bölgen

    2016-08-01

    Full Text Available Polymeric scaffolds produced by cryogelation technique have attracted increasing attention for tissue engineering applications. Cryogelation is a technique which enables to produce interconnected porous matrices from the frozen reaction mixtures of polymers or monomeric precursors. Chitosan is a biocompatible, biodegradable, nontoxic, antibacterial, antioxidant and antifungal natural polymer that is obtained by deacetylation of chitin, which is mostly found in the exoskeleton of many crustacean. In this study, chitin was isolated from the exoskeleton of blue crap (Callinectes sapidus using a chemical method. Callinectes sapidus samples were collected from a market, as a waste material after it has been consumed as food. Demineralization, deproteinization and decolorization steps were applied to the samples to obtain chitin. Chitosan was prepared from isolated chitin by deacetylation at high temperatures. The chemical compositon of crab shell, extracted chitin and chitosan were characterized with FTIR analyses. And also to determine the physicochemical and functional properties of the produced chitosan; solubility, water binding and fat binding analysis were performed. Chitosan cryogel scaffolds were prepared by crosslinking reaction at cryogenic conditions at constant amount of chitosan (1%, w/v with different ratios of glutaraldehyde (1, 3, and 6%, v/v as crosslinker. The chemical structure of the scaffolds were examined by FTIR. Also, the water uptake capacity of scaffolds have been determined. Collectively, the results suggested that the characterized chitosan cryogels can be potential scaffolds to be used in tissue engineering applications.

  2. Aging phenomena of chitosan and chitosan-diclofenac sodium system detected by low-frequency dielectric spectroscopy.

    Science.gov (United States)

    Bodek, K H; Bak, G W

    1999-09-01

    The use of natural polymers for design of dosage form has received considerable attention recently, especially from the safety point of view. Among these polymers, chitosan shows very interesting biological, chemical and physical properties which makes it possible to use chitosan for various pharmaceutical applications. Microcrystalline chitosan (MCCh) is a special multifunctional polymeric material existing in the form of either of gelatinous water dispersion or a powder. Thermal aging of chitosan and chitosan-diclofenac sodium mixture have been studied using low-frequency dielectric measurements. The aging was carried out by annealing in ambient atmosphere in the temperature range between 25 degrees C and 100 degrees C. The dielectric losses in the aged samples proved to decrease by about one order of magnitude. The additional measurements of molecular weight distribution and infrared absorption were also carried out for better understanding of nature of the ageing phenomena. Partial evacuation of water, cross-linking and improvement of structural order may be suggested to be a result of thermal aging of the investigated materials.

  3. Borax methylene blue: a spectroscopic and staining study.

    Science.gov (United States)

    Donaldson, P T; Russo, A; Reynolds, C; Lillie, R D

    1978-07-01

    Borax methylene blue is quite stable at room temperatures of 22-25 C. At 30 C polychroming is slow; during 50 days in a water bath at this temperature the absorption peak moves from 665 to 656 nm. At 35 C, the absorption peak reaches 660 nm in 7 days, 654 nm in 14. At 60 C polychroming is rapid, the absorption peak reaching 640-620 nm in 3 days. When the pH of the borax methylene blue solutions, normally about 9.0, is adjusted to pH 6.5, the absorption peak remains at 665 nm even when incubated at 60 C for extended periods. When used as a blood stain 0.4 ml borax methylene blue (1% methylene blue in 1% borax), 4 ml acetone, 2 ml borax-acid phosphate buffer to bring the solution to pH 6.5, and distilled water to make 40 ml, with 0.2 ml 1% eosin added just before using, an excellent Nocht-Giemsa type stain is achieved after 30 minutes staining. The material plasmodia P. falciparum, P. vivax, and P. berghei stain moderate blue with dark red chromatin and green to black pigment granules. The study confirms Malachowski's 1891 results and explains Gautier's 1896-98 failure to duplicate it.

  4. Application of irradiated chitosan for fruit preservation

    Energy Technology Data Exchange (ETDEWEB)

    Lan, K.N. [Post-harvest Technology Institute, 4, Ngo Quyen-Ha Noi (Viet Nam); Lam, N.D. [Ha Noi Radiation Center, VAEC, 5T-160, Nghiado, Tuliem, Ha Noi (Viet Nam); Kume, Tamikazu [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment

    2000-03-01

    Preliminary test of mango (Mangifera indica) preservation by irradiated chitosan coating has been investigated. The coating by using irradiated chitosan in 1.5% solution has extended the shelf life of mango from 7 to 15 days. At the 15th day mango coated by irradiated chitosan has been keeping good color, natural ripening, without spoilage, weight loss 10%, whereas the mango without coating was spoiled completely and the coating of fruit with unirradiated chitosan inhibited the ripening. (author)

  5. Application of irradiated chitosan for fruit preservation

    International Nuclear Information System (INIS)

    Lan, K.N.; Lam, N.D.; Kume, Tamikazu

    2000-01-01

    Preliminary test of mango (Mangifera indica) preservation by irradiated chitosan coating has been investigated. The coating by using irradiated chitosan in 1.5% solution has extended the shelf life of mango from 7 to 15 days. At the 15th day mango coated by irradiated chitosan has been keeping good color, natural ripening, without spoilage, weight loss 10%, whereas the mango without coating was spoiled completely and the coating of fruit with unirradiated chitosan inhibited the ripening. (author)

  6. Preparation of alginate coated chitosan microparticles for vaccine delivery

    Directory of Open Access Journals (Sweden)

    Wei YuQuan

    2008-11-01

    Full Text Available Abstract Background Absorption of antigens onto chitosan microparticles via electrostatic interaction is a common and relatively mild process suitable for mucosal vaccine. In order to increase the stability of antigens and prevent an immediate desorption of antigens from chitosan carriers in gastrointestinal tract, coating onto BSA loaded chitosan microparticles with sodium alginate was performed by layer-by-layer technology to meet the requirement of mucosal vaccine. Results The prepared alginate coated BSA loaded chitosan microparticles had loading efficiency (LE of 60% and loading capacity (LC of 6% with mean diameter of about 1 μm. When the weight ratio of alginate/chitosan microparticles was greater than 2, the stable system could be obtained. The rapid charge inversion of BSA loaded chitosan microparticles (from +27 mv to -27.8 mv was observed during the coating procedure which indicated the presence of alginate layer on the chitosan microparticles surfaces. According to the results obtained by scanning electron microscopy (SEM, the core-shell structure of BSA loaded chitosan microparticles was observed. Meanwhile, in vitro release study indicated that the initial burst release of BSA from alginate coated chitosan microparticles was lower than that observed from uncoated chitosan microparticles (40% in 8 h vs. about 84% in 0.5 h. SDS-polyacrylamide gel electrophoresis (SDS-PAGE assay showed that alginate coating onto chitosan microparticles could effectively protect the BSA from degradation or hydrolysis in acidic condition for at least 2 h. The structural integrity of alginate modified chitosan microparticles incubated in PBS for 24 h was investigated by FTIR. Conclusion The prepared alginate coated chitosan microparticles, with mean diameter of about 1 μm, was suitable for oral mucosal vaccine. Moreover, alginate coating onto the surface of chitosan microparticles could modulate the release behavior of BSA from alginate coated chitosan

  7. Rheological study of chitosan acetate solutions containing chitin nanofibrils

    Czech Academy of Sciences Publication Activity Database

    Mikešová, Jana; Hašek, Jindřich; Tishchenko, Galina; Morganti, P.

    2014-01-01

    Roč. 112, 4 November (2014), s. 753-757 ISSN 0144-8617 EU Projects: European Commission(XE) 315233 - N-CHITOPACK Institutional support: RVO:61389013 Keywords : rheology * chitosan solutions * chitin nanofibrils Subject RIV: CD - Macromolecular Chemistry Impact factor: 4.074, year: 2014

  8. Chitosan-nanosilica hybrid materials: Preparation and properties

    International Nuclear Information System (INIS)

    Podust, T.V.; Kulik, T.V.; Palyanytsya, B.B.; Gun’ko, V.M.; Tóth, A.; Mikhalovska, L.; Menyhárd, A.; László, K.

    2014-01-01

    Highlights: • Hybrid chitosan-nanosilica materials were synthesized using an adsorption modification method. • The chitosan adsorption capacity is higher on the silica/titania and silica/alumina than on the fumed silica. • Nanosilicas undergo structural and textural alterations due to modification by chitosan. • The more severe chitosan thermodestruction occurs on the silica/titania and silica/alumina surfaces than on the plain silica surface. - Abstract: The research focuses on the synthesis of novel organic–inorganic hybrid materials based on polysaccharide chitosan and nanosilicas (SiO 2 , TiO 2 /SiO 2 and Al 2 O 3 /SiO 2 ). The chitosan modified nanooxides were obtained by the equilibrium adsorption method. The chitosan adsorption capacities of silica/titania and silica/alumina are higher than of the plain silica due to the additional active sites present on the surfaces of the mixed oxides. The hybrid materials were characterized by low-temperature nitrogen adsorption/desorption, photon correlation spectroscopy (PCS), scanning electron microscopy (SEM), thermogravimetry (TG/DTG) and temperature-programmed desorption with mass spectrometry control (TPD MS) methods. The chitosan treatment only modestly influences the surface area S BET of the nanooxides but the rearrangement of the secondary and tertiary structures (aggregates and agglomerates) results in an enhancement of the mesoporosity and affects the size of the aggregates. The more severe thermodestruction of the polysaccharide desorbing from the modified mixed silicas indicates a stronger interaction between the chitosan and the mixed oxides compared to the silanol groups of the plain silica surface

  9. Chitosan-nanosilica hybrid materials: Preparation and properties

    Energy Technology Data Exchange (ETDEWEB)

    Podust, T.V., E-mail: tania_list@yahoo.com [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Kulik, T.V., E-mail: tanyakulyk@i.ua [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Palyanytsya, B.B.; Gun’ko, V.M. [Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kyiv 03164 (Ukraine); Tóth, A. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary); Mikhalovska, L. [School of Pharmacy and Biomolecular Sciences, University of Brighton, Lewes Road, Brighton BN2 4GJ (United Kingdom); Menyhárd, A. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary); Institute of Materials Science and Environmental Chemistry, Research Centre for Natural Sciences, Hungarian Academy of Sciences (Hungary); László, K. [Department of Physical Chemistry and Material Science, Budapest University of Technology and Economics, H-1521 Budapest (Hungary)

    2014-11-30

    Highlights: • Hybrid chitosan-nanosilica materials were synthesized using an adsorption modification method. • The chitosan adsorption capacity is higher on the silica/titania and silica/alumina than on the fumed silica. • Nanosilicas undergo structural and textural alterations due to modification by chitosan. • The more severe chitosan thermodestruction occurs on the silica/titania and silica/alumina surfaces than on the plain silica surface. - Abstract: The research focuses on the synthesis of novel organic–inorganic hybrid materials based on polysaccharide chitosan and nanosilicas (SiO{sub 2}, TiO{sub 2}/SiO{sub 2} and Al{sub 2}O{sub 3}/SiO{sub 2}). The chitosan modified nanooxides were obtained by the equilibrium adsorption method. The chitosan adsorption capacities of silica/titania and silica/alumina are higher than of the plain silica due to the additional active sites present on the surfaces of the mixed oxides. The hybrid materials were characterized by low-temperature nitrogen adsorption/desorption, photon correlation spectroscopy (PCS), scanning electron microscopy (SEM), thermogravimetry (TG/DTG) and temperature-programmed desorption with mass spectrometry control (TPD MS) methods. The chitosan treatment only modestly influences the surface area S{sub BET} of the nanooxides but the rearrangement of the secondary and tertiary structures (aggregates and agglomerates) results in an enhancement of the mesoporosity and affects the size of the aggregates. The more severe thermodestruction of the polysaccharide desorbing from the modified mixed silicas indicates a stronger interaction between the chitosan and the mixed oxides compared to the silanol groups of the plain silica surface.

  10. Gamma sterilization of diclofenac sodium loaded- N-trimethyl chitosan nanoparticles for ophthalmic use.

    Science.gov (United States)

    Asasutjarit, Rathapon; Theerachayanan, Thitaree; Kewsuwan, Prartana; Veeranondha, Sukitaya; Fuongfuchat, Asira; Ritthidej, Garnpimol C

    2017-02-10

    This study was conducted to investigate the effect of gamma irradiation on physicochemical properties of N-trimethyl chitosan (TMC), diclofenac sodium (DC) and diclofenac sodium loaded N-trimethylchitosan nanoparticles (DC-TMCNs), and to determine suitable doses of gamma rays for sterilization of DC-TMCNs. Physicochemical properties of TMC, DC and DC-TMCNs before and after exposure to gamma rays at various doses were investigated. It was found that gamma irradiation at doses of 5-25kGy did not cause any significant changes in physical and chemical properties of TMC, DC and DC-TMCNs. The bioburden of DC-TMCNs was 1.5×10 6 CFU/vial. The initial contaminating bacteria were radiosensitive bacteria. A number of microorganisms was reduced to 10 -6 after exposure to 9.9kGy of gamma rays. Therefore, DC-TMCNs could be sterilized by gamma irradiation at a dose of 10kGy, which did not alter their physicochemical properties and did not produce any substances toxic to the eye. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Regioselective Sequential Modification of Chitosan via Azide-Alkyne Click Reaction: Synthesis, Characterization, and Antimicrobial Activity of Chitosan Derivatives and Nanoparticles

    Science.gov (United States)

    Sarwar, Atif; Katas, Haliza; Samsudin, Siti Noradila; Zin, Noraziah Mohamad

    2015-01-01

    Recently, the attention of researchers has been drawn toward the synthesis of chitosan derivatives and their nanoparticles with enhanced antimicrobial activities. In this study, chitosan derivatives with different azides and alkyne groups were synthesized using click chemistry, and these were further transformed into nanoparticles by using the ionotropic gelation method. A series of chitosan derivatives was successfully synthesized by regioselective modification of chitosan via an azide-alkyne click reaction. The amino moieties of chitosan were protected during derivatization by pthaloylation and subsequently unblocked at the end to restore their functionality. Nanoparticles of synthesized derivatives were fabricated by ionic gelation to form complexes of polyanionic penta-sodium tripolyphosphate (TPP) and cationic chitosan derivatives. Particle size analysis showed that nanoparticle size ranged from 181.03 ± 12.73 nm to 236.50 ± 14.32 nm and had narrow polydispersity index and positive surface charge. The derivatives and corresponding nanoparticles were evaluated in vitro for antibacterial and antifungal activities against three gram-positive and gram-negative bacteria and three fungal strains, respectively. The minimum inhibitory concentration (MIC) of all derivatives ranged from 31.3 to 250 µg/mL for bacteria and 188 to1500 µg/mL for fungi and was lower than that of native chitosan. The nanoparticles with MIC ranging from 1.56 to 25 µg/mLfor bacteria and 94 to 750 µg/mL for fungi exhibited higher activity than the chitosan derivatives. Chitosan O-(1-methylbenzene) triazolyl carbamate and chitosan O-(1-methyl phenyl sulfide) triazolyl carbamate were the most active against the tested bacterial and fungal strains. The hemolytic assay on erythrocytes and cell viability test on two different cell lines (Chinese hamster lung fibroblast cells V79 and Human hepatic cell line WRL68) demonstrated the safety; suggesting that these derivatives could be used in future

  12. A facile modification of g-C{sub 3}N{sub 4} with enhanced photocatalytic activity for degradation of methylene blue

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Fei, E-mail: feichang@usst.edu.cn [School of Environment and Architecture, University of Shanghai for Science and Technology, Shanghai 200093 (China); Xie, Yunchao; Li, Chenlu; Chen, Juan; Luo, Jieru [School of Environment and Architecture, University of Shanghai for Science and Technology, Shanghai 200093 (China); Hu, Xuefeng, E-mail: xfhu@yic.ac.cn [Key Laboratory of Coastal Zone Environmental Processes and Ecological Remediation, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai, Shandong 264003 (China); Shen, Jiaowen [School of Urban Development and Environmental Engineering, Shanghai Second Polytechnic University, Shanghai 201209 (China)

    2013-09-01

    In this investigation, a facile modification of g-C{sub 3}N{sub 4} through co-pyrolysis of melamine and sodium nitrate or potassium nitrate was reported and the as-synthesized samples were characterized by a collection of techniques, such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy, UV–vis diffuse reflectance spectroscopy, nitrogen adsorption–desorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and elemental analysis. Based upon the analysis, we speculated that the g-C{sub 3}N{sub 4} framework was partially destroyed to produce cyano-containing fragments, which resulted into the variation of physical and optical properties, further affecting the adsorption and photocatalytic performance of g-C{sub 3}N{sub 4} on the dye methylene blue. Furthermore, we found that nitrate anions rather than sodium or potassium ions had important effect on the structure and photocatalytic performance of g-C{sub 3}N{sub 4}. In addition, the photocatalysis mechanism and reusability test were also investigated and discussed in the study.

  13. New sizing agents and flocculants derived from chitosan

    International Nuclear Information System (INIS)

    Hebeish, A.; Higay, A.; El-Shafei, A.

    2005-01-01

    Novel approaches for development of new textile sizing agents and flocculants were undertaken. One of these approaches is based on acid hydrolysis of chitosan and the other involves its carboxy methylation. Characterization of the hydrolyzed chitosan was performed through monitoring nitrogen content and apparent viscosity, while carboxymethyl chitosan was analyzed for degree of substitution (DS) along with apparent viscosity. Factors affecting both hydrolysis and carboxy methylation were investigated. The nitrogen content and apparent viscosity of chitosan decrease variably by increasing HCl concentration as well as time and temperature of hydrolysis. On the other hand, the DS of carboxymethyl chitosan increases by increasing the concentration of both sodium hydroxide and monochloroacetic acid and similarly increases by prolonging the duration and raising the temperature of carboxy methylation; in contrast with apparent viscosity which is inversely related to these parameters. Aqueous solutions of hydrolyzed chitosan or carboxymethyl chitosan were applied to light cotton fabric with a view to envision the technical feasibility of such water soluble chitosan for textile sizing. The size add-on on the light fabric is directly related to the concentration of the hydrolyzed or carboxymethyl chitosan in the sizing solution and so does the apparent viscosity of the latter. Hundred percent size removals could be achieved with the hydrolyzed chitosan irrespective or the size solution concentration provided that the latter is not less than 8%. Different situation is encountered with carboxymethyl chitosan where the percent size removal increase from 81% to 95% by increasing its concentration in the sizing solution from 5 % to 15%. Drying the sized fabric at 80 degree C for 5 minutes or 120 degree C for 3 minutes has practically no effect on percent size removal. The same holds true for heat treatment of the sized fabric at higher temperatures (up to 160 degree C) for longer

  14. Effect of gamma radiation on the mechanical and barrier properties of HEMA grafted chitosan-based films

    International Nuclear Information System (INIS)

    Khan, Avik; Huq, Tanzina; Khan, Ruhul A.; Dussault, Dominic; Salmieri, Stephane; Lacroix, Monique

    2012-01-01

    Chitosan films were prepared by dissolving 1% (w/v) chitosan powder in 2% (w/v) aqueous acetic acid solution. Chitosan films were prepared by solution casting. The values of puncture strength (PS), viscoelasticity coefficient and water vapor permeability (WVP) of the films were found to be 565 N/mm, 35%, and 3.30 g mm/m 2 day kPa, respectively. Chitosan solution was exposed to gamma irradiation (0.1–5 kGy) and it was revealed that PS values were reduced significantly (p≤0.05) after 1 kGy dose and it was not possible to form films after 5 kGy. Monomer, 2-hydroxyethyl methacrylate (HEMA) solution (0.1–1%, w/v) was incorporated into the chitosan solution and the formulation was exposed to gamma irradiation (0.3 kGy). A 0.1% (w/v) HEMA concentration at 0.3 kGy dose was found optimal-based on PS values for chitosan grafting. Then radiation dose (0.1–5 kGy) was optimized for HEMA grafting. The highest PS values (672 N/mm) were found at 0.7 kGy. The WVP of the grafted films improved significantly (p≤0.05) with the rise of radiation dose. - highlights: ► HEMA and Silane monomer were incorporated into the MC-based formulation and films. ► Films were exposed to gamma radiation. ► HEMA containing films showed the highest PS values. ► Surface morphology of the grafted films suggested better appearance.

  15. Surface functionalization of detonation nanodiamonds by phosphonic dichloride derivatives.

    Science.gov (United States)

    Presti, Charlene; Alauzun, Johan G; Laurencin, Danielle; Mutin, P Hubert

    2014-08-05

    A new method for the functionalization of detonation nanodiamonds (DNDs) is proposed, on the basis of surface modification with phosphonic dichloride derivatives. DNDs were first modified by phenylphosphonic dichloride, and the grafting modes and hydrolytic stability under neutral conditions were investigated using (1)H, (13)C, and (31)P solid state NMR spectroscopy, Fourier transform infrared spectroscopy, as well as elemental analysis. Then, in order to illustrate the possibilities offered by this method, DNDs functionalized by mesityl imidazolium groups were obtained by postmodification of DNDs modified by 12-bromododecylphosphonic dichloride. The oxidative thermal stability of the functionalized DNDs was investigated using thermogravimetric analysis.

  16. Preparations, properties and applications of chitosan based nanofibers fabricated by electrospinning

    Directory of Open Access Journals (Sweden)

    2011-04-01

    Full Text Available Chitosan is soluble in most acids. The protonation of the amino groups on the chitosan backbone inhibits the electrospinnability of pure chitosan. Recently, electrospinning of nanofibers based on chitosan has been widely researched and numerous nanofibers containing chitosan have been prepared by decreasing the number of the free amino groups of chitosan as the nanofibiers have enormous possibilities for better utilization in various areas. This article reviews the preparations and properties of the nanofibers which were electrospun from pure chitosan, blends of chitosan and synthetic polymers, blends of chitosan and protein, chitosan derivatives, as well as blends of chitosan and inorganic nanoparticles, respectively. The applications of the nanofibers containing chitosan such as enzyme immobilization, filtration, wound dressing, tissue engineering, drug delivery and catalysis are also summarized in detail.

  17. Effect of enzymatic degradation of chitosan in polyhydroxybutyrate/chitosan/calcium phosphate composites on in vitro osteoblast response.

    Science.gov (United States)

    Giretova, Maria; Medvecky, Lubomir; Stulajterova, Radoslava; Sopcak, Tibor; Briancin, Jaroslav; Tatarkova, Monika

    2016-12-01

    Polyhydroxybutyrate/chitosan/calcium phosphate composites are interesting biomaterials for utilization in regenerative medicine and they may by applied in reconstruction of deeper subchondral defects. Insufficient informations were found in recent papers about the influence of lysozyme degradation of chitosan in calcium phosphate/chitosan based composites on in vitro cytotoxicity and proliferation activity of osteoblasts. The effect of enzymatic chitosan degradation on osteoblasts proliferation was studied on composite films in which the porosity of origin 3D scaffolds was eliminated and the surface texture was modified. The significantly enhanced proliferation activity with faster population growth of osteoblasts were found on enzymatically degraded biopolymer composite films with α-tricalcium phosphate and nanohydroxyapatite. No cytotoxicity of composite films prepared from lysozyme degraded scaffolds containing a large fraction of low molecular weight chitosans (LMWC), was revealed after 10 days of cultivation. Contrary to above in the higher cytotoxicity origin untreated nanohydroxyapatite films and porous composite scaffolds. The results showed that the synergistic effect of surface distribution, morphology of nanohydroxyapatite particles, microtopography and the presence of LMWC due to chitosan degradation in composite films were responsible for compensation of the cytotoxicity of nanohydroxyapatite composite films or porous composite scaffolds.

  18. Maillard reaction products from chitosan-xylan ionic liquid solution.

    Science.gov (United States)

    Luo, Yuqiong; Ling, Yunzhi; Wang, Xiaoying; Han, Yang; Zeng, Xianjie; Sun, Runcang

    2013-10-15

    A facile method is reported to prepare Maillard reaction products (MRPs) from chitosan and xylan in co-solvent ionic liquid. UV absorbance and fluorescence changes were regarded as indicators of the occurrence of Maillard reaction. FT-IR, NMR, XRD and TG were used to investigate the structure of chitosan-xylan conjugate. The results revealed that when chitosan reacted with xylan in ionic liquid, the hydrogen bonds in chitosan were destroyed, the facts resulted in the formation of chitosan-xylan MRPs. Moreover, when the mass ratio of chitosan to xylan was 1:1, the Maillard reaction proceeded easily. In addition, relatively high antioxidant property was also noted for the chitosan-xylan conjugate with mass ratio 1:1. So the obtained chitosan-xylan MRP is a promising antioxidant agent for food industry. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Chitosan: A potential biopolymer for wound management.

    Science.gov (United States)

    Bano, Ijaz; Arshad, Muhammad; Yasin, Tariq; Ghauri, Muhammad Afzal; Younus, Muhammad

    2017-09-01

    It has been seen that slow healing and non-healing wounds conditions are treatable but still challenging to humans. Wound dressing usually seeks for biocompatible and biodegradable recipe. Natural polysaccharides like chitosan have been examined for its antimicrobial and healing properties on the basis of its variation in molecular weight and degree of deacetylation. Chitosan adopts some vital characteristics for treatment of various kinds of wounds which include its bonding nature, antifungal, bactericidal and permeability to oxygen. Chitosan therefore has been modified into various forms for the treatment of wounds and burns. The purpose of this review article is to understand the exploitation of chitosan and its derivatives as wound dressings. This article will also provide a concise insight on the properties of chitosan necessary for skin healing and regeneration, particularly highlighting the emerging role of chitosan films as next generation skin substitutes for the treatment of full thickness wounds. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Molecular interactions in gelatin/chitosan composite films.

    Science.gov (United States)

    Qiao, Congde; Ma, Xianguang; Zhang, Jianlong; Yao, Jinshui

    2017-11-15

    Gelatin and chitosan were mixed at different mass ratios in solution forms, and the rheological properties of these film-forming solutions, upon cooling, were studied. The results indicate that the significant interactions between gelatin and chitosan promote the formation of multiple complexes, reflected by an increase in the storage modulus of gelatin solution. Furthermore, these molecular interactions hinder the formation of gelatin networks, consequently decreasing the storage modulus of polymer gels. Both hydrogen bonds and electrostatic interactions are formed between gelatin and chitosan, as evidenced by the shift of the amide-II bands of polymers. X-ray patterns of composite films indicate that the contents of triple helices decrease with increasing chitosan content. Only one glass transition temperature (T g ) was observed in composite films with different composition ratios, and it decreases gradually with an increase in chitosan proportion, indicating that gelatin and chitosan have good miscibility and form a wide range of blends. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Suppression of Zn stress on barley by irradiated chitosan

    Energy Technology Data Exchange (ETDEWEB)

    Nagasawa, N.; Mitomo, H. [Gunma Univ., Faculty of Engineering, Department of Biological and Chemical Engineering, Kiryu, Gunma (Japan); Ha, P.T.L. [Nuclear Research Institute, Dalat (Viet Nam); Watanabe, S.; Ito, T.; Takeshita, H.; Yoshii, F.; Kume, T. [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment

    2001-03-01

    Chitosan was irradiated up to 1000 kGy in solid state. Irradiation of chitosan caused the reduction of molecular weight. The molecular weight of the chitosan reduced from ca. 4 x 10{sup 5} to ca. 6 x 10{sup 3} by irradiation at 1000 kGy. For the barley growth promotion, irradiated chitosan showed the significant effect and 1000 kGy irradiated chitosan improved 20% of growth. Using the positron emitting tracer imaging system (PETIS), the effect of chitosan on uptake and transportation of {sup 62}Zn in barley were investigated. It was found that the transportation of Zn from root to shoot and the damage of plant by Zn were suppressed with irradiated chitosan. (author)

  2. Chitosan Fibers Modified with HAp/β–TCP Nanoparticles

    Directory of Open Access Journals (Sweden)

    Dariusz Wawro

    2011-10-01

    Full Text Available This paper describes a method for preparing chitosan fibers modified with hydroxyapatite (HAp, tricalcium phosphate (β-TCP, and HAp/β-TCP nanoparticles. Fiber-grade chitosan derived from the northern shrimp (Pandalus borealis and nanoparticles of tricalcium phosphate (β-TCP and hydroxyapatite (HAp suspended in a diluted chitosan solution were used in the investigation. Diluted chitosan solution containing nanoparticles of Hap/β-TCP was introduced to a 5.16 wt% solution of chitosan in 3.0 wt% acetic acid. The properties of the spinning solutions were examined. Chitosan fibers modified with nanoparticles of HAp/β-TCP were characterized by a level of tenacity and calcium content one hundred times higher than that of regular chitosan fibers.

  3. Suppression of Zn stress on barley by irradiated chitosan

    International Nuclear Information System (INIS)

    Nagasawa, N.; Mitomo, H.; Ha, P.T.L.; Watanabe, S.; Ito, T.; Takeshita, H.; Yoshii, F.; Kume, T.

    2001-01-01

    Chitosan was irradiated up to 1000 kGy in solid state. Irradiation of chitosan caused the reduction of molecular weight. The molecular weight of the chitosan reduced from ca. 4 x 10 5 to ca. 6 x 10 3 by irradiation at 1000 kGy. For the barley growth promotion, irradiated chitosan showed the significant effect and 1000 kGy irradiated chitosan improved 20% of growth. Using the positron emitting tracer imaging system (PETIS), the effect of chitosan on uptake and transportation of 62 Zn in barley were investigated. It was found that the transportation of Zn from root to shoot and the damage of plant by Zn were suppressed with irradiated chitosan. (author)

  4. Electrochemical and Thermal Studies of Prepared Conducting Chitosan Biopolymer Film

    International Nuclear Information System (INIS)

    Hlaing Hlaing Oo; Kyaw Naing; Kyaw Myo Naing; Tin Tin Aye; Nyunt Wynn

    2005-09-01

    In this paper, chitosan based conducting bipolymer films were prepared by casting and solvent evaporating technique. All prepared chitosan films were of pale yellow colour, transparent, and smooth. Sulphuric acid was chosen as the cross-linking agent. It enhanced conduction pathway in cross-linked chitosan films. Mechanical properties, solid-state, and thermal behavior of prepared chitosan fimls were studied by means of a material testing machine, powder X-ray diffractometry (XRD), thermogravimetric analysis (TG-DTG), and differential scanning calorimetry (DSC). By the XRD diffraction pattern, high molecular weight of chitosan product indicates the semi-crystalline nature, but the prepared chitosan film and doped chitosan film indicate significantly lower in crystallinity prove which of the amorphous characteristics. In addition, DSC thermogram of pure chitosan film exhibited exothermic peak around at 300 C, indicating polymer decomposition of chitosan molecules in chitosan films. Furthermore, these DSC thermograms clearly showed that while pure chitosan film display exothermal decomposition, the doped chitosan films mainly endothermic characteristics. The ionic conductivity of doped chitosan films were in the order of 10 to 10 S cm , which is in the range of semi-conductor. These results showed that cross-linked chitoson films may be used as polymer electrolyte film to fabricate solid state electrochemical cells

  5. Synthesis and characterization of chitosan impregnated calcium alginate beads for removal of uranium from aquatic stream

    International Nuclear Information System (INIS)

    Singhal, R.K.; Basu, H.; Manisha, V.; Reddy, A.V.R.; Sawant, Manjiri; Kamane, Suman

    2015-01-01

    The present study was conducted to study the feasibility of chitosan impregnated calcium alginate beads (Cal-Alg-Chi) to sorb the excess uranium from the aquatic stream. Chitosan is a linear polysaccharide composed of randomly distributed β-(1-4)-linked D glucosamine (deacetylated unit) and N-acetyl-D-glucosamine (acetylated unit). The optimal composition of calcium alginate chitosan beads is 4 % (wt/vol) alginate gel having 5% loading of chitosan. The nature and morphology of pure and uranium sorbed calcium alginate chitosan beads were characterized by scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS), and attenuated total reflectance Fourier transform infrared spectroscopy (ATRFTIR). The results of batch sorption experiments suggest that Cal-Alg-Chi beads are very effective for removal of uranium in the pH range of 2.0-5.0 and sorption is more than 80 % in the concentration range of 1-100 mgL -1

  6. Some features of irradiated chitosan and its biological effect

    International Nuclear Information System (INIS)

    Hai, Le; Hien, Nguyen Quoc; Luan, Le Quang; Hanh, Truong Thi; Man, Nguyen Tan; Ha, Pham Thi Le; Thuy, Tran Thi; Yoshii, Fumio; Kume, Tamikazu

    2001-01-01

    Preparation of chitosan oligomer by radiation degradation was carried out on the gamma Co-60 source. The radiation degradation yield (G d ) of the chitosan was found to be of 1.03. The oligochitosan with 50% of dp>8 fraction was obtained by irradiating the 10% (w/v) chitosan solution in 5% acetic acid at 45 kGy for the chitosan having the initial viscometric average molecular weight, Mv=60,000. Irradiated chitosan showed higher antifungal effect than that of unirradiated one. Furthermore, the irradiated chitosan also showed the growth-promotion effect for plants. (author)

  7. Mucoadhesive properties and interaction with P-glycoprotein (P-gp) of thiolated-chitosans and -glycol chitosans and corresponding parent polymers: a comparative study.

    Science.gov (United States)

    Trapani, Adriana; Palazzo, Claudio; Contino, Marialessandra; Perrone, Maria Grazia; Cioffi, Nicola; Ditaranto, Nicoletta; Colabufo, Nicola Antonio; Conese, Massimo; Trapani, Giuseppe; Puglisi, Giovanni

    2014-03-10

    The aim of the present work was to compare the mucoadhesive and efflux pump P-glycoprotein (P-gp) interacting properties of chitosan (CS)- and glycolchitosan (GCS)-based thiomers and corresponding unmodified parent polymers. For this purpose, the glycol chitosan-N-acetyl-cysteine (GCS-NAC) and glycol chitosan-glutathione (GCS-GSH) thiomers were prepared under simple and mild conditions. Their mucoadhesive characteristics were studied by turbidimetric and zeta potential measurements. The P-gp interacting properties were evaluated measuring the effects of thiolated- and unmodified-polymers on the bidirectional transport (BA/AB) of rhodamine-123 across Caco-2 cells as well as in the calcein-AM and ATPase activity assays. Although all the thiomers and unmodified polymers showed optimal-excellent mucoadhesive properties, the best mucoadhesive performances have been obtained by CS and CS-based thiomers. Moreover, it was found that the pretreatment of Caco-2 cell monolayer with GCS-NAC or GCS restores Rho-123 cell entrance by inhibiting P-gp activity. Hence, GCS-NAC and GCS may constitute new biomaterials useful for improving the bioavailability of P-gp substrates.

  8. [Sensitive determination of Bi3+ by spectrofluorimetry based on graphene oxide-methylene blue system].

    Science.gov (United States)

    Zhai, Qiu-ge; Guo, Peng; Zhou, Lin; Liu, Yan-ming

    2014-08-01

    Graphene oxide was prepared by the modified Hummers method and characterized by field emission scanning electron microscopy. The interaction of graphene with methylene blue was studied by UV absorption, the intensity of two main absorption peaks of methylene blue decreased significantly after the fluorescence was quenched, and the energy transfer didn't occur because the overlap of the absorption spectrum of GO and the emission spectrum of MB is too small. Therefore, the fluorescence quenching of MB and GO was static. When adding a certain amount of Bi3+ in the graphene-methylene blue system, Bi3+ replaces the methylene blue from the graphene-methylene blue complexes because Bi3+ has the smaller volume and is more positively charged. The methylene blue therefore dissociates from the GO-MB complexes, resulting in the recovery of fluorescence of the system. Furthermore, the fluorescence of the system increases with the increase in the amount of Bi3+ due to the enhanced amount of MB in the system. A novel spectrofluorimetric method was therefore developed for the sensitive determination of Bi3+. Some parameters including the concentration of methylene blue, the amount of graphene oxide, the amount of nitric acid and the sequence of reagent adding were optimized to obtain higher sensitivity. The fluorescence of the system was detected at an emission wavelength of 667 nm with excitation at 690 nm. Under the optimized conditions, the concentration of Bi3+ showed good linear relationships with the fluorescence intensity in the range of 0.5-100 micromol x L(-1), with correlation coefficients of r = 0.9955. The limits of detection for Bi3+ was 1.0 x 10(-8) mol x L(-1) (S/N=3). The selectivity of the proposed method was evaluated and the results showed that 1000-fold K+, Ca+, Na+, Mg2+, Cu2+; 100-fold Fe3+, Be2+, SiO2- Al3+, Ni2+, Sb3+, NO3-, Cl-, F-, and 20-fold Pb2+, Hg2+, Cd2+ had negligible interference with the determination of Bi3+. The method has advantages of

  9. Modified methylene blue injection improves lymph node harvest in rectal cancer.

    Science.gov (United States)

    Liu, Jianpei; Huang, Pinjie; Zheng, Zongheng; Chen, Tufeng; Wei, Hongbo

    2017-04-01

    The presence of nodal metastases in rectal cancer plays an important role in accurate staging and prognosis, which depends on adequate lymph node harvest. The aim of this prospective study is to investigate the feasibility and survival benefit of improving lymph node harvest by a modified method with methylene blue injection in rectal cancer specimens. One hundred and thirty-one patients with rectal cancer were randomly assigned to the control group in which lymph nodes were harvested by palpation and sight, or to the methylene blue group using a modified method of injection into the superior rectal artery with methylene blue. Analysis of clinicopathologic records, including a long-term follow-up, was performed. In the methylene blue group, 678 lymph nodes were harvested by simple palpation and sight. Methylene blue injection added 853 lymph nodes to the total harvest as well as 32 additional metastatic lymph nodes, causing a shift to node-positive stage in four patients. The average number of lymph nodes harvested was 11.7 ± 3.4 in the control group and 23.2 ± 4.7 in the methylene blue group, respectively. The harvest of small lymph nodes (rectal cancer, especially small node and metastatic node retrieval, which provided more accurate staging. However, it was not associated with overall survival. © 2014 Royal Australasian College of Surgeons.

  10. X-ray diffraction studies of chitosan acetate-based polymer electrolytes

    International Nuclear Information System (INIS)

    Osman, Z.; Ibrahim, Z.A.; Abdul Kariem Arof

    2002-01-01

    Chitosan is the product when partially deacetylated chitin dissolves in dilute acetic acid. This paper presents the x-ray diffraction patterns of chitosan acetate, plasticised chitosan acetate and plasticised-salted chitosan acetate films. The results show that the chitosan acetate based polymer electrolyte films are not completely amorphous but it is partially crystalline. X-ray diffraction study also confirms the occurrence of the complexation between chitosan and the salt and the interaction between salt and plasticizer. The salt-chitosan interaction is clearly justified by infrared spectroscopy. (Author)

  11. FT-IR studies on interactions among components in hexanoyl chitosan-based polymer electrolytes

    Science.gov (United States)

    Winie, Tan; Arof, A. K.

    2006-03-01

    Fourier transform infrared (FT-IR) spectroscopic studies have been undertaken to investigate the interactions among components in a system of hexanoyl chitosan-lithium trifluoromethanesulfonate (LiCF 3SO 3)-diethyl carbonate (DEC)/ethylene carbonate (EC). LiCF 3SO 3 interacts with the hexanoyl chitosan to form a hexanoyl chitosan-salt complex that results in the shifting of the N(COR) 2, C dbnd O sbnd NHR and OCOR bands to lower wavenumbers. Interactions between EC and DEC with LiCF 3SO 3 has been noted and discussed. Evidence of interaction between EC and DEC has been obtained experimentally. Studies on polymer-plasticizer spectra suggested that there is no interaction between the polymer host and plasticizers. Competition between plasticizer and polymer on associating with Li + ions was observed from the spectral data for gel polymer electrolytes. The obtained spectroscopic data has been correlated with the conductivity performance of hexanoyl chitosan-based polymer electrolytes.

  12. Determination of the Optimum Conditions for Production of Chitosan Nanoparticles

    Directory of Open Access Journals (Sweden)

    A. Dustgani

    2007-12-01

    Full Text Available Bioedegradable nanoparticles are intensively investigated for their potential applications in drug delivery systems. Being a biocompatible and biodegradable polymer, chitosan holds great promise for use in this area. This investigation was concerned with determination and optimization of the effective parameters involved in the production of chitosan nanoparticles using ionic gelation method. Studied variables were concentration and pH of the chitosan solution, the ratio of chitosan to sodium tripolyphosphate therein and the molecular weight of chitosan. For this purpose, Taguchistatistical method was used for design of experiments in three levels. The size of chitosan nanoparticle was determined using laser light scattering. The experimental results showed that concentration of chitosan solution was the most important parameter and chitosan molecular weight the least effective parameter. The optimum conditions for preparation of nanoparticles were found to be 1 mg/mL chitosan solution with pH=5, chitosan to sodium tripolyphosphate ratio of 3 and chitosan molecular weight of 200,000 daltons. The average nanoparticle size at optimum conditions was found to be about 150 nm.

  13. In vitro osteoclastogenesis on textile chitosan scaffold

    Directory of Open Access Journals (Sweden)

    C Heinemann

    2010-02-01

    Full Text Available Textile chitosan fibre scaffolds were evaluated in terms of interaction with osteoclast-like cells, derived from human primary monocytes. Part of the scaffolds was further modified by coating with fibrillar collagen type I in order to make the surface biocompatible. Monocytes were cultured directly on the scaffolds in the presence of macrophage colony stimulating factor (M-CSF and receptor activator of nuclear factor kappaB ligand (RANKL for up to 18 days. Confocal laser scanning microscopy (CLSM as well as scanning electron microscopy (SEM revealed the formation of multinuclear osteoclast-like cells on both the raw chitosan fibres and the collagen-coated scaffolds. The modified surface supported the osteoclastogenesis. Differentiation towards the osteoclastic lineage was confirmed by the microscopic detection of cathepsin K, tartrate resistant acid phosphatase (TRAP, acidic compartments using 3-(2,4-dinitroanillino-3’-amino-N-methyldipropylamine (DAMP, immunological detection of TRAP isoform 5b, and analysis of gene expression of the osteoclastic markers TRAP, cathepsin K, vitronectin receptor, and calcitonin receptor using reverse transcription-polymerase chain reaction (RT-PCR. The feature of the collagen-coated but also of the raw chitosan fibre scaffolds to support attachment and differentiation of human monocytes facilitates cell-induced material resorption – one main requirement for successful bone tissue engineering.

  14. Chitosan coating as an antibacterial surface for biomedical applications.

    Directory of Open Access Journals (Sweden)

    Mélanie D'Almeida

    Full Text Available A current public health issue is preventing post-surgical complications by designing antibacterial implants. To achieve this goal, in this study we evaluated the antibacterial activity of an animal-free chitosan grafted onto a titanium alloy.Animal-free chitosan binding on the substrate was performed by covalent link via a two-step process using TriEthoxySilylPropyl Succinic Anhydride (TESPSA as the coupling agent. All grafting steps were studied and validated by means of X-ray Photoelectron Spectroscopy (XPS, Time-of-Flight secondary ion mass spectrometry (ToF-SIMS analyses and Dynamic-mode Secondary Ion Mass Spectrometry (DSIMS. The antibacterial activity against Escherichia coli and Staphylococcus aureus strains of the developed coating was assessed using the number of colony forming units (CFU.XPS showed a significant increase in the C and N atomic percentages assigned to the presence of chitosan. A thick layer of polymer deposit was detected by ToF-SIMS and the results obtained by DSIMS measurements are in agreement with ToF-SIMS and XPS analyses and confirms that the coating synthesis was a success. The developed coating was active against both gram negative and gram positive tested bacteria.The success of the chitosan immobilization was proven using the surface characterization techniques applied in this study. The coating was found to be effective against Escherichia coli and Staphylococcus aureus strains.

  15. Some features of irradiated chitosan and its biological effect

    Energy Technology Data Exchange (ETDEWEB)

    Hai, Le; Hien, Nguyen Quoc; Luan, Le Quang; Hanh, Truong Thi; Man, Nguyen Tan; Ha, Pham Thi Le; Thuy, Tran Thi [Nuclear Research Institute, VAEC, Dalat (Viet Nam); Yoshii, Fumio; Kume, Tamikazu [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment

    2001-03-01

    Preparation of chitosan oligomer by radiation degradation was carried out on the gamma Co-60 source. The radiation degradation yield (G{sub d}) of the chitosan was found to be of 1.03. The oligochitosan with 50% of dp>8 fraction was obtained by irradiating the 10% (w/v) chitosan solution in 5% acetic acid at 45 kGy for the chitosan having the initial viscometric average molecular weight, Mv=60,000. Irradiated chitosan showed higher antifungal effect than that of unirradiated one. Furthermore, the irradiated chitosan also showed the growth-promotion effect for plants. (author)

  16. Degree of Acetylization Chitosan Gonggong Snail Shells

    Science.gov (United States)

    Horiza, H.; Iskandar, I.; Aldo, N.

    2018-04-01

    Chitosan is a polysaccharide obtained from the deacetylation of chitin, which is generally derived from crustacean animal waste and animal skins other sea. One marine animals that have compounds that can be processed chitin chitosan is derived from the snail Gonggong marine waters of Riau Islands province. The purpose of this study was to determine the degree of chitosan from the shells of snails asetilisasi Gonggong. This research is an experimental research laboratory. The results of this study indicate that the degree of chitosan shell snail deasetilisasi Gonggong is 70.27%.

  17. Chitosan pretreatment for cotton dyeing with black tea

    Science.gov (United States)

    Campos, J.; Díaz-García, P.; Montava, I.; Bonet-Aracil, M.; Bou-Belda, E.

    2017-10-01

    Chitosan is used in a wide range of applications due to its intrinsic properties. Chitosan is a biopolymer obtained from chitin and among their most important aspects highlights its bonding with cotton and its antibacterial properties. In this study two different molecular weight chitosan are used in the dyeing process of cotton with black tea to evaluate its influence. In order to evaluate the effect of the pretreatment with chitosan, DSC and reflection spectrophotometer analysis are performed. The curing temperature is evaluated by the DSC analysis of cotton fabric treated with 15 g/L of chitosan, whilst the enhancement of the dyeing is evaluated by the colorimetric coordinates and the K/S value obtained spectrophotometrically. This study shows the extent of improvement of the pretreatment with chitosan in dyeing with natural products as black tea.

  18. Selective adsorption of silver(I) ions over copper(II) ions on a sulfoethyl derivative of chitosan.

    Science.gov (United States)

    Petrova, Yulia S; Pestov, Alexandr V; Usoltseva, Maria K; Neudachina, Ludmila K

    2015-12-15

    This study presents a simple and effective method of preparation of N-(2-sulfoethyl) chitosan (NSE-chitosan) that allows obtaining a product with a degree of modification up to 1.0. The chemical structure of the obtained polymers was confirmed by FT-IR and 1H NMR spectroscopies. Cross-linking of N-(2-sulfoethyl) chitosans by glutaraldehyde allows preparation of sorbents for removal and concentration of metal ions. Capacity of sorbents towards hydroxide ions was determined depending on the degree of sulfoethylation under static and dynamic conditions. Dissociation constants of functional amino groups of the analyzed sorbents were determined by potentiometric titration. It was shown that basicity of the amino groups decreased (wherein pKa decreased from 6.53 to 5.67) with increase in degree of sulfoethylation. It explains the significant influence of sulfo groups on selectivity of sorption of metal ions on N-(2-sulfoethyl) chitosan-based sorbents. The investigated substances selectively remove copper(II) and silver(I) ions from solutions of complex composition. Wherein the selectivity coefficient KAg/Cu increased to 20 (pH 6.5, ammonium acetate buffer solution) with increase in degree of sulfoethylation of the sorbent up to 1.0. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Swelling kinetics of spray-dried chitosan acetate assessed by magnetic resonance imaging and their relation to drug release kinetics of chitosan matrix tablets.

    Science.gov (United States)

    Huanbutta, Kampanart; Sriamornsak, Pornsak; Limmatvapirat, Sontaya; Luangtana-anan, Manee; Yoshihashi, Yasuo; Yonemochi, Etsuo; Terada, Katsuhide; Nunthanid, Jurairat

    2011-02-01

    Magnetic resonance imaging (MRI) was used to assess in situ swelling behaviors of spray-dried chitosan acetate (CSA) in 0.1N HCl, pH 6.8 and pH 5.0 Tris-HCl buffers. The in vitro drug releases from CSA matrix tablets containing the model drugs, diclofenac sodium and theophylline were investigated in all media using USP-4 apparatus. The effect of chitosan molecular weight, especially in pH 6.8 Tris-HCl, was also studied. In 0.1N HCl, the drug release from the matrix tablets was the lowest in relation to the highest swelling of CSA. The swelling kinetics in Tris-HCl buffers are Fickian diffusion according to their best fit to Higuchi's model as well as the drug release kinetics in all the media. The high swelling rate (k(s)(')) was found to delay the drug release rate (k'). The linear relationship between the swelling and fractions of drug release in Tris-HCl buffers was observed, indicating an important role of the swelling on controlling the drug release mechanism. Additionally, CSA of 200 and 800 kDa chitosan did not swell in pH 6.8 Tris-HCl but disintegrated into fractions, and the drug release from the matrix tablets was the highest. Copyright © 2010 Elsevier B.V. All rights reserved.

  20. Degradation of chitosan-based materials after different sterilization treatments

    International Nuclear Information System (INIS)

    San Juan, A; Montembault, A; Royaud, I; David, L; Gillet, D; Say, J P; Rouif, S; Bouet, T

    2012-01-01

    Biopolymers have received in recent years an increasing interest for their potential applications in the field of biomedical engineering. Among the natural polymers that have been experimented, chitosan is probably the most promising in view of its exceptional biological properties. Several techniques may be employed to sterilize chitosan-based materials. The aim of our study was to compare the effect of common sterilization treatments on the degradation of chitosan-based materials in various physical states: solutions, hydrogels and solid flakes. Four sterilization methods were compared: gamma irradiation, beta irradiation, exposure to ethylene oxide and saturated water steam sterilization (autoclaving). Exposure to gamma or beta irradiation was shown to induce an important degradation of chitosan, regardless of its physical state. The chemical structure of chitosan flakes was preserved after ethylene oxide sterilization, but this technique has a limited use for materials in the dry state. Saturated water steam sterilization of chitosan solutions led to an important depolymerization. Nevertheless, steam sterilization of chitosan flakes bagged or dispersed in water was found to preserve better the molecular weight of the polymer. Hence, the sterilization of chitosan flakes dispersed in water would represent an alternative step for the preparation of sterilized chitosan solutions. Alternatively, autoclaving chitosan physical hydrogels did not significantly modify the macromolecular structure of the polymer. Thus, this method is one of the most convenient procedures for the sterilization of physical chitosan hydrogels after their preparation.

  1. Humidity detection using chitosan film based sensor

    Science.gov (United States)

    Nasution, T. I.; Nainggolan, I.; Dalimunthe, D.; Balyan, M.; Cuana, R.; Khanifah, S.

    2018-02-01

    A humidity sensor made of the natural polymer chitosan has been successfully fabricated in the film form by a solution casting method. Humidity testing was performed by placing a chitosan film sensor in a cooling machine room, model KT-2000 Ahu. The testing results showed that the output voltage values of chitosan film sensor increased with the increase in humidity percentage. For the increase in humidity percentage from 30 to 90% showed that the output voltage of chitosan film sensor increased from 32.19 to 138.75 mV. It was also found that the sensor evidenced good repeatability and stability during the testing. Therefore, chitosan has a great potential to be used as new sensing material for the humidity detection of which was cheaper and environmentally friendly.

  2. Antifungal activity of low molecular weight chitosan produced from non-traditional marine resources

    Directory of Open Access Journals (Sweden)

    Francisco Pires Avelelas

    2014-06-01

    Full Text Available The four plants pathogens, Botrytis cinerea, Phytophthora cinnamomi, Cryphonectria parasitica and Heterobasidion annosum are responsible for several diseases affecting different plant species in Portugal, such as pines (H. annosum, chestnuts (P. cinnamomi and C. parasitica and eucalyptus (B. cinerea. These pathogens incurs in large economic losses, and ultimately causes the death of these plants. The use of biopolymers as antimicrobial agents, such as chitosan (derived from chitin, is increasing, in order to reduce the negative impact of conventional chemical treatments on the environment, avoiding health risks. Therefore, eco-friendly polymers were produced through (1 N-acetylation with addition of acetic anhydride and (2 hydrogen peroxide of chitosan samples, obtained from two different sources: shrimp (commercial chitosan and swimming crab bycatch specie Polybius henslowii. The chemical structure and molecular weight of the prepared chitosan derivatives, water soluble chitosan (WSC and chitooligosaccharides (COS, was confirmed by Fourier Transform Infrared (FT-IR and Gel Permeation Chromatography (GPC and their antifungal activity evaluated against Botrytis cinerea, Phytophthora cinnamomi, Cryphonectria parasitica and Heterobasidion annosum. The concentration range varied from 0.0125 to 0.1 mg/mL and inhibition percentages were determined by differences in radial growth on the agar plates for all species. Although not all species tested exhibited equal vulnerability towards the concentrations range, antifungal activity of chitosan samples proved to be dependent, increasing the inhibitory capacity with lower concentrations. The results obtained support the use of chitosan fromPolybius henslowii when compared with commercial chitosan with shrimp towards antifungal approaches, suggesting that chitin producers can rely on this crab waste as a raw material for chitin extraction, adding value to this bycatch specie. Financial support was obtained

  3. An Investigation of Chitosan for Sorption of Radionuclides

    Science.gov (United States)

    2012-06-05

    Valenta et al. found that hydrogels made of EDTA-chitsoan were resistant to bacterial growth [88]. Nishi et al. found that alka- line earth metals...reviews of chitosan deriva- tives have been recently published [8, 21, 75, 89]. 10 Table 2.1: Select applications of chitosan. From [72, 75]. Agriculture ...pharmaceuticals 2.1.3 Chitosan applications Chitosan has found applications in a wide range of fields, including agriculture , water treatment, biomedical

  4. Effects of sulfate chitosan derivatives on nonalcoholic fatty liver disease

    Science.gov (United States)

    Yu, Mingming; Wang, Yuanhong; Jiang, Tingfu; Lv, Zhihua

    2014-06-01

    Sulfate chitosan derivatives have good solubility and therapeutic effect on the cell model of NAFLD. The aim of this study was to examine the therapeutic effect of sulfate chitosan derivatives on NAFLD. The male Wistar rats were orally fed high fat emulsion and received sulfate chitosan derivatives for 5 weeks to determine the pre-treatment effect of sulfate chitosan derivatives on NAFLD. To evaluate the therapeutic effect of sulfate chitosan derivatives on NAFLD, the rats were orally fed with high concentration emulsion for 5 weeks, followed by sulfate chitosan derivatives for 3 weeks. Histological analysis and biomedical assays showed that sulfate chitosan derivatives can dramatically prevent the development of hepatic steatosis in hepatocyte cells. In animal studies, pre-treatment and treatment with sulfate chitosan derivatives significantly protected against hepatic steatohepatitis induced by high fat diet according to histological analysis. Furthermore, increased TC, ALT, MDA, and LEP in NAFLD were significantly ameliorated by pre-treatment and treatment with sulfate chitosan derivatives. Furthermore, increased TG, AST, and TNF-α in NAFLD were significantly ameliorated by treatment with sulfate chitosan derivatives. Sulfate chitosan derivatives have good pre-treatment and therapeutic effect on NAFLD.

  5. Effect of chitosan coatings on postharvest green asparagus quality.

    Science.gov (United States)

    Qiu, Miao; Jiang, Hengjun; Ren, Gerui; Huang, Jianying; Wang, Xiangyang

    2013-02-15

    Fresh postharvest green asparagus rapidly deteriorate due to its high respiration rate. The main benefits of edible active coatings are their edible characteristics, biodegradability and increase in food safety. In this study, the quality of the edible coatings based on 0.50%, 0.25% high-molecular weight chitosan (H-chitosan), and 0.50%, 0.25% low-molecular weight chitosan (L-chitosan) on postharvest green asparagus was investigated. On the basis of the results obtained, 0.25% H-chitosan and 0.50% L-chitosan treatments ensured lower color variation, less weight loss and less ascorbic acid, decrease presenting better quality of asparagus than other concentrations of chitosan treatments and the control during the cold storage, and prolonging a shelf life of postharvest green asparagus. Copyright © 2012 Elsevier Ltd. All rights reserved.

  6. Sol–gel synthesis of tantalum oxide and phosphonic acid-modified carbon nanotubes composite coatings on titanium surfaces

    International Nuclear Information System (INIS)

    Maho, Anthony; Detriche, Simon; Delhalle, Joseph; Mekhalif, Zineb

    2013-01-01

    Carbon nanotubes used as fillers in composite materials are more and more appreciated for the outstanding range of accessible properties and functionalities they generate in numerous domains of nanotechnologies. In the framework of biological and medical sciences, and particularly for orthopedic applications and devices (prostheses, implants, surgical instruments, …), titanium substrates covered by tantalum oxide/carbon nanotube composite coatings have proved to constitute interesting and successful platforms for the conception of solid and biocompatible biomaterials inducing the osseous regeneration processes (hydroxyapatite growth, osteoblasts attachment). This paper describes an original strategy for the conception of resistant and homogeneous tantalum oxide/carbon nanotubes layers on titanium through the introduction of carbon nanotubes functionalized by phosphonic acid moieties (-P(=O)(OH) 2 ). Strong covalent C-P bonds are specifically inserted on their external sidewalls with a ratio of two phosphonic groups per anchoring point. Experimental results highlight the stronger “tantalum capture agent” effect of phosphonic-modified nanotubes during the sol–gel formation process of the deposits compared to nanotubes bearing oxidized functions (-OH, -C=O, -C(=O)OH). Particular attention is also paid to the relative impact of the rate of functionalization and the dispersion degree of the carbon nanotubes in the coatings, as well as their wrapping level by the tantalum oxide matrix material. The resulting effect on the in vitro growth of hydroxyapatite is also evaluated to confirm the primary osseous bioactivity of those materials. Chemical, structural and morphological features of the different composite deposits described herein are assessed by X-ray photoelectron spectroscopy (XPS), scanning (SEM) and transmission (TEM) electronic microscopies, energy dispersive X-rays analysis (EDX) and peeling tests. Highlights: ► Formation of tantalum/carbon nanotube

  7. Sol–gel synthesis of tantalum oxide and phosphonic acid-modified carbon nanotubes composite coatings on titanium surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Maho, Anthony [Laboratory of Chemistry and Electrochemistry of Surfaces, University of Namur (FUNDP), Rue de Bruxelles 61, B-5000 Namur (Belgium); Fonds pour la Formation à la Recherche dans l' Industrie et dans l' Agriculture (FRIA), Rue d' Egmont 5, B-1000 Bruxelles (Belgium); Detriche, Simon; Delhalle, Joseph [Laboratory of Chemistry and Electrochemistry of Surfaces, University of Namur (FUNDP), Rue de Bruxelles 61, B-5000 Namur (Belgium); Mekhalif, Zineb, E-mail: zineb.mekhalif@fundp.ac.be [Laboratory of Chemistry and Electrochemistry of Surfaces, University of Namur (FUNDP), Rue de Bruxelles 61, B-5000 Namur (Belgium)

    2013-07-01

    Carbon nanotubes used as fillers in composite materials are more and more appreciated for the outstanding range of accessible properties and functionalities they generate in numerous domains of nanotechnologies. In the framework of biological and medical sciences, and particularly for orthopedic applications and devices (prostheses, implants, surgical instruments, …), titanium substrates covered by tantalum oxide/carbon nanotube composite coatings have proved to constitute interesting and successful platforms for the conception of solid and biocompatible biomaterials inducing the osseous regeneration processes (hydroxyapatite growth, osteoblasts attachment). This paper describes an original strategy for the conception of resistant and homogeneous tantalum oxide/carbon nanotubes layers on titanium through the introduction of carbon nanotubes functionalized by phosphonic acid moieties (-P(=O)(OH){sub 2}). Strong covalent C-P bonds are specifically inserted on their external sidewalls with a ratio of two phosphonic groups per anchoring point. Experimental results highlight the stronger “tantalum capture agent” effect of phosphonic-modified nanotubes during the sol–gel formation process of the deposits compared to nanotubes bearing oxidized functions (-OH, -C=O, -C(=O)OH). Particular attention is also paid to the relative impact of the rate of functionalization and the dispersion degree of the carbon nanotubes in the coatings, as well as their wrapping level by the tantalum oxide matrix material. The resulting effect on the in vitro growth of hydroxyapatite is also evaluated to confirm the primary osseous bioactivity of those materials. Chemical, structural and morphological features of the different composite deposits described herein are assessed by X-ray photoelectron spectroscopy (XPS), scanning (SEM) and transmission (TEM) electronic microscopies, energy dispersive X-rays analysis (EDX) and peeling tests. Highlights: ► Formation of tantalum

  8. Interaction between chitosan and its related enzymes: A review.

    Science.gov (United States)

    Shinya, Shoko; Fukamizo, Tamo

    2017-11-01

    Chitosan-related enzymes including chitosanases, exo-β-glucosaminidases, and enzymes having chitosan-binding modules recognize ligands through electrostatic interactions between the acidic amino acids in proteins and amino groups of chitosan polysaccharides. However, in GH8 chitosanases, several aromatic residues are also involved in substrate recognition through stacking interactions, and these enzymes consequently hydrolyze β-1,4-glucan as well as chitosan. The binding grooves of these chitosanases are extended and opened at both ends of the grooves, so that the enzymes can clamp a long chitosan polysaccharide. The association/dissociation of positively charged glucosamine residues to/from the binding pocket of a GH2 exo-β-glucosaminidase controls the p K a of the catalytic acid, thereby maintaining the high catalytic potency of the enzyme. In contrast to chitosanases, chitosan-binding modules only accommodate a couple of glucosamine residues, predominantly recognizing the non-reducing end glucosamine residue of chitosan by electrostatic interactions and a hydrogen-bonding network. These structural findings on chitosan-related enzymes may contribute to future applications for the efficient conversion of the chitin/chitosan biomass. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. β-Chitin and chitosan from squid gladius: Biological activities of chitosan and its application as clarifying agent for apple juice.

    Science.gov (United States)

    Abdelmalek, Baha Eddine; Sila, Assaâd; Haddar, Anissa; Bougatef, Ali; Ayadi, Mohamed Ali

    2017-11-01

    Chitin is the second most abundant polysaccharide in biomass after cellulose and the term chitosan usually refers to a family of polymers obtained after chitin deacetylation. The aim of this work was the preparation and the characterization of chitin and chitosan from the gladius (pen) of the European squid (Loligo vulgaris). A high level of deproteinization (more than 80%) was recorded using Alcalase ® with an enzyme/protein ratio of 10U/mg. The demineralization of the gladius was completely achieved within 8h at room temperature in HCl. 13 C NMR, FTIR, and XRD diffractograms of prepared chitin and chitosan were taken and then degree of deacetylation of chitosan was calculated using 13 C CP/MAS-NMR Spectroscopic. Further, in vitro antioxidant capacity of chitosan was evaluated on 1,1-diphenyl-2-picrylhydrazyl method (IC 50 =3.2mgmL -1 ) and the β-carotene bleaching assay (IC 50 =3.3mgmL -1 ). Antimicrobial activity was also investigated and assays indicated that prepared chitosan exhibited marked inhibitory activity against all microbial strains tested. Additionally, chitosan was tested such as clarifying agent for apple juice and showed powerful clarification capability, without affecting nutritional value. Furthermore, the results suggested that prepared chitosan could be used as alternative additive in pharmaceutical preparations and food industry. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Synthesis of N-rich microporous carbon materials from chitosan by alkali activation using Na_2CO_3

    International Nuclear Information System (INIS)

    Ilnicka, Anna; Lukaszewicz, Jerzy P.

    2015-01-01

    Highlights: • The novel manufacturing procedure of nitrogen-rich carbon materials. • The biopolymer chitosan can be activated by sodium carbonate. • The effect of the addition of activator and the temperature of carbonization was investigated. • The N-rich carbon materials exhibit high specific surface area and microporous structure. - Abstract: The paper presents the first systematic study on the synthesis of nitrogen-rich nanoporous activated carbons by chitosan carbonization in the presence of a hard template (activator), i.e. Na_2CO_3. Carbonization process was carried out in the range of 600–900 °C under a flow of nitrogen. The effect of the addition of different volumes of activator and the temperature of carbonization on the development of specific surface area and pore structure (pore volume and median pore diameter) of the activated carbons was investigated. Additionally, the nitrogen content and nitrogen-containing surface species were determined by means of XPS and combustion elemental analysis. The nitrogen content was placed in the range of 2.4–13.1 wt.%. On the grounds of the low-temperature adsorption of nitrogen, it was found that obtained adsorption isotherms were of type-I, based on the IUPAC classification, which is typical for microporous materials.

  11. Poly(acrylonitrile)chitosan composite membranes for urease immobilization.

    Science.gov (United States)

    Gabrovska, Katya; Georgieva, Aneliya; Godjevargova, Tzonka; Stoilova, Olya; Manolova, Nevena

    2007-05-10

    (Poly)acrylonitrile/chitosan (PANCHI) composite membranes were prepared. The chitosan layer was deposited on the surface as well as on the pore walls of the base membrane. This resulted in the reduction of the pore size of the membrane and in an increase of their hydrophilicity. The pore structure of PAN and PANCHI membranes were determined by TEM and SEM analyses. It was found that the average size of the pore under a selective layer base PAN membrane is 7 microm, while the membrane coated with 0.25% chitosan shows a reduced pore size--small or equal to 5 microm and with 0.35% chitosan--about 4 microm. The amounts of the functional groups, the degree of hydrophilicity and transport characteristics of PAN/Chitosan composite membranes were determined. Urease was covalently immobilized onto all kinds of PAN/chitosan composite membranes using glutaraldehyde. Both the amount of bound protein and relative activity of immobilized urease were measured. The highest activity (94%) was measured for urease bound to PANCHI2 membranes (0.25% chitosan). The basic characteristics (pH(opt), pH(stability), T(opt), T(stability), heat inactivation and storage stability) of immobilized urease were determined. The obtained results show that the poly(acrylonitrile)chitosan composite membranes are suitable for enzyme immobilization.

  12. Emerging Chitosan-Based Films for Food Packaging Applications.

    Science.gov (United States)

    Wang, Hongxia; Qian, Jun; Ding, Fuyuan

    2018-01-17

    Recent years have witnessed great developments in biobased polymer packaging films for the serious environmental problems caused by the petroleum-based nonbiodegradable packaging materials. Chitosan is one of the most abundant biopolymers after cellulose. Chitosan-based materials have been widely applied in various fields for their biological and physical properties of biocompatibility, biodegradability, antimicrobial ability, and easy film forming ability. Different chitosan-based films have been fabricated and applied in the field of food packaging. Most of the review papers related to chitosan-based films are focusing on antibacterial food packaging films. Along with the advances in the nanotechnology and polymer science, numerous strategies, for instance direct casting, coating, dipping, layer-by-layer assembly, and extrusion, have been employed to prepare chitosan-based films with multiple functionalities. The emerging food packaging applications of chitosan-based films as antibacterial films, barrier films, and sensing films have achieved great developments. This article comprehensively reviews recent advances in the preparation and application of engineered chitosan-based films in food packaging fields.

  13. Animal experiments and clinical trials of {sup 166}Ho-chitosan for various cancers

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Sang Moo; Choi, C W; Kim, E H; Woo, K S; Chung, W S; Lee, J I; Park, S Y; Son, Y S; Lee, S H; Kim, S J; Kim, B G; Kim, J H; Lee, C H [Korea Cancer Center Hospital, Seoul (Korea, Republic of)

    1997-07-01

    {sup 166}Ho is a good therapeutic radionuclide because of its suitable half-life (26.8 hours), high beta energy and 6% gamma ray for imaging. Chitosan is a kind of N-glucosamine with 400 to 500 kD MW, which chelates metal ions and degrades slowly in vivo. As a preclinical studies, we performed cytotoxic effect of {sup 166}Ho-chitosan in a variety of cancer cell lines derived from stomach or ovarian cancer based on MTT assay and HTCA method. To evaluated the absorbed dose to the cavitary wall from {sup 166}Ho-chitosan, intraperitoneal administration of {sup 166}Ho-chitosan in the rat and simulation of energy transfer from the beta particles to the cavity wall using the Monte Carlo code EGS4 was done, and used as a standard for the planning therapy. Intracavitary {sup 166}Ho-chitosan therapy were tried in peritoneal metastatic ovarian and stomach cancers and cystic brain tumors. Intraarterial injection in inoperable primary liver cancer was also tried. As a radiation synovectomy agent, biocompatibility study in the knee joints of rabbits were performed. {sup 166}Ho-chitosan showed synergistic effects with 5-FU or cisplatin in vitro. 97-99% of {sup 166}Ho-chitosan was localized within the peritoneal cavity, and more than 90% of {sup 166}Ho-chitosan was attached to the peritoneal wall. Partial response were observed in 4 among 5 patients with ovarian cancer without severe toxicity. In the cystic brain tumor, 5 of 8 cysts were shrunken in size with thinning of the wall, 2 out of 8 showed growth retardation. In the primary liver cancer, radioactivity was distributed in the teritory of selected hepatic arterial branch, and partial responses were observed in 2 cases. In the knee joints of the rabbits, more than 98% of {sup 166}Ho-chitosan remained in the joint cavity and was stable upto 1 week. 49 refs., 22 tabs. (author)

  14. Lipase entrapment in PVA/Chitosan biodegradable film for reactor coatings

    Energy Technology Data Exchange (ETDEWEB)

    Batista, Karla A. [Departamento de Bioquímica e Biologia Molecular, Laboratório de Química de Proteínas, Universidade Federal de Goiás, Cx. Postal 131, 74001-970, Goiânia, GO (Brazil); Lopes, Flavio Marques [Departamento de Bioquímica e Biologia Molecular, Laboratório de Química de Proteínas, Universidade Federal de Goiás, Cx. Postal 131, 74001-970, Goiânia, GO (Brazil); Unidade Universitária de Ciências Exatas e Tecnológicas, Universidade Estadual de Goiás, Anápolis, GO (Brazil); Yamashita, Fabio [Departamento de Tecnologia de Alimentos e Medicamentos, Laboratório de Tecnologia, Universidade Estadual de Londrina, Cx. Postal 6001, CEP 86051-990, Londrina, PR (Brazil); Fernandes, Kátia Flávia, E-mail: katia@icb.ufg.br [Departamento de Bioquímica e Biologia Molecular, Laboratório de Química de Proteínas, Universidade Federal de Goiás, Cx. Postal 131, 74001-970, Goiânia, GO (Brazil)

    2013-04-01

    This study reports the development and characterization of novel biodegradable film, based on chitosan and polyvinyl alcohol containing lipase entrapped. The films showed a thickness of 70.4 and 79 μm to PVA/Chitosan and PVA/Chitosan/Lipase, respectively. The entrapment of lipase in PVA/Chitosan film resulted in increasing of 69.4% tensile strength (TS), and 52.4% of elongation. SEM images showed the formation of a continuous film, without pores or cracks. The lipase entrapment efficiency was estimated in 92% and the films were repeatedly used for 25 hydrolytic cycles, maintaining 62% of initial activity. The PVA/Chitosan/Lipase film was used for olive oil hydrolysis of high performance. These results indicate that PVA/Chitosan/Lipase is a promising material for biotechnology applications such as triacylglycerol hydrolysis and biodiesel production. - Highlights: ► Development and characterization of PVA/Chitosan biodegradable film ► Lipase immobilization onto PVA/Chitosan film ► PVA/Chitosan/Lipase film for reactor coating ► Olive oil hydrolysis using PVA/Chitosan/Lipase film.

  15. Lipase entrapment in PVA/Chitosan biodegradable film for reactor coatings

    International Nuclear Information System (INIS)

    Batista, Karla A.; Lopes, Flavio Marques; Yamashita, Fabio; Fernandes, Kátia Flávia

    2013-01-01

    This study reports the development and characterization of novel biodegradable film, based on chitosan and polyvinyl alcohol containing lipase entrapped. The films showed a thickness of 70.4 and 79 μm to PVA/Chitosan and PVA/Chitosan/Lipase, respectively. The entrapment of lipase in PVA/Chitosan film resulted in increasing of 69.4% tensile strength (TS), and 52.4% of elongation. SEM images showed the formation of a continuous film, without pores or cracks. The lipase entrapment efficiency was estimated in 92% and the films were repeatedly used for 25 hydrolytic cycles, maintaining 62% of initial activity. The PVA/Chitosan/Lipase film was used for olive oil hydrolysis of high performance. These results indicate that PVA/Chitosan/Lipase is a promising material for biotechnology applications such as triacylglycerol hydrolysis and biodiesel production. - Highlights: ► Development and characterization of PVA/Chitosan biodegradable film ► Lipase immobilization onto PVA/Chitosan film ► PVA/Chitosan/Lipase film for reactor coating ► Olive oil hydrolysis using PVA/Chitosan/Lipase film

  16. Grape Preservation Using Chitosan Combined with β-Cyclodextrin

    Directory of Open Access Journals (Sweden)

    Yu Youwei

    2013-01-01

    Full Text Available The effect of 1% chitosan combined with 2% β-cyclodextrin to the preservation of fresh grapes under ambient temperature was investigated. The results indicated that the hydrogen bond formed between the hydroxyl group of β-cyclodextrin and the amidogen or hydroxyl group of chitosan and the crystal form of chitosan was also changed when cyclodextrin was doped into chitosan coating. The compound coating could prolong the shelf life of grapes, maintain lower respiration rate and higher activities of superoxide dismutase, peroxidase, and catalase during storage time, and restrain weight loss and malonaldehyde content increase. Coating grapes with chitosan + β-cyclodextrin was a good method in postharvested grape preservation.

  17. A novel analytical method for D-glucosamine quantification and its application in the analysis of chitosan degradation by a minimal enzyme cocktail

    DEFF Research Database (Denmark)

    Mekasha, Sophanit; Toupalová, Hana; Linggadjaja, Eka

    2016-01-01

    Enzymatic depolymerization of chitosan, a β-(1,4)-linked polycationic polysaccharide composed of D-glucosamine (GlcN) and N-acetyl-D-glucosamine (GlcNAc) provides a possible route to the exploitation of chitin-rich biomass. Complete conversion of chitosan to mono-sugars requires the synergistic...... action of endo- and exo- chitosanases. In the present study we have developed an efficient and cost-effective chitosan-degrading enzyme cocktail containing only two enzymes, an endo-attacking bacterial chitosanase, ScCsn46A, from Streptomyces coelicolor, and an exo-attacking glucosamine specific β...

  18. N-(2-hydroxy) propyl-3-trimethylammonium chitosan chloride: An immune-enhancing adjuvant for hepatitis E virus recombinant polypeptide vaccine in mice.

    Science.gov (United States)

    Tao, Wei; Zheng, Hai-Qun; Fu, Ting; He, Zhuo-Jing; Hong, Yan

    2017-08-03

    Adjuvants are essential for enhancing vaccine potency by improving the humoral and/or cell-mediated immune response to vaccine antigens. This study was performed to evaluate the immuno-enhancing characteristic of N-(2-hydroxy) propyl-3-trimethylammonium chitosan chloride (HTCC), the cationically modified chitosan, as an adjuvant for hepatitis E virus (HEV) recombinant polypeptide vaccine. Animal experiments showed that HTCC provides adjuvant activity when co-administered with HEV recombinant polypeptide vaccine by intramuscularly route. Vaccination using HTCC as an adjuvant was associated with increases of the serum HEV-specific IgG antibodies, splenocytes proliferation and the growths of CD4 + CD8 - T lymphocytes and IFN-γ-secreting T lymphocytes in peripheral blood. These findings suggested that HTCC had strong immuno-enhancing effect. Our findings are the first to demonstrate that HTCC is safe and effective in inducing a good antibody response and stimulating Th1-biased immune responses for HEV recombinant polypeptide vaccine.

  19. Adhesion and viability of two enterococcal strains on covalently grafted chitosan and chitosan/kappa-carrageenan multilayers

    NARCIS (Netherlands)

    Bratskaya, S.; Marinin, D.; Simon, F.; Synytska, A.; Zschoche, S.; Busscher, H. J.; Jager, D.; van der Mei, H. C.

    Chitosans are natural aminopolysaccharides, whose low cytotoxicity suggests their potential use for nonadhesive, antibacterial coatings on biomaterials implant surfaces. Here, the antiadhesive behavior and ability to kill bacteria upon adhesion ("contact killing") of chitosan coatings were evaluated

  20. Effect of degree of deacetylation of chitosan on adsorption capacity and reusability of chitosan/polyvinyl alcohol/TiO2 nano composite.

    Science.gov (United States)

    Habiba, Umma; Joo, Tan Chin; Siddique, Tawsif A; Salleh, Areisman; Ang, Bee Chin; Afifi, Amalina M

    2017-11-01

    The chitosan/polyvinyl alcohol/TiO 2 composite was synthesized. Two different degrees of deacetylation of chitosan were prepared by hydrolysis to compare the effectiveness of them. The composite was analyzed via field emission scanning electron microscopy, Fourier transform infrared, X-ray diffraction, thermal gravimetric analysis, weight loss test and adsorption study. The FTIR and XRD results proved the interaction among chitosan, PVA and TiO 2 without any chemical reaction. It was found that, chitosan with higher degree of deacetylation has better stability. Furthermore, it also showed that higher DD of chitosan required less time to reach equilibrium for methyl orange. The adsorption followed the pseudo-second-order kinetic model. The Langmuir and Freundlich isotherm models were fitted well for isotherm study. Adsorption capacity was higher for the composite containing chitosan with higher DD. The dye removal rate was independent of the dye's initial concentration. The adsorption capacity was increased with temperature and it was found from reusability test that the composite containing chitosan with higher DD is more reusable. It was notable that adsorption capacity was even after 15 runs. Therefore, chitosan/PVA/TiO 2 composite can be a very useful material for dye removal. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Radiation-induced degradation of carboxymethylated chitosan and its application in preparation of ionic liquids and silver nanoparticles

    International Nuclear Information System (INIS)

    Zhai Maolin; Huang Ling; Peng Jing; Li Jiuqiang; Wei Genshuan

    2006-01-01

    Radiation effect of γ-ray on carboxymethylated chitosan (CM-chitosan) in solid state and aqueous solution were studied. The changes in molecular weight of CM-chitosan with absorbed dose were monitored by viscosity method. In solid state, there are random chain scissions in the radiation process of CM-chitosan. XRD patterns identified that the degradation of CM-chitosan occurred mostly in amorphous region. Radiation chemical yield (G d ) of CM-chitosan in solid state in N 2 atmosphere was 0.49, which showed CM-chitosan has high radiation stability. Biomaterials composed of CM-chitosan can be thought to sterilize with low absorbed doses. While aqueous solutions of CM-chitosan were irradiated with γ-rays in various conditions, degradations of CM-chitosan were faster in the presence of nitrous oxide or hydrogen peroxide, however, it was inhibited obviously by adding isopropanol because of concentration changes of hydroxyl radicals in different conditions. This indicated that hydroxyl radicals play an important role in radiation degradation of CM-chitosan. Furthermore, FTIR and UV spectra of CM-chitosan radiation-degraded in its solid state status or in aqueous solution showed that main chain structures of CM-chitosan were kept and some carbonyl/carboxyl groups formed during the irradiation were similar to radiation degradation products of chitosan. The method can be used to prepare low molecular weight CM-chitosan. Due to special physical and chemical properties, ionic liquids have attracted much attention in green chemistry field. Environment-friendly ionic liquids ([emim]CM-chitosan) were prepared in acid-base neutralization reactions based on 1-ethyl-3-methylimidazolium hydroxide and CM-chitosan with molecular weights ranging from 2000 to 600 Da. Results of thermal analysis showed that molecular weight of CM-chitosan have little influence on glass transition temperature, melting point and decomposing temperature of [emim]CM-chitosan ionic liquids. Conductivities

  2. Chemical, biochemical, and microbiological aspects of chitosan quaternary salt as active coating on sliced apples

    Directory of Open Access Journals (Sweden)

    Douglas de Britto

    2012-09-01

    Full Text Available The biocompatibility of chitosan and chitosan quaternary salt coatings was evaluated for use as edible coatings for sliced apple. Measurement of water loss, color change, and fungal growth appearance were monitored as a function of time. A significant brownish effect was observed on chitosan coated slices, varying greatly from L* = 76.5 and Hue angle = 95.9° (t = 0 to L* = 45.3 and Hue angle = 69.8° (t = 3 days, whilst for TMC coated samples the variation was considerable lower (L* = 74.1; Hue angle = 95.0° to (L* = 67.0; Hue angle = 83.8° within the same period. The hydrosoluble derivative N,N,N-trimethylchitosan demonstrated good antifungal activity against P. expansum although highly dependent on the polymer properties such as degree of quaternization. The most efficient formulation was that prepared from derivative having a degree of quaternization of 45%, high solubility, and high viscosity. This formulation restrained fungus spreading up to 30%, while for the control it reached almost 80% of the total assessed surfaces during 7 days of storage.

  3. 166Ho-chitosan as a radiation synovectomy agent - biocompatibility study of 166Ho-chitosan in rabbits

    International Nuclear Information System (INIS)

    Kim, Sug Jun; Lee, Soo Yong; Jeon, Dae Geun; Lee Jong Seok

    1997-01-01

    Radiation synovectomy is a noninvasive therapy that has been investigated as an alternative to surgical synovectomy. It is been successfully employed in the treatment of synovitis in rheumatoid arthrits and other inflammatory arthropathies. We developed the 166 Ho-chitosan complex for possible use as a radiation synovectomy agent. Holmium is the more practical isotope based on its higher radioactivity and logner half-life. And isotope based on its higher radioactivity and logner half-life. And chitosan is ideal and suitable particles based on its soluble and biodegradable characteristics. So we investigated the biocompatibility of the 166 Ho-chitosan complex to evaluated the suitability as a radiation synovectomy agent. In this study, we performed in vivo and in vitro stability test and biodistribution test. Our results indicate that 166 Ho-chitosan may be an effective radiopharmaceutical for radiation synovectomy. (author). 30 refs., 7 tabs

  4. Effect of moisture and chitosan layered silicate on morphology and properties of chitosan/layered silicates films

    International Nuclear Information System (INIS)

    Silva, J.R.M.B. da; Santos, B.F.F. dos; Leite, I.F.

    2014-01-01

    Thin chitosan films have been for some time an object of practical assessments. However, to obtain biopolymers capable of competing with common polymers a significant improvement in their properties is required. Currently, the technology of obtaining polymer/layered silicates nanocomposites has proven to be a good alternative. This work aims to evaluate the effect of chitosan content (CS) and layered silicates (AN) on the morphology and properties of chitosan/ layered silicate films. CS/AN bionanocomposites were prepared by the intercalation by solution in the proportion 1:1 and 5:1. Then were characterized by infrared spectroscopy (FTIR), diffraction (XRD) and X-ray thermogravimetry (TG). It is expected from the acquisition of films, based on different levels of chitosan and layered silicates, choose the best composition to serve as a matrix for packaging drugs and thus be used for future research. (author)

  5. An unusual methylene aziridine refined in P2(1)/c and the nonstandard setting P2(1)/n.

    Science.gov (United States)

    Feast, George C; Haestier, James; Page, Lee W; Robertson, Jeremy; Thompson, Amber L; Watkin, David J

    2009-12-01

    The unusual methylene aziridine 6-tert-butyl-3-oxa-2-thia-1-azabicyclo[5.1.0]oct-6-ene 2,2-dioxide, C(9)H(15)NO(3)S, was found to crystallize with two molecules in the asymmetric unit. The structure was solved in both the approximately orthogonal and the oblique settings of space group No. 14, viz. P2(1)/n and P2(1)/c, respectively. A comparison of these results clearly displayed an increase in the correlation between coordinates in the ac plane for the oblique cell. The increase in the corresponding covariances makes a significant contribution to the standard uncertainties of derived parameters, e.g. bond lengths. Since there is yet no CIF definition for the full variance-covariance matrix, there are clear advantages to reporting the structure in the nonstandard space-group setting.

  6. nanocomposites chitosan /clay for electrochemical sensors

    International Nuclear Information System (INIS)

    Braga, Carla R. Costa; Melo, Frank M. Araujo de; Costa, Gilmara M. Silva; Silva, Suedina M. Lima

    2009-01-01

    This study was performed to obtain films of nanocomposites chitosan/bentonite and chitosan/montmorillonite intercalation by the technique of solution in the proportions of 5:1 and 10:1. The nanocomposites were characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD) and the nanocomposites Chitosan/montmorillonite also were characterized by thermogravimetric analysis (TG). The results indicated that the feasibility of obtaining films of nanocomposites exfoliate. Among the suggested applications for films developed in this study includes them use for electrochemical sensors. (author)

  7. Functional Comparison for Lipid Metabolism and Intestinal and Fecal Microflora Enzyme Activities between Low Molecular Weight Chitosan and Chitosan Oligosaccharide in High-Fat-Diet-Fed Rats.

    Science.gov (United States)

    Chiu, Chen-Yuan; Feng, Shih-An; Liu, Shing-Hwa; Chiang, Meng-Tsan

    2017-07-24

    The present study investigated and compared the regulatory effects on the lipid-related metabolism and intestinal disaccharidase/fecal bacterial enzyme activities between low molecular weight chitosan and chitosan oligosaccharide in high-fat-diet-fed rats. Diet supplementation of low molecular weight chitosan showed greater efficiency than chitosan oligosaccharide in suppressing the increased weights in body and in liver and adipose tissues of high-fat-diet-fed rats. Supplementation of low molecular weight chitosan also showed a greater improvement than chitosan oligosaccharide in imbalance of plasma, hepatic, and fecal lipid profiles, and intestinal disaccharidase activities in high-fat-diet-fed rats. Moreover, both low molecular weight chitosan and chitosan oligosaccharide significantly decreased the fecal microflora mucinase and β-glucuronidase activities in high-fat-diet-fed rats. These results suggest that low molecular weight chitosan exerts a greater positive improvement than chitosan oligosaccharide in lipid metabolism and intestinal disaccharidase activity in high-fat-diet-induced obese rats.

  8. Use of the montmorillonite as crosslink agents for chitosan

    International Nuclear Information System (INIS)

    Barbosa, Rossemberg C.; Lima, Rosemary S. Cunha; Braga, Carla R. Costa; Fook, Marcus V. Lia; Silva, Suedina M. Lima

    2009-01-01

    The montmorillonite (the main constituent of bentonite) has been the most commonly used inorganic load in the formation of nanocomposites chitosan / layered silicate. To evaluate its effect as an agent for the reticulation of chitosan, a sodium montmorillonite, Cloisite Na + , supplied by Southern Clay Products, Texas, USA, was used. For the reticulation of chitosan dispersions of chitosan / Cloisite Na + were prepared in different proportions and the obtained films characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermogravimetric analysis (TG). The results indicated that the Cloisite Na + was for efficient and the reticulation of the chitosan and can be used in place of sulfuric acid, which is one of the most common reticulants for chitosan. (author)

  9. Enhancement of Antibacterial activity of Chitosan by gamma irradiation

    International Nuclear Information System (INIS)

    Bashandy, A.S.; Ibrahim, H.M.M.

    2006-01-01

    The antibacterial activity of irradiated and non-irradiated chitosan against E.coli, S.aureus, Salmonella, Strep. fecalis,Closteridium and P. aerugenosa was studied. Up to 1.25 mg/l, chitosan hardly suppressed the growth of all the strains while 3 mg/l of chitosan clearly inhibited the growth of all the studied strains. Therefore, the concentration of 3 mg/l of chitosan in the medium was adopted in this study. Irradiation at 100 KGy under dry conditions was effective in increasing the activity of chitosan and the growth of bacterial strains which was completely inhibited. It was also found that the addition of chitosan to dressing membranes present good barrier properties against microbes especially that irradiated at 100 KGy

  10. Validation of an ergonomic method to withdraw [99mTc] radiopharmaceuticals.

    Science.gov (United States)

    Blondeel-Gomes, Sandy; Marie, Solène; Fouque, Julien; Loyeau, Sabrina; Madar, Olivier; Lokiec, François

    2017-11-10

    The main objective of the present work was to ensure quality of radiopharmaceuticals syringes withdrawn with a "Spinal needle/obturator In-Stopper" system. Methods: Visual examinations and physicochemical tests are performed at T0 and T+4h for [ 99m Tc]albumin nanocolloid and T+7h for [ 99m Tc]eluate, [ 99m Tc] HydroxyMethylene DiPhosphonate and [ 99m Tc]Human Serum Albumin. Microbiological validation was performed according to European pharmacopoeia. Fingertip radiation exposure was evaluated to confirm the safety of the system. Results: Results show stable visual and physicochemical properties. The integrity of the connector was not affected after 30 punctures (no cores). No microbiological contamination was found on tested syringes. Conclusion: The system could be used 30 times. The stability of syringes drawing with this method is guaranteed up to 4 hours for [ 99m Tc]albumin nanocolloid and 7 hours for [ 99m Tc]eluate, [ 99m Tc]HydroxyMethylene DisPhosphonate and [ 99m Tc]Human serum albumin. Copyright © 2017 by the Society of Nuclear Medicine and Molecular Imaging, Inc.

  11. Ionic flotation of uranium contained in industrial phosphoric acid

    International Nuclear Information System (INIS)

    Jdid; Blazy; Bessiere

    1983-01-01

    A new process for uranium recovery from industrial phosphoric acid at 30% of P 2 O 5 is applied by the ionic flotation process. Research is carried out on determination of the nature of ionic species of U in H 3 PO 4 5.5 M and the behavior of reagents from CECA Co. in very acid media. Reagents able to form complexes directly with uranium and stable in phosphoric acid selected are: potassium ethylene diamine tetra (methylene phosphonate) (INIPOL AD32) and sodium dialkyldiphosphonate (34S). Uranium IV, obtained by reduction of uranium VI with iron powder, is precipitated by these reagents. Flotation of the precipitate obtained with INIPOL AD 32 is realized by addition of hexylamino bis (methylene phosphonic acid). A recovery of 80 wt% is obtained. Flotation of the coprecipitate 34S-U(IV) is obtained without any other additions because 34S is a surfactant. Metal recovery is better than 90% and the coprecipitate contains more than 10% U. The process is fast precipitation 10 minutes and flotation 5 minutes and is efficient even at 60 0 C [fr

  12. Design and Synthesis of Fluorescent Acyclic Nucleoside Phosphonates as Potent Inhibitors of Bacterial Adenylate Cyclases

    Czech Academy of Sciences Publication Activity Database

    Břehová, Petra; Šmídková, Markéta; Skácel, Jan; Dračínský, Martin; Mertlíková-Kaiserová, Helena; Velasquez, M. P. S.; Watts, V. J.; Janeba, Zlatko

    2016-01-01

    Roč. 11, č. 22 (2016), s. 2534-2546 ISSN 1860-7179 R&D Projects: GA MV VG20102015046; GA MŠk LO1302 Institutional support: RVO:61388963 Keywords : adenylate cyclase toxin * acyclic nucleoside phosphonates * anthranilic acid Subject RIV: CC - Organic Chemistry Impact factor: 3.225, year: 2016

  13. Thiolated chitosans: useful excipients for oral drug delivery.

    Science.gov (United States)

    Werle, Martin; Bernkop-Schnürch, Andreas

    2008-03-01

    To improve the bioavailability of orally administered drugs, formulations based on polymers are of great interest for pharmaceutical technologists. Thiolated chitosans are multifunctional polymers that exhibit improved mucoadhesive, cohesive and permeation-enhancing as well as efflux-pump-inhibitory properties. They can be synthesized by derivatization of the primary amino groups of chitosan with coupling reagents bearing thiol functions. Various data gained in-vitro as well as in-vivo studies clearly demonstrate the potential of thiolated chitosans for oral drug delivery. Within the current review, the synthesis and characterization of thiolated chitosans so far developed is summarized. Features of thiolated chitosans important for oral drug delivery are discussed as well. Moreover, different formulation approaches, such as matrix tablets and micro-/nanoparticles, as well as the applicability of thiolated chitosans for the oral delivery of various substance classes including peptides and efflux pump substrates, are highlighted.

  14. Rapidly photo-cross-linkable chitosan hydrogel for peripheral neurosurgeries.

    Science.gov (United States)

    Rickett, Todd A; Amoozgar, Zohreh; Tuchek, Chad A; Park, Joonyoung; Yeo, Yoon; Shi, Riyi

    2011-01-10

    Restoring continuity to severed peripheral nerves is crucial to regeneration and enables functional recovery. However, the two most common agents for coaptation, sutures and fibrin glues, have drawbacks such as inflammation, pathogenesis, and dehiscence. Chitosan-based adhesives are a promising alternative, reported to have good cytocompatibility and favorable immunogenicity. A photo-cross-linkable hydrogel based on chitosan is proposed as a new adhesive for peripheral nerve anastomosis. Two Az-chitosans were synthesized by conjugating 4-azidobenzoic acid with low (LMW, 15 kDa) and high (HMW, 50-190 kDa) molecular weight chitosans. These solutions formed a hydrogel in less than 1 min under UV light. The LMW Az-chitosan was more tightly cross-linked than the HMW variant, undergoing significantly less swelling and possessing a higher rheological storage modulus, and both Az-chitosan gels were stiffer than commercial fibrin glue. Severed nerves repaired by Az-chitosan adhesives tolerated longitudinal forces comparable or superior to fibrin glue. Adhesive exposure to intact nerves and neural cell culture showed both Az-chitosans to be nontoxic in the acute (minutes) and chronic (days) time frames. These results demonstrate that Az-chitosan hydrogels are cytocompatible and mechanically suitable for use as bioadhesives in peripheral neurosurgeries.

  15. Poly(D,L-Lactide-Co-Glycolide) Tubes With Multifilament Chitosan Yarn or Chitosan Sponge Core in Nerve Regeneration.

    Science.gov (United States)

    Wlaszczuk, Adam; Marcol, Wiesław; Kucharska, Magdalena; Wawro, Dariusz; Palen, Piotr; Lewin-Kowalik, Joanna

    2016-11-01

    The influence of different kinds of nerve guidance conduits on regeneration of totally transected rat sciatic nerves through a 7-mm gap was examined. Five different types of conduits made of chitosan and poly(D,L-lactide-co-glycolide) (PLGA) were constructed and tested in vivo. We divided 50 animals into equal groups of 10, with a different type of conduit implanted in each group: chitosan sponge core with an average molecular mass of polymer (Mv) of 287 kDa with 7 channels in a PLGA sleeve, chitosan sponge core with an Mv of 423 kDa with 7 channels in a PLGA sleeve, chitosan sponge core (Mv, 423 kDa) with 13 channels in a PLGA sleeve, chitosan multifilament yarn in a PLGA sleeve, and a PLGA sleeve only. Seven weeks after the operation, we examined the distance covered by regenerating nerve fibers, growing of nerves into the conduit's core, and intensity and type of inflammatory reaction in the conduit, as well as autotomy behavior (reflecting neuropathic pain intensity) in the animals. Two types of conduits were allowing nerve outgrowth through the gap with minor autotomy and minor inflammatory reactions. These were the conduits with chitosan multifilament yarn in a PLGA sleeve and the conduits with 13-channel microcrystalline chitosan sponge in a PLGA sleeve. The type of chitosan used to build the nerve guidance conduit influences the intensity and character of inflammatory reaction present during nerve regeneration, which in turn affects the distance crossed by regenerating nerve fibers, growing of the nerve fibers into the conduit's core, and the intensity of autotomy in the animals. Copyright © 2016 American Association of Oral and Maxillofacial Surgeons. Published by Elsevier Inc. All rights reserved.

  16. Effects of Plant Growth Hormones on Mucor indicus Growth and Chitosan and Ethanol Production.

    Science.gov (United States)

    Safaei, Zahra; Karimi, Keikhosro; Golkar, Poorandokht; Zamani, Akram

    2015-07-22

    The objective of this study was to investigate the effects of indole-3-acetic acid (IAA) and kinetin (KIN) on Mucor indicus growth, cell wall composition, and ethanol production. A semi-synthetic medium, supplemented with 0-5 mg/L hormones, was used for the cultivations (at 32 °C for 48 h). By addition of 1 mg/L of each hormone, the biomass and ethanol yields were increased and decreased, respectively. At higher levels, however, an inverse trend was observed. The glucosamine fraction of the cell wall, as a representative for chitosan, followed similar but sharper changes, compared to the biomass. The highest level was 221% higher than that obtained without hormones. The sum of glucosamine and N-acetyl glucosamine (chitin and chitosan) was noticeably enhanced in the presence of the hormones. Increase of chitosan was accompanied by a decrease in the phosphate content, with the lowest phosphate (0.01 g/g cell wall) being obtained when the chitosan was at the maximum (0.45 g/g cell wall). In conclusion, IAA and KIN significantly enhanced the M. indicus growth and chitosan production, while at the same time decreasing the ethanol yield to some extent. This study shows that plant growth hormones have a high potential for the improvement of fungal chitosan production by M. indicus.

  17. Synthesis, characterization and antibacterial activity of hybrid chitosan-cerium oxide nanoparticles: As a bionanomaterials.

    Science.gov (United States)

    Senthilkumar, R P; Bhuvaneshwari, V; Ranjithkumar, R; Sathiyavimal, S; Malayaman, V; Chandarshekar, B

    2017-11-01

    The hybrid chitosan cerium oxide nanoparticles were prepared for the first time by green chemistry approach using plant leaf extract. The intense peak observed around 292nm in the UV-vis spectrum indicate the formation of cerium oxide nanoparticles. The XRD pattern revealed that the hybrid chitosan-cerium oxide nanoparticles have a polycrystalline structure with cubic fluorite phase. The FTIR spectrum of prepared samples showed the formation of Ce-O bonds and chitosan main chains COC and CO. The FESEM image of hybrid chitosan cerium oxide nanoparticles revealed that the particles are spherical in shape with grains size varying from 23.12nm to 89.91nm. EDAX analysis confirmed the presence of Ce, O, C and N elements in the prepared sample. TEM images showed that the prepared hybrid chitosan-cerium oxide nanoparticles are predominantly uniform in size and most of the particles are spherical in shape with less agglomeration and the particles size varies from 3.61nm to 24.40nm. The prepared chitosan cerium oxide nanoparticles of 50μL concentration showed good antibacterial properties against test pathogens, which was confirmed by the FESEM analysis. The prepared small particle size facilitate that these hybrid ChiCO 2 NPs could effectively be used in biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Chitosan derivatives with antimicrobial, antitumour and antioxidant activities--a review.

    Science.gov (United States)

    Jarmila, Vinsová; Vavríková, Eva

    2011-01-01

    Chitosan is a linear polysaccharide with a good biodegradability, biocompatibility, and no toxicity, which provide it with huge potential for future development. The chitosan molecule appears to be a suitable polymeric complex for many biomedical applications. This review gathers current findings on the antibacterial, antifungal, antitumour and antioxidant activities of chitosan derivatives and concurs with our previous review presenting data collected up to 2008. Antibacterial activity is based on molecular weight, the degree of deacetylation, the type of substitutents, which can be cationic or easily form cations, and the type of bacterium. In general, high molecular weight chitosan cannot pass through cell membranes and forms a film that protects cells against nutrient transport through the microbial cell membrane. Low molecular weight chitosan derivatives are water soluble and can better incorporate the active molecule into the cell. Gram-negative bacteria, often represented by Escherichia coli, have an anionic bacterial surface on which cationic chitosan derivatives interact electrostatically. Thus, many chitosan conjugates have cationic components such as ammonium, pyridinium or piperazinium substituents introduced into their molecules to increase their positive charge. Gram-positive bacteria like Staphylococcus aureus are inhibited by the binding of lower molecular weight chitosan derivatives to DNA or RNA. Chitosan nanoparticles exhibit an increase in loading capacity and efficacy. Antitumour active compounds such as doxorubicin, paclitaxel, docetaxel and norcantharidin are used as drug carriers. It is evident that chitosan, with its low molecular weight, is a useful carrier for molecular drugs requiring targeted delivery. The antioxidant scavenging activity of chitosan has been established by the strong hydrogen-donating ability of chitosan. The low molecular weight and greater degree of quarternization have a positive influence on the antioxidant activity

  19. Phytase-mediated enzymatic mineralization of chitosan-enriched hydrogels

    DEFF Research Database (Denmark)

    Lišková, Jana; Douglas, Timothy E.L.; Wijnants, Robbe

    2018-01-01

    Hydrogels mineralized with calcium phosphate (CaP) are increasingly popular bone regeneration biomaterials. Mineralization can be achieved by phosphatase enzyme incorporation and incubation in calcium glycerophosphate (CaGP). Gellan gum (GG) hydrogels containing the enzyme phytase and chitosan...... oligomer were mineralized in CaGP solution and characterized with human osteoblast-like MG63 cells and adipose tissue-derived stem cells (ADSC). Phytase induced CaP formation. Chitosan concentration determined mineralization extent and hydrogel mechanical reinforcement. Phytase-induced mineralization...... promoted MG63 adhesion and proliferation, especially in the presence of chitosan, and was non-toxic to MG63 cells (with and without chitosan). ADSC adhesion and proliferation were poor without mineralization. Chitosan did not affect ADSC osteogenic differentiation....

  20. Synthesis of (2-pyridyl)-Acetyl Chitosan and Its Antioxidant Activity

    International Nuclear Information System (INIS)

    Li, Rongchun

    2011-01-01

    In this paper, chloracetyl chitosan (CACTS) was prepared at first. In the molecules of CACTS, there are active chlorine groups, which can take part in other reactions. Thus, number of chitosan derivatives will be obtained after chlorine is substituted. Choosing pyridine as the active group, a novel water-soluble chitosan derivative, (2-pyridyl)-acetyl chitosan (PACTS) was obtained and its antioxidant activity against hydroxyl radicals and superoxide radicals was assessed. The results indicated that PACTS had better antioxidant activity than that of chitosan, carboxymethyl chitosan (CMCTS), hydroxypropyl chitosan (HPCTS), and Vitamin C. And the IC 50 values against hydroxyl radicals and superoxide radicals were 0.31 mg/mL and 0.21 mg/mL, respectively

  1. Chitosan functionalized poly-ε-caprolactone electrospun fibers and 3D printed scaffolds as antibacterial materials for tissue engineering applications.

    Science.gov (United States)

    Tardajos, Myriam G; Cama, Giuseppe; Dash, Mamoni; Misseeuw, Lara; Gheysens, Tom; Gorzelanny, Christian; Coenye, Tom; Dubruel, Peter

    2018-07-01

    Tissue engineering (TE) approaches often employ polymer-based scaffolds to provide support with a view to the improved regeneration of damaged tissues. The aim of this research was to develop a surface modification method for introducing chitosan as an antibacterial agent in both electrospun membranes and 3D printed poly-ε-caprolactone (PCL) scaffolds. The scaffolds were functionalized by grafting methacrylic acid N-hydroxysuccinimide ester (NHSMA) onto the surface after Ar-plasma/air activation. Subsequently, the newly-introduced NHS groups were used to couple with chitosan of various molecular weights (Mw). High Mw chitosan exhibited a better coverage of the surface as indicated by the higher N% detected by X-ray photoelectron spectroscopy (XPS) and the observations with either scanning electron microscopy (SEM)(for fibers) or Coomassie blue staining (for 3D-printed scaffolds). A lactate dehydrogenase assay (LDH) using L929 fibroblasts demonstrated the cell-adhesion and cell-viability capacity of the modified samples. The antibacterial properties against S. aureus ATCC 6538 and S. epidermidis ET13 revealed a slower bacterial growth rate on the surface of the chitosan modified scaffolds, regardless the chitosan Mw. Copyright © 2018 Elsevier Ltd. All rights reserved.

  2. Preparation and characterization of magnetic chitosan particles for hyperthermia application

    International Nuclear Information System (INIS)

    Park, Ji-Ho; Im, Ki-Hyeong; Lee, Se-Ho; Kim, Dong-Hyun; Lee, Doug-Youn; Lee, Yong-Keun; Kim, Kwang-Mahn; Kim, Kyoung-Nam

    2005-01-01

    The size and shape of magnetic chitosan particles were found to be dependent on both the barium ferrite/chitosan (BF/C) ratio and viscosity of a chitosan solution. The saturation magnetization of magnetic chitosan particles varied directly with the BF/C ratio, while coercivity remained almost constant. Notably, incorporated chitosan was shown to exert substantial activity with regard to low cytotoxicity and high heating rate

  3. Development of dual-sensitive smart polymers by grafting chitosan with poly (N-isopropylacrylamide: an overview

    Directory of Open Access Journals (Sweden)

    Nívia do Nascimento Marques

    2015-06-01

    Full Text Available AbstractA great deal of research on polymers over the past two decades has been focused on the development of stimuli-responsive polymers to obtain materials able to respond to specific surroundings. In this paper, an overview is presented of the concepts, behavior and applicability of these “smart polymers”. Polymers that are temperature- or pH-sensitive are discussed in detail, including the response mechanisms and types of macromolecules, because they are easy to handle and have a wide range of applications. Finally, the combination of pH and temperature responsive properties by means of graft copolymerization of chitosan with poly (N-isopropylacrylamide (PNIPAM was chosen to represent some synthetic routes and properties of dual-sensitive polymeric systems developed currently.

  4. Rheological study of chitosan in solution

    International Nuclear Information System (INIS)

    Silva, Italo Guimaraes Medeiros da; Alves, Keila dos Santos; Balaban, Rosangela de Carvalho

    2009-01-01

    Chitosan is an abundant biopolymer with remarkable physicochemical and biological properties, usually employed in a wide range of applications. It acts as a cationic polyelectrolyte in aqueous acid solutions, leading to unique characteristics. In this work, chitosan was characterized by 1 H NMR and its rheological behavior were studied as function of chitosan sample, shear rate, polymer concentration, ionic strength, time and temperature. In order to calculate rheological parameters and to understand the macromolecular dynamic in solution, the Otswald-de Waele model was fitted. (author)

  5. Development and characterization of chitosan-PEG-TAT nanoparticles for the intracellular delivery of siRNA

    Directory of Open Access Journals (Sweden)

    Malhotra M

    2013-05-01

    Full Text Available Meenakshi Malhotra,1 Catherine Tomaro-Duchesneau,1 Shyamali Saha,2 Imen Kahouli,3 Satya Prakash11Biomedical Technology and Cell Therapy Research Laboratory, Department of Biomedical Engineering, Faculty of Medicine, 2Faculty of Dentistry, 3Department of Experimental Medicine, McGill University, Montreal, QC, CanadaAbstract: Recently, cell-penetrating peptides have been proposed to translocate antibodies, proteins, and other molecules in targeted drug delivery. The proposed study presents the synthesis and characterization of a peptide-based chitosan nanoparticle for small interfering RNA (siRNA delivery, in-vitro. Specifically, the synthesis included polyethylene glycol (PEG, a hydrophilic polymer, and trans-activated transcription (TAT peptide, which were chemically conjugated on the chitosan polymer. The conjugation was achieved using N-Hydroxysuccinimide-PEG-maleimide (heterobifunctional PEG as a cross-linker, with the bifunctional PEG facilitating the amidation reaction through its N-Hydroxysuccinimide group and reacting with the amines on chitosan. At the other end of PEG, the maleimide group was chemically conjugated with the cysteine-modified TAT peptide. The degree of substitution on chitosan with PEG and on PEG with TAT was confirmed using colorimetric assays. The resultant polymer was used to form nanoparticles complexing siRNA, which were then characterized for particle size, morphology, cellular uptake, and cytotoxicity. The nanoparticles were tested in-vitro on mouse neuroblastoma cells (Neuro2a. Particle size and surface charge were characterized and an optimal pH condition and PEG molecular weight were determined to form sterically stable nanoparticles. Results indicate 7.5% of the amines in chitosan polymer were conjugated to the PEG and complete conjugation of TAT peptide was observed on the synthesized PEGylated chitosan polymer. Compared with unmodified chitosan nanoparticles, the nanoparticles formed at pH 6 were

  6. Preoperative Localization of Mediastinal Parathyroid Adenoma with Intra-arterial Methylene Blue

    Energy Technology Data Exchange (ETDEWEB)

    Salman, Rida; Sebaaly, Mikhael G. [American University of Beirut Medical Center, Department of Diagnostic Radiology (Lebanon); Wehbe, Mohammad Rachad; Sfeir, Pierre; Khalife, Mohamad [American University of Beirut Medical Center, Department of General Surgery (Lebanon); Al-Kutoubi, Aghiad, E-mail: mk00@aub.edu.lb [American University of Beirut Medical Center, Department of Diagnostic Radiology (Lebanon)

    2017-06-15

    Ectopic parathyroid is found in 16% of patients with hyperparathyroidism. 2% of ectopic parathyroid adenomas are not accessible to standard cervical excision. In such cases, video-assisted thoracoscopic resection is the recommended definitive treatment. We present a case of mediastinal parathyroid adenoma localized preoperatively by injecting methylene blue within a branch of the internal mammary artery that is supplying the adenoma. Intra-arterial methylene blue injection facilitated visualization and resection of the adenoma. The preoperative intra-arterial infusion of methylene blue appears to be an effective and safe method for localization of ectopic mediastinal parathyroid adenomas and allows rapid identification during thoracoscopic resection.

  7. Chitosan in Mucoadhesive Drug Delivery: Focus on Local Vaginal Therapy

    Directory of Open Access Journals (Sweden)

    Toril Andersen

    2015-01-01

    Full Text Available Mucoadhesive drug therapy destined for localized drug treatment is gaining increasing importance in today’s drug development. Chitosan, due to its known biodegradability, bioadhesiveness and excellent safety profile offers means to improve mucosal drug therapy. We have used chitosan as mucoadhesive polymer to develop liposomes able to ensure prolonged residence time at vaginal site. Two types of mucoadhesive liposomes, namely the chitosan-coated liposomes and chitosan-containing liposomes, where chitosan is both embedded and surface-available, were made of soy phosphatidylcholine with entrapped fluorescence markers of two molecular weights, FITC-dextran 4000 and 20,000, respectively. Both liposomal types were characterized for their size distribution, zeta potential, entrapment efficiency and the in vitro release profile, and compared to plain liposomes. The proof of chitosan being both surface-available as well as embedded into the liposomes in the chitosan-containing liposomes was found. The capability of the surface-available chitosan to interact with the model porcine mucin was confirmed for both chitosan-containing and chitosan-coated liposomes implying potential mucoadhesive behavior. Chitosan-containing liposomes were shown to be superior in respect to the simplicity of preparation, FITC-dextran load, mucoadhesiveness and in vitro release and are expected to ensure prolonged residence time on the vaginal mucosa providing localized sustained release of entrapped model substances.

  8. Chitosan-thioglycolic acid as a versatile antimicrobial agent.

    Science.gov (United States)

    Geisberger, Georg; Gyenge, Emina Besic; Hinger, Doris; Käch, Andres; Maake, Caroline; Patzke, Greta R

    2013-04-08

    As functionalized chitosans hold great potential for the development of effective and broad-spectrum antibiotics, representative chitosan derivatives were tested for antimicrobial activity in neutral media: trimethyl chitosan (TMC), carboxy-methyl chitosan (CMC), and chitosan-thioglycolic acid (TGA; medium molecular weight: MMW-TGA; low molecular weight: LMW-TGA). Colony forming assays indicated that LMW-TGA displayed superior antimicrobial activity over the other derivatives tested: a 30 min incubation killed 100% Streptococcus sobrinus (Gram-positive bacteria) and reduced colony counts by 99.99% in Neisseria subflava (Gram-negative bacteria) and 99.97% in Candida albicans (fungi). To elucidate LMW-TGA effects at the cellular level, microscopic studies were performed. Use of fluorescein isothiocyanate (FITC)-labeled chitosan derivates in confocal microscopy showed that LMW-TGA attaches to microbial cell walls, while transmission electron microscopy indicated that this derivative severely affects cell wall integrity and intracellular ultrastructure in all species tested. We therefore propose LMW-TGA as a promising and effective broad-band antimicrobial compound.

  9. Mechanical property, degradation rate, and bone cell growth of chitosan coated titanium influenced by degree of deacetylation of chitosan.

    Science.gov (United States)

    Yuan, Youling; Chesnutt, Betsy M; Wright, Lee; Haggard, Warren O; Bumgardner, Joel D

    2008-07-01

    Chitosan has shown promise as a coating for dental/craniofacial and orthopaedic implants. However, the effects of degree of deacetylation (DDA) of chitosan on coating bond strength, degradation, and biological performance is not known. The aim of this project was to evaluate bonding, degradation, and bone cell growth on titanium coated with chitosans of different DDA and from different manufacturers. Three different chitosans, 80.6%, 81.7%, and 92.3% DDA were covalently bonded to titanium coupons via silane-glutaraldehyde molecules. Bond strengths were evaluated in mechanical tensile tests, and degradation, over 5 weeks, was conducted in cell culture medium with and without 100 microg/mL lysozyme. Cytocompatibility was evaluated for 10 days using UMR 106 osteoblastic cells. Results showed that mean chitosan coating bond strengths ranged from 2.2-3.8 MPa, and that there was minimal affect of DDA on coating bond strengths. The coatings exhibited little dissolution over 5 weeks in medium with or without lysozyme. However, the molecular weight (MW) of the chitosan coatings remaining on the titanium samples after 5 weeks decreased by 69-85% with the higher DDA chitosan coatings exhibiting less percent change in MW than the lower DDA materials. The growth of the UMR 106 osteoblast cells on the 81.7% DDA chitosan coating was lower on days 3 and 5, as compared with the other two coatings, but by day 10, there were no differences in growth among three coatings or to the uncoated titanium controls. Differences in growth were attributed to differences in manufacturer source material, though all coatings were judged to be osteocompatible in vitro. 2007 Wiley Periodicals, Inc.

  10. Probing cellular behaviors through nanopatterned chitosan membranes

    International Nuclear Information System (INIS)

    Yang, Chung-Yao; Sung, Chun-Yen; Shuai, Hung-Hsun; Cheng, Chao-Min; Yeh, J Andrew

    2013-01-01

    This paper describes a high-throughput method for developing physically modified chitosan membranes to probe the cellular behavior of MDCK epithelial cells and HIG-82 fibroblasts adhered onto these modified membranes. To prepare chitosan membranes with micro/nanoscaled features, we have demonstrated an easy-to-handle, facile approach that could be easily integrated with IC-based manufacturing processes with mass production potential. These physically modified chitosan membranes were observed by scanning electron microscopy to gain a better understanding of chitosan membrane surface morphology. After MDCK cells and HIG-82 fibroblasts were cultured on these modified chitosan membranes for various culture durations (i.e. 1, 2, 4, 12 and 24 h), they were investigated to decipher cellular behavior. We found that both cells preferred to adhere onto a flat surface rather than on a nanopatterned surface. However, most (> 80%) of the MDCK cells showed rounded morphology and would suspend in the cultured medium instead of adhering onto the planar surface of negatively nanopatterned chitosan membranes. This means different cell types (e.g. fibroblasts versus epithelia) showed distinct capabilities/preferences of adherence for materials of varying surface roughness. We also showed that chitosan membranes could be re-used at least nine times without significant contamination and would provide us consistency for probing cell–material interactions by permitting reuse of the same substrate. We believe these results would provide us better insight into cellular behavior, specifically, microscopic properties and characteristics of cells grown under unique, nanopatterned cell-interface conditions. (paper)

  11. Properties of Chitosan-Laminated Collagen Film

    Directory of Open Access Journals (Sweden)

    Vera Lazić

    2012-01-01

    Full Text Available The objective of this study is to determine physical, mechanical and barrier properties of chitosan-laminated collagen film. Commercial collagen film, which is used for making collagen casings for dry fermented sausage production, was laminated with chitosan film layer in order to improve the collagen film barrier properties. Different volumes of oregano essential oil per 100 mL of filmogenic solution were added to chitosan film layer: 0, 0.2, 0.4, 0.6 and 0.8 mL to optimize water vapour barrier properties. Chitosan layer with 0.6 or 0.8 % of oregano essential oil lowered the water vapour transmission rate to (1.85±0.10·10–6 and (1.78±0.03·10–6 g/(m2·s·Pa respectively, compared to collagen film ((2.51±0.05·10–6 g/(m2·s·Pa. However, chitosan-laminated collagen film did not show improved mechanical properties compared to the collagen one. Tensile strength decreased from (54.0±3.8 MPa of the uncoated collagen film to (36.3±4.0 MPa when the film was laminated with 0.8 % oregano essential oil chitosan layer. Elongation at break values of laminated films did not differ from those of collagen film ((18.4±2.7 %. Oxygen barrier properties were considerably improved by lamination. Oxygen permeability of collagen film was (1806.8±628.0·10–14 cm3/(m·s·Pa and values of laminated films were below 35·10–14 cm3/(m·s·Pa. Regarding film appearance and colour, lamination with chitosan reduced lightness (L and yellowness (+b of collagen film, while film redness (+a increased. These changes were not visible to the naked eye.

  12. Synthesis and Characterization of Chitosan-p-t-Butylcalix[4]arene acid

    Science.gov (United States)

    Handayani, D. S.; Frimadasi, W.; Kusumaningsih, T.; Pranoto

    2018-03-01

    The synthesis of chitosan-p-t-butylcalix[4]arene acid was done with DIC (N, N’-diisopropylcarbodiimide) as the coupling agent. The structural analysis of the chitosan-p-t-butylcalix[4]arene acid was conducted by spectrophotometer Fourier Transform Infra Red (FTIR) and X-Ray Diffraction (XRD). Meanwhile, the surface area was investigated by Surface Area Analysis, the Scanning Electrone Microscope (SEM) analysed the surface morphology, and also the melting point temperature was determined. FTIR analysis on Chitosan-p-t-butylcalix[4]arene provides an overlapped absorption of -OH and -NH groups at 3438.26 cm-1. Meanwhile, a C = C aromatic bond present at 1480.43 cm-1. XRD analysis shows some broaden peaks due to the amorphous phase of the prepared material. The prepared material is a brownish yellow solid, odorless and porous. The melting point, surface area, and the average pore radius are above 300 °C, 9.42 m2 / g, and 52.5938 Å, respectively.

  13. Photocrosslinkable chitosan as a biological adhesive.

    Science.gov (United States)

    Ono, K; Saito, Y; Yura, H; Ishikawa, K; Kurita, A; Akaike, T; Ishihara, M

    2000-02-01

    A photocrosslinkable chitosan to which both azide and lactose moieties were introduced (Az-CH-LA) was prepared as a biological adhesive for soft tissues and its effectiveness was compared with that of fibrin glue. Introduction of the lactose moieties resulted in a much more water-soluble chitosan at neutral pH. Application of ultraviolet light (UV) irradiation to photocrosslinkable Az-CH-LA produced an insoluble hydrogel within 60 s. This hydrogel firmly adhered two pieces of sliced ham with each other, depending upon the Az-CH-LA concentration. The binding strength of the chitosan hydrogel prepared from 30-50 mg/mL of Az-CH-LA was similar to that of fibrin glue. Compared to the fibrin glue, the chitosan hydrogel more effectively sealed air leakage from pinholes on isolated small intestine and aorta and from incisions on isolated trachea. Neither Az-CH-LA nor its hydrogel showed any cytotoxicity in cell culture tests of human skin fibroblasts, coronary endothelial cells, and smooth muscle cells. Furthermore, all mice studied survived for at least 1 month after implantation of 200 microL of photocrosslinked chitosan gel and intraperitoneal administration of up to 1 mL of 30 mg/mL of Az-CH-LA solution. These results suggest that the photocrosslinkable chitosan developed here has the potential of serving as a new tissue adhesive in medical use. Copyright 2000 John Wiley & Sons, Inc.

  14. Controlling chitosan-based encapsulation for protein and vaccine delivery

    Science.gov (United States)

    Koppolu, Bhanu prasanth; Smith, Sean G.; Ravindranathan, Sruthi; Jayanthi, Srinivas; Kumar, Thallapuranam K.S.; Zaharoff, David A.

    2014-01-01

    Chitosan-based nano/microencapsulation is under increasing investigation for the delivery of drugs, biologics and vaccines. Despite widespread interest, the literature lacks a defined methodology to control chitosan particle size and drug/protein release kinetics. In this study, the effects of precipitation-coacervation formulation parameters on chitosan particle size, protein encapsulation efficiency and protein release were investigated. Chitosan particle sizes, which ranged from 300 nm to 3 μm, were influenced by chitosan concentration, chitosan molecular weight and addition rate of precipitant salt. The composition of precipitant salt played a significant role in particle formation with upper Hofmeister series salts containing strongly hydrated anions yielding particles with a low polydispersity index (PDI) while weaker anions resulted in aggregated particles with high PDIs. Sonication power had minimal effect on mean particle size, however, it significantly reduced polydispersity. Protein loading efficiencies in chitosan nano/microparticles, which ranged from 14.3% to 99.2%, was inversely related to the hydration strength of precipitant salts, protein molecular weight and directly related to the concentration and molecular weight of chitosan. Protein release rates increased with particle size and were generally inversely related to protein molecular weight. This study demonstrates that chitosan nano/microparticles with high protein loading efficiencies can be engineered with well-defined sizes and controllable release kinetics through manipulation of specific formulation parameters. PMID:24560459

  15. Surface modification of protein enhances encapsulation in chitosan nanoparticles

    Science.gov (United States)

    Koyani, Rina D.; Andrade, Mariana; Quester, Katrin; Gaytán, Paul; Huerta-Saquero, Alejandro; Vazquez-Duhalt, Rafael

    2018-04-01

    Chitosan nanoparticles have a huge potential as nanocarriers for environmental and biomedical purposes. Protein encapsulation in nano-sized chitosan provides protection against inactivation, proteolysis, and other alterations due to environmental conditions, as well as the possibility to be targeted to specific tissues by ligand functionalization. In this work, we demonstrate that the chemical modification of the protein surface enhances the protein loading in chitosan nanocarriers. Encapsulation of green fluorescent protein and the cytochrome P450 was studied. The increase of electrostatic interactions between the free amino groups of chitosan and the increased number of free carboxylic groups in the protein surface enhance the protein loading, protein retention, and, thus, the enzymatic activity of chitosan nanoparticles. The chemical modification of protein surface with malonic acid moieties reduced drastically the protein isoelectric point increasing the protein interaction with the polycationic biomaterial and chitosan. The chemical modification of protein does not alter the morphology of chitosan nanoparticles that showed an average diameter of 18 nm, spheroidal in shape, and smooth surfaced. The strategy of chemical modification of protein surface, shown here, is a simple and efficient technique to enhance the protein loading in chitosan nanoparticles. This technique could be used for other nanoparticles based on polycationic or polyanionic materials. The increase of protein loading improves, doubtless, the performance of protein-loaded chitosan nanoparticles for biotechnological and biomedical applications.

  16. Chitosan: collagen sponges. In vitro mineralization

    International Nuclear Information System (INIS)

    Martins, Virginia da C.A.; Silva, Gustavo M.; Plepis, Ana Maria G.

    2011-01-01

    The regeneration of bone tissue is a problem that affects many people and scaffolds for bone tissue growth has been widely studied. The aim of this study was the in vitro mineralization of chitosan, chitosan:native collagen and chitosan:anionic collagen sponges. The sponges were obtained by lyophilization and mineralization was made by soaking the sponges in alternating solutions containing Ca 2+ and PO 4 3- . The mineralization was confirmed by infrared spectroscopy, energy dispersive X-ray and X-ray diffraction observing the formation of phosphate salts, possibly a carbonated hydroxyapatite since Ca/P=1.80. The degree of mineralization was obtained by thermogravimetry calculating the amount of residue at 750 deg C. The chitosan:anionic collagen sponge showed the highest degree of mineralization probably due to the fact that anionic collagen provides additional sites for interaction with the inorganic phase. (author)

  17. SOLID-STATE FERMENTATIVE PRODUCTION AND BIOACTIVITY OF FUNGAL CHITOSAN

    Directory of Open Access Journals (Sweden)

    Barry Aigbodion Omogbai

    2013-10-01

    Full Text Available Chitosan production was investigated using a laboratory-scale solid substrate fermentation (SSF technique with four species of fungi: Penicillium expansum, Aspergillus niger, Rhizopus oryzae and Fusarium moniliforme.The peak growth for the organisms was after 16 days. Aspergillus niger had the highest growth with a maximal dry cell biomass of 15.8g/kg after 16 days cultivation on corn straw under solid substrate fermentation. This was closely followed by Rhizopus oryzae (14.6g/kg, Penicillium expansum (13.8g/kg and Fusarium moniliforme (10.6g/kg respectively. The fungus Rhizopus oryzae had the highest chitosan production with a maximum of 8.57g/kg in 16 days under solid substrate fermentation (SSF with a medium containing corn straw. Aspergillus niger showed a modest chitosan yield of 6.8g/kg. Penicillium expansum and Fusarium moniliforme had low chitosan yields of 4.31g/kg and 3.1g/kg respectively. The degree of deacetylation of fungal chitosans ranged between 75.3-91.5% with a viscosity of 3.6-7.2 centipoises (Cp.Chitosan extracted from Rhizopus oryzae was found to have antibacterial activity on some bacterial isolates. At a concentration of 50mg/L, Rhizopus oryzae chitosan paralleled crab chitosan in susceptibility testing against some food-borne bacterial pathogens. Escherichia coli, Salmonella typhi, Pseudomonas aeruginosa and Bacillus subtilis showed inhibition rates of 83.2%, 67.9%, 63.8% and 62.4% respectively in response to 50mg/l Rhizopus oryzae chitosan in 24 h. The rate of inhibition (% increased with increase in chitosan concentration.

  18. Chitosan-based nanocarriers for antimalarials

    Science.gov (United States)

    Dreve, Simina; Kacso, Iren; Popa, Adriana; Raita, Oana; Bende, A.; Borodi, Gh.; Bratu, I.

    2012-02-01

    The objective of this research was to synthesize and characterize chitosan-based liquid and solid materials with unique absorptive and mechanical properties as carriers for quinine - one of the most used antimalarial drug. The use of chitosan (CTS) as base in polyelectrolyte complex systems, to prepare solid release systems as sponges is presented. The preparation by double emulsification of CTS hydrogels carrying quinine as anti-malarial drug is reported. The concentration of quinine in the CTS hydrogel was 0.08 mmol. Chitosan - drug loaded hydrogel was used to generate solid sponges by freeze-drying at -610°C and 0.09 atm. Structural investigations of the solid formulations were done by Fourier-transformed infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-VIS), spectrofluorimetry, differential scanning calorimetry (DSC) and X-ray diffractometry. The results indicated that the drug molecule is forming temporary chelates in CTS hydrogels and sponges. Electron paramagnetic resonance (EPR) demonstrates the presence of free radicals in a wide range and the antioxidant activity for chitosan - drug supramolecular cross-linked assemblies.

  19. Study of extraction-spectrophotometric micro-determination of boron with methylene blue and its application

    International Nuclear Information System (INIS)

    Zhu Daohong

    1990-08-01

    A sensitive extraction-spectrophotometric method for microdetermination of boron with methylene blue was investigated. The method was based on the extraction of a BF 4 - -methylene blue complex into dichloroethane. Boron was determined directly by measuring the absorbance at 658 nm. The calibration graph was linear over the range of 2.5 x 10 -9 to 8 x 10 -8 g/mL. The blank, mechanism of the reactions, interference of other ions and some optimum conditions of the method were studied in detail. The main source of the blank resulted from methylene blue and the complex of F - -methylene blue. In order to reduce the blank, the amounts of methylene blue, H 2 SO 4 and HF were used as less as possible. Only one to one complex BF 4 - -methylene blue was formed in the medium of H 2 SO 4 . About 90% of methylene blue and F - -methylene blue complex was removre with 5 ml of water and only a little amount of BF 4 -methylene blue complex was decomposed. The extraction-spectrophotometric method with methylene blue was first applied to the microdetermination of boron in sodium metal and UF 6 . The sample of sodium metal was taken and weighed in the glovebox filled with argon. Then sodium metal was oxidized, hydrolyzed, netralized and fluorizated with H 2 O, H 2 SO 4 and HF, respectively. The 0.5 ppm of boron in sodium metal was determined with a relative error about ±4%. This method can be applied to the determination of boron in sodium metal, sodium sulfate and sodium hydroxide at diffeent grades. The species of boron in the hydrolysate of UF 6 is BF 4 - anion, so the sample can be directly analyzed. Boron contents in the range of 0.1 to 0.5 ppm was determined with a relative error about ±3%. Six samples could be analysed in 2h

  20. Electrophoretic deposition of composite hydroxyapatite-chitosan coatings

    International Nuclear Information System (INIS)

    Pang Xin; Zhitomirsky, Igor

    2007-01-01

    Cathodic electrophoretic deposition has been utilized for the fabrication of composite hydroxyapatite-chitosan coatings on 316L stainless steel substrates. The addition of chitosan to the hydroxyapatite suspensions promoted the electrophoretic deposition of the hydroxyapatite nanoparticles and resulted in the formation of composite coatings. The obtained coatings were investigated by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning and transmission electron microscopy, potentiodynamic polarization measurements, and electrochemical impedance spectroscopy. It was shown that the deposit composition can be changed by a variation of the chitosan or hydroxyapatite concentration in the solutions. Experimental conditions were developed for the fabrication of hydroxyapatite-chitosan nanocomposites containing 40.9-89.8 wt.% hydroxyapatite. The method enabled the formation of adherent and uniform coatings of thicknesses up to 60 μm. X-ray studies revealed that the preferred orientation of the hydroxyapatite nanoparticles in the chitosan matrix increases with decreasing hydroxyapatite content in the composite coatings. The obtained coatings provided the corrosion protection for the 316L stainless steel substrates

  1. Chitosan magnetic nanoparticles for drug delivery systems.

    Science.gov (United States)

    Assa, Farnaz; Jafarizadeh-Malmiri, Hoda; Ajamein, Hossein; Vaghari, Hamideh; Anarjan, Navideh; Ahmadi, Omid; Berenjian, Aydin

    2017-06-01

    The potential of magnetic nanoparticles (MNPs) in drug delivery systems (DDSs) is mainly related to its magnetic core and surface coating. These coatings can eliminate or minimize their aggregation under physiological conditions. Also, they can provide functional groups for bioconjugation to anticancer drugs and/or targeted ligands. Chitosan, as a derivative of chitin, is an attractive natural biopolymer from renewable resources with the presence of reactive amino and hydroxyl functional groups in its structure. Chitosan nanoparticles (NPs), due to their huge surface to volume ratio as compared to the chitosan in its bulk form, have outstanding physico-chemical, antimicrobial and biological properties. These unique properties make chitosan NPs a promising biopolymer for the application of DDSs. In this review, the current state and challenges for the application magnetic chitosan NPs in drug delivery systems were investigated. The present review also revisits the limitations and commercial impediments to provide insight for future works.

  2. Chitosan/bentonite bionanocomposites: morphology and mechanical behavior

    International Nuclear Information System (INIS)

    Braga, C.R.C.; Melo, F.M.A. de; Vitorino, I.F.; Fook, M.V.L.; Silva, S.M.L.

    2010-01-01

    This study chitosan/bentonite bionanocomposite films were prepared by solution intercalation process, seeking to investigate the effect of the chitosan/bentonite ratio (5/1 e 10/1) on the morphology and mechanical behavior of the bionanocomposites. It was used as nanophase, Argel sodium bentonite (AN), was provided by Bentonit Uniao Nordeste-BUN (Campina Grande, Brazil) and as biopolymer matrix the chitosan of low molecular weight and degree of deacetylation of 86,7% was supplied by Polymar (Fortaleza, Brazil). The bionanocomposites was investigated by X-ray diffraction and tensile properties. According to the results, the morphology and the mechanical behavior of the bionanocomposite was affected by the ratio of chitosan/bentonite. The chitosan/bentonite ratio (5/1 and 10/1) indicated the formation of an intercalated nanostructure and of the predominantly exfoliated nanostructure, respectively. And the considerable increases in the resistance to the traction were observed mainly for the bionanocomposite with predominantly exfoliated morphology. (author)

  3. Preparation of thermally stable microcapsules with a chitosan-silica hybrid.

    Science.gov (United States)

    Kang, Hong-Yi; Chen, Hui-Huang

    2014-09-01

    Addition of microcapsules with a high dielectric constant and low specific heat capacity to a battered layer was designed to create a higher temperature in the crust than in the prefried fish nuggets to prevent the water vapor in the fish nuggets from migrating to the crust during microwave heating. Therefore, chitosan-silica hybrids and soybean oil were utilized to prepare the shell and core of the thermally stable microcapsules (MC(CS)), respectively. The MC(CS) were prepared by sol-gel coacervation from an oil-in-water emulsion. The sodium silicate was hydrolyzed and coacervated through polymerization for 24 h at pH 5. The zeta potential analysis indicated that chitosan with a positive charge and silica with a negative charge interacted through electrostatic attraction to form a hybrid shell. The volume mean particle size and encapsulation efficiency of the MC(CS) were 9.6 ± 0.2 μm and 75.6% ± 1.3%, respectively, when oil/chitosan = 0.2 and chitosan/silica = 0.5 (w/w). In addition to H-bonding and electrostatic attraction, Si-O-N bonds were formed between chitosan and silica. Dehydration of the bound water in the MC(CS) was observed in the range of 25 to 250 °C in the differential scanning calorimetry thermal analysis, with the lack of apparent thermal peaks indicating its high thermal stability. The decrease of force to cut the crust observed by texture analysis as well as the increase of hedonic score by consumer acceptance test revealed the addition of 1% MC(CS) significantly improved the crispness of the crust in the microwave-reheated nuggets. © 2014 Institute of Food Technologists®

  4. Electrochemical behavior of an anticancer drug 5-fluorouracil at methylene blue modified carbon paste electrode

    International Nuclear Information System (INIS)

    Bukkitgar, Shikandar D.; Shetti, Nagaraj P.

    2016-01-01

    A novel sensor for the determination of 5-fluorouracil was constructed by electrochemical deposition of methylene blue on surface of carbon paste electrode. The electrode surface morphology was studied using Atomic force microscopy and XRD. The electrochemical activity of modified electrode was characterized using cyclic voltammetry and differential pulse method. The developed sensor shows impressive enlargement in sensitivity of 5-fluorouracil determination. The peak currents obtained from differential pulse voltammetry was linear with concentration of 5-fluorouracil in the range 4 × 10 −5 –1 × 10 −7 M and detection limit and quantification limit were calculated to be 2.04 nM and 6.18 nM respectively. Further, the sensor was successfully applied in pharmaceutical and biological fluid sample analysis. - Highlights: • Electrochemical oxidation of 5-fluorouracil has been investigated for first time at methylene blue modified carbon paste electrode • The electrode process was irreversible and diffusion controlled • Probable electrochemical mechanism was proposed which involved two proton and two electron transfer reaction • The LOD and LOQ values were calculated to be 2.04 nM and 6.18 nM, respectively, with good selectivity and sensitivity. • Proposed method was applied to 5-Fluorouracil determination in pharmaceutical and spiked human urine samples

  5. Chitosan-based dressings loaded with neurotensin--an efficient strategy to improve early diabetic wound healing.

    Science.gov (United States)

    Moura, Liane I F; Dias, Ana M A; Leal, Ermelindo C; Carvalho, Lina; de Sousa, Hermínio C; Carvalho, Eugénia

    2014-02-01

    One important complication of diabetes mellitus is chronic, non-healing diabetic foot ulcers (DFUs). This study aims to develop and use dressings based on chitosan derivatives for the sustained delivery of neurotensin (NT), a neuropeptide that acts as an inflammatory modulator in wound healing. Three different derivatives, namely N-carboxymethyl chitosan, 5-methyl pyrrolidinone chitosan (MPC) and N-succinyl chitosan, are presented as potential biomaterials for wound healing applications. Our results show that MPC has the best fluid handling capacity and delivery profile, also being non-toxic to Raw 264.7 and HaCaT cells. NT-loaded and non-loaded MPC dressings were applied to control/diabetic wounds to evaluate their in vitro/in vivo performance. The results show that the former induced more rapid healing (50% wound area reduction) in the early phases of wound healing in diabetic mice. A NT-loaded MPC foam also reduced expression of the inflammatory cytokine TNF-α (Pdiabetic skin (P<0.001), significantly increasing fibroblast migration and collagen (COL1A1, COL1A2 and COL3A1) expression and deposition. These results suggest that MPC-based dressings may work as an effective support for sustained NT release to reduce DFUs. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  6. 2H Solid-State NMR Analysis of the Dynamics and Organization of Water in Hydrated Chitosan

    Directory of Open Access Journals (Sweden)

    Fenfen Wang

    2016-04-01

    Full Text Available Understanding water–biopolymer interactions, which strongly affect the function and properties of biopolymer-based tissue engineering and drug delivery materials, remains a challenge. Chitosan, which is an important biopolymer for the construction of artificial tissue grafts and for drug delivery, has attracted extensive attention in recent decades, where neutralization with an alkali solution can substantially enhance the final properties of chitosan films cast from an acidic solution. In this work, to elucidate the effect of water on the properties of chitosan films, we investigated the dynamics and different states of water in non-neutralized (CTS-A and neutralized (CTS-N hydrated chitosan by mobility selective variable-temperature (VT 2H solid-state NMR spectroscopy. Four distinct types of water exist in all of the samples with regards to dynamic behavior. First, non-freezable, rigid and strongly bound water was found in the crystalline domain at low temperatures. The second component consists of weakly bound water, which is highly mobile and exhibits isotropic motion, even below 260 K. Another type of water undergoes well-defined 180° flips around their bisector axis. Moreover, free water is also present in the films. For the CTS-A sample in particular, another special water species were bounded to acetic acid molecules via strong hydrogen bonding. In the case of CTS-N, the onset of motions of the weakly bound water molecules at 260 K was revealed by 2H-NMR spectroscopy. This water is not crystalline, even below 260 K, which is also the major contribution to the flexibility of chitosan chains and thus toughness of materials. By contrast, such motion was not observed in CTS-A. On the basis of the 2H solid-state NMR results, it is concluded that the unique toughness of CTS-N mainly originates from the weakly bound water as well as the interactions between water and the chitosan chains.

  7. Nitrate adsorption from aqueous solution using granular chitosan-Fe{sup 3+} complex

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Qili [School of Water Resources and Environment, China University of Geosciences (Beijing), Beijing, 100083 (China); Key Laboratory of Groundwater Cycle and Environment Evolution,China University of Geosciences (Beijing), Ministry of Education, Beijing, 100083 (China); Chen, Nan, E-mail: chennan@cugb.edu.cn [School of Water Resources and Environment, China University of Geosciences (Beijing), Beijing, 100083 (China); Key Laboratory of Groundwater Cycle and Environment Evolution, China University of Geosciences (Beijing), Ministry of Education, Beijing, 100083 (China); Feng, Chuanping [School of Water Resources and Environment, China University of Geosciences (Beijing), Beijing, 100083 (China); Key Laboratory of Groundwater Cycle and Environment Evolution, China University of Geosciences (Beijing), Ministry of Education, Beijing, 100083 (China); Hu, WeiWu [The Journal Center, China University of Geosciences (Beijing), Beijing, 100083 (China)

    2015-08-30

    Highlights: • Granular chitosan-Fe{sup 3+} complex had high performance for nitrate adsorption. • Granular chitosan-Fe{sup 3+} complex had shorter equilibrium time (1.5 h). • Nitrate adsorption was ascribed to ion exchange and electrostatic attraction. • Granular chitosan-Fe{sup 3+} complex could be regenerated using NaCl solution. - Abstract: In the present study, In order to efficiently remove nitrate, granular chitosan-Fe{sup 3+} complex with high chemical stability and good environmental adaptation was synthesized through precipitation method and characterized using SEM, XRD, BET and FTIR. The nitrate adsorption performance was evaluated by batch experiments. The results indicated that granular chitosan-Fe{sup 3+} complex was an amorphous and mesoporous material. The BET specific surface area and average pore size were 8.98 m{sup 2} g{sup −1} and 56.94 Å, respectively. The point of zero charge was obtained at pH 5. The maximum adsorption capacity reached 8.35 mg NO{sub 3}{sup −}-N g{sup −1} based on Langmuir–Freundlich model. Moreover, no significant change in the nitrate removal efficiency was observed in the pH range of 3.0–10.0. The adverse influence of sulphate on nitrate removal was the most significant, followed by bicarbonate and fluoride, whereas chloride had slightly adverse effect. Adsorption process followed the pseudo-second-order kinetic model, and the experimental equilibrium data were fitted well with the Langmuir–Freundlich and D–R isotherm models. Thermodynamic parameters revealed that nitrate adsorption was a spontaneous and exothermic process. Granular chitosan-Fe{sup 3+} complex could be effectively regenerated by NaCl solution.

  8. Adsorption dynamics and equilibrium studies of Zn (II) onto chitosan

    Indian Academy of Sciences (India)

    Unknown

    Adsorption dynamics and equilibrium studies of Zn (II) onto chitosan. G KARTHIKEYAN*, K ANBALAGAN and N MUTHULAKSHMI ANDAL. Department of Chemistry, Gandhigram Rural Institute – Deemed University, Gandhigram 624 302, India e-mail: drg_karthikeyan@rediffmail.com. MS received 3 June 2003; revised 12 ...

  9. Methylene Blue to Treat Protamine-induced Anaphylaxis Reactions. An Experimental Study in Pigs

    Directory of Open Access Journals (Sweden)

    Agnes Afrodite S. Albuquerque

    Full Text Available ABSTRACT Objective: To examine if methylene blue (MB can counteract or prevent protamine (P cardiovascular effects. Methods: The protocol included five heparinized pig groups: Group Sham -without any drug; Group MB - MB 3 mg/kg infusion; Group P - protamine; Group P/MB - MB after protamine; Group MB/P - MB before protamine. Nitric oxide levels were obtained by the nitric oxide/ozone chemiluminescence method, performed using the Nitric Oxide Analizer 280i (Sievers, Boulder, CO, USA. Malondialdehyde plasma levels were estimated using the thiobarbiturate technique. Results: 1 Groups Sham and MB presented unchanged parameters; 2 Group P - a Intravenous protamine infusion caused mean arterial pressure decrease and recovery trend after 25-30 minutes, b Cardiac output decreased and remained stable until the end of protamine injection, and c Sustained systemic vascular resistance increased until the end of protamine injection; 3 Methylene blue infusion after protamine (Group P/MB - a Marked mean arterial pressure decreased after protamine, but recovery after methylene blue injection, b Cardiac output decreased after protamine infusion, recovering after methylene blue infusion, and c Sustained systemic vascular resistance increased after protamine infusion and methylene blue injections; 4 Methylene blue infusion before protamine (Group MB/P - a Mean arterial pressure decrease was less severe with rapid recovery, b After methylene blue, there was a progressive cardiac output increase up to protamine injection, when cardiac output decreased, and c Sustained systemic vascular resistance decreased after protamine, followed by immediate Sustained systemic vascular resistance increase; 5 Plasma nitrite/nitrate and malondialdehyde values did not differ among the experimental groups. Conclusion: Reviewing these experimental results and our clinical experience, we suggest methylene blue safely prevents and treats hemodynamic protamine complications, from the

  10. Progress of research on the adsorption of chitosan and its derivatives to uranium

    International Nuclear Information System (INIS)

    Wang Caixia; Liu Yunhai; Hua Rong; Pang Cui; Wang Yong

    2010-01-01

    This paper has summarized the study on the adsorption of chitosan and its derivatives to uranium in recent years at home and abroad. It was found that the derivatives can be serine-type chitosan, methyl phosphoric acid modified chitosan, 3,4-dihydroxy benzoic acid-type chitosan, chitosan with 3,4-dihydroxybenzoic acid moiety, chitosan resin possessing a phenylarsonic acid moiety, quadrol modified chitosan, chitosan modified with molecular imprinting technique, polyacrylamide hydrogel, chitosan-coated perlite and so on. The application vista of chitosan and its derivatives to Absorpt uranium in water has been prospected. (authors)

  11. Study of sorption properties of nickel on chitosan; Studium sorpcnych vlastnosti niklu na chitosan

    Energy Technology Data Exchange (ETDEWEB)

    Pivarciova, L; Rosskopfova, O; Galambos, M [Univerzita Komenskeho v Bratislave, Prirodovedecka fakulta, Katedra jadrovej chemie, 84215 Bratislava (Slovakia)

    2012-04-25

    Sorption of nickel on the selected sorbent was studied by a batch method. The effect of contact time and pH to reach sorption equilibrium was studied. During sorption of Ni{sup 2+} ions there proceed predominantly ion-exchange reactions on its surface. Time to reach sorption equilibrium of nickel on chitosan was 14 hours. Sorption percentage after 14 hours reached a value of 84 %. Solutions with starting pH value between 3.9 and 8.1 were used for sorption of nickel. A sorption of nickel on chitosan was > 97% in monitored interval of pH after 24 hours of contact . At an initial pH from 3.9 to 6.4 was the final pH 6.6 due to protonisation of amino groups. A pH value was 6.4 after sorption of 7.1. Sorption of nickel is reduced by increasing of concentrations of Ni{sup 2+} ions in the solution. Langmuir isotherm was used for interpretation of nickel sorption on chitosan. A maximum sorption capacity for chitosan was 2,67 {center_dot} 10{sup -3} mol/g{sup -}1. (authors)

  12. The efficient synthesis of 2-arylpyrimidine acyclic nucleoside phosphonates using Liebeskind-Srogl cross-coupling reaction

    Czech Academy of Sciences Publication Activity Database

    Břehová, Petra; Česnek, Michal; Dračínský, Martin; Holý, Antonín; Janeba, Zlatko

    2011-01-01

    Roč. 67, č. 38 (2011), s. 7379-7385 ISSN 0040-4020 R&D Projects: GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z40550506 Keywords : Liebeskind-Srogl cross - coupling * acyclic nucleoside phosphonates * pyrimidines * arylboronic acids * microwave Subject RIV: CC - Organic Chemistry Impact factor: 3.025, year: 2011

  13. The shelf life extension of refrigerated grass carp (Ctenopharyngodon idellus) fillets by chitosan coating combined with glycerol monolaurate.

    Science.gov (United States)

    Yu, Dawei; Jiang, Qixing; Xu, Yanshun; Xia, Wenshui

    2017-08-01

    A novel chitosan-based coating solution was prepared by combining glycerol monolaurate (GML) for shelf life extension of refrigerated grass carp fillets. The control and coated fillets were analyzed periodically for physicochemical (pH, thiobarbituric acid (TBA) value, total volatile basic nitrogen (TVB-N) value, K value, and shear force), microbiological (total viable counts (TVC), psychrophilic bacteria counts (PTC), Pseudomonads and H 2 S-producing bacteria) and sensorial characteristics. The results showed that chitosan-GML coated samples presented better quality preservation effects than chitosan coating alone. In addition, 2% chitosan enriched with 0.3% GML showed the significant (Pchitosan coating enriched with GML was a promising method to extend the shelf life of refrigerated fillets. Copyright © 2017. Published by Elsevier B.V.

  14. Biological evaluation of 153Sm-ethylenediaminetetra methylene phosphonate (EDTMP)

    International Nuclear Information System (INIS)

    Ranganatha, D.K.; Lal, Ramji

    1997-01-01

    Samarium-153 EDTMP has been studied in rats to establish bone localisation in normal bone tissue and the uptake in the soft tissue. Biodistribution results were highly promising with >3% of the injected dose localizing in the femurs and 15 days. (author). 4 refs., 2 tabs

  15. Aerogels from Chitosan Solutions in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Gonzalo Santos-López

    2017-12-01

    Full Text Available Chitosan aerogels conjugates the characteristics of nanostructured porous materials, i.e., extended specific surface area and nano scale porosity, with the remarkable functional properties of chitosan. Aerogels were obtained from solutions of chitosan in ionic liquids (ILs, 1-butyl-3-methylimidazolium acetate (BMIMAc, and 1-ethyl-3-methyl-imidazolium acetate (EMIMAc, in order to observe the effect of the solvent in the structural characteristics of this type of materials. The process of elaboration of aerogels comprised the formation of physical gels through anti-solvent vapor diffusion, liquid phase exchange, and supercritical CO2 drying. The aerogels maintained the chemical identity of chitosan according to Fourier transform infrared spectrophotometer (FT-IR spectroscopy, indicating the presence of their characteristic functional groups. The internal structure of the obtained aerogels appears as porous aggregated networks in microscopy images. The obtained materials have specific surface areas over 350 m2/g and can be considered mesoporous. According to swelling experiments, the chitosan aerogels could absorb between three and six times their weight of water. However, the swelling and diffusion coefficient decreased at higher temperatures. The structural characteristics of chitosan aerogels that are obtained from ionic liquids are distinctive and could be related to solvation dynamic at the initial state.

  16. Metal Complexation with Chitosan and its Grafted Copolymer

    International Nuclear Information System (INIS)

    Abo-Hussen, A.A.; Elkholy, S.S.; Elsabee, M.Z.

    2005-01-01

    The adsorption of M (II); Co (II), Ni (If), Cu (II), Zn (II) and Cd (II) from aqueous solutions by chitosan flakes and beads have been studied. The maximum up-take of M (II) ions on chitosan beads was greater than on flakes. Batch adsorption experiments were carried out as a function of ph, agitation period and initial concentration of the metal ions. A ph of 6.0 was found to be optimum for M (II) adsorption on chitosan flakes and beads. The uptake of the ions was determined from the changes in its concentration, as measured by ultraviolet and visible spectroscopy. The metal ions uptake of chitosan grafted with vinyl pyridine (VP) is higher than that of the chitosan. The experimental data of the adsorption equilibrium from M (II)-solutions correlated well with the Langmuir and Freundlich equations. Several spectroscopic methods have been used to study the formation of the polymer/metal cation complex. The cation coordination is accompanied by proton displacement off the polymer or by fixation of a hydroxide ion in aqueous solutions. The largest ionic displacement is observed with Cu (II) and Zn (II) demonstrating the largest affinity of chitosan for these ions. The FT-IR spectral of the complexes show that both the amino and hydroxyl groups of chitosan participated in the chelation process. The ESR spectra of Cu-complex show an absorption at gi 2.06, g// = 2.23, A// x 10-4 (cm-1) = 160 and G = 3.8 indicating the formation of square planar structure. The adsorption of M (II) ions followed the sequence Cu (II) > Zn (II) > Cd (II) > Ni (II) > Co (II), this order seems to be independent on the size and the physical form of chitosan. SEM shows small membranous structure on the surface of chitosan flakes as compared to Cu (Il)- chitosan complex. EDTA was used for the desorption studies

  17. Process for crosslinking methylene-containing aromatic polymers with ionizing radiation

    Science.gov (United States)

    Bell, Vernon L. (Inventor); Havens, Stephen J. (Inventor)

    1990-01-01

    A process for crosslinking aromatic polymers containing radiation-sensitive methylene groups (-CH2-) by exposing the polymers to ionizing radiation thereby causing crosslinking of the polymers through the methylene groups is described. Crosslinked polymers are resistant to most organic solvents such as acetone, alcohols, hydrocarbons, methylene, chloride, chloroform, and other halogenated hydrocarbons, to common fuels and to hydraulic fluids in contrast to readily soluble uncrosslinked polymers. In addition, the degree of crosslinking of the polymers depends upon the percentage of the connecting groups which are methylene which ranges from 5 to 50 pct and preferably from 25 to 50 pct of the connecting groups, and is also controlled by the level of irradiation which ranges from 25 to 1000 Mrads and preferably from 25 to 250 Mrads. The temperature of the reaction conditions ranges from 25 to 200 C and preferably at or slightly above the glass transition temperature of the polymer. The crosslinked polymers are generally more resistant to degradation at elevated temperatures such as greater than 150 C, have a reduced tendency to creep under load, and show no significant embrittlement of parts fabricated from the polymers.

  18. Effect of chitosan coating on the characteristics of DPPC liposomes

    Directory of Open Access Journals (Sweden)

    Mohsen M. Mady

    2010-07-01

    Full Text Available Because it is both biocompatible and biodegradable, chitosan has been used to provide a protective capsule in new drug formulations. The present work reports on investigations into some of the physicochemical properties of chitosan-coated liposomes, including drug release rate, transmission electron microscopy (TEM, zeta potential and turbidity measurement. It was found that chitosan increases liposome stability during drug release. The coating of DPPC liposomes with a chitosan layer was confirmed by electron microscopy and the zeta potential of liposomes. The coating of liposomes by chitosan resulted in a marginal increase in the size of the liposomes, adding a layer of (92 ± 27.1 nm. The liposomal zeta potential was found to be increasingly positive as chitosan concentration increased from 0.1% to 0.3% (w/v, before stabilising at a relatively constant value. Turbidity studies revealed that the coating of DPPC liposomes with chitosan did not significantly modify the main phase transition temperature of DPPC at examined chitosan concentrations. The appropriate combination of liposomal and chitosan characteristics may produce liposomes with specific, prolonged and controlled release.

  19. Synthesis of alpha-Branched Acyclic Nucleoside Phosphonates as Potential Inhibitors of Bacterial Adenylate Cyclases

    Czech Academy of Sciences Publication Activity Database

    Frydrych, Jan; Skácel, Jan; Šmídková, Markéta; Mertlíková-Kaiserová, Helena; Dračínský, Martin; Gnanasekaran, Ramachandran; Lepšík, Martin; Soto-Velasquez, M.; Watts, V. J.; Janeba, Zlatko

    2018-01-01

    Roč. 13, č. 2 (2018), s. 199-206 ISSN 1860-7179 R&D Projects: GA MV VG20102015046; GA ČR(CZ) GBP208/12/G016; GA MŠk LO1302 Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonates * adenylate cyclase toxin * bisamidates * Bordetella pertussis * prodrugs Subject RIV: CC - Organic Chemistry OBOR OECD: Organic chemistry Impact factor: 3.225, year: 2016

  20. Hydrophobization and antimicrobial activity of chitosan and paper-based packaging material.

    Science.gov (United States)

    Bordenave, Nicolas; Grelier, Stephane; Coma, Veronique

    2010-01-11

    This study reports the elaboration of water-resistant, antimicrobial, chitosan and paper-based materials as environmentally friendly food packaging materials. Two types of papers were coated with chitosan-palmitic acid emulsions or with a blend of chitosan and O,O'-dipalmitoylchitosan (DPCT). Micromorphology studies showed that inclusion of hydrophobic compounds into the chitosan matrix was enhanced by grafting them onto chitosan and that this led to their penetration of the paper's core. Compared to chitosan-coated papers, the coating of chitosan-palmitic emulsion kept vapor-barrier properties unchanged (239 and 170 g.m(-2).d(-1) versus 241 and 161 g.m(-2).d(-1)), while the coating of chitosan-DPCT emulsion dramatically deteriorated them (441 and 442 g.m(-2).d(-1)). However, contact angle measurements (110-120 degrees after 1 min) and penetration dynamics analysis showed that both strategies improved liquid-water resistance of the materials. Kit-test showed that all hydrophobized chitosan-coated papers kept good grease barrier properties (degree of resistance 6-8/12). Finally, all chitosan-coated materials exhibited over 98% inhibition on Salmonella Typhimurium and Listeria monocytogenes .

  1. Effect of chitosan-N-acetylcysteine conjugate in a mouse model of botulinum toxin B-induced dry eye.

    Science.gov (United States)

    Hongyok, Teeravee; Chae, Jemin J; Shin, Young Joo; Na, Daero; Li, Li; Chuck, Roy S

    2009-04-01

    To evaluate the effect of a thiolated polymer lubricant, chitosan-N-acetylcysteine conjugate (C-NAC), in a mouse model of dry eye. Eye drops containing 0.5% C-NAC, 0.3% C-NAC, a vehicle (control group), artificial tears, or fluorometholone were applied in a masked fashion in a mouse model of induced dry eye from 3 days to 4 weeks after botulinum toxin B injection. Corneal fluorescein staining was periodically recorded. Real-time reverse transcriptase-polymerase chain reaction and immunofluorescence staining were performed at the end of the study to evaluate inflammatory cytokine expressions. Mice treated with C-NAC, 0.5%, and fluorometholone showed a downward trend that was not statistically significant in corneal staining compared with the other groups. Chitosan-NAC formulations, fluorometholone, and artificial tears significantly decreased IL-1beta (interleukin 1beta), IL-10, IL-12alpha, and tumor necrosis factor alpha expression in ocular surface tissues. The botulinum toxin B-induced dry eye mouse model is potentially useful in evaluating new dry eye treatment. Evaluation of important molecular biomarkers suggests that C-NAC may impart some protective ocular surface properties. However, clinical data did not indicate statistically significant improvement of tear production and corneal staining in any of the groups tested. Topically applied C-NAC might protect the ocular surface in dry eye syndrome, as evidenced by decreased inflammatory cytokine expression.

  2. Chitosan composite hydrogels reinforced with natural clay nanotubes.

    Science.gov (United States)

    Huang, Biao; Liu, Mingxian; Zhou, Changren

    2017-11-01

    Here, chitosan composites hydrogels were prepared by addition of halloysite nanotubes (HNTs) in the chitosan KOH/LiOH/urea solution. The raw chitosan and chitosan/HNTs composite hydrogels were obtained by heat treatment at 60°C for 8h and then regeneration in ethanol solution. The viscosity of the composite solution is increased with HNTs content. The Fourier transform infrared spectroscopy (FT-IR) shows that the hydrogen bonds interactions exist between the HNTs and the chitosan. X-ray diffraction (XRD) results show that the crystal structure of HNT is not changed in the composite hydrogels. The compressive property test and storage modulus determination show that the mechanical properties and anti-deformation ability of the composite hydrogel significantly increase owing to the reinforcing effect of HNTs. The composites hydrogel with 66.7% HNTs can undergo 7 times compression cycles without breaking with compressive strength of 0.71MPa at 70% deformation, while pure chitosan hydrogel is broken after bearing 5 compression cycles with compressive strength of 0.14MPa and a maximum deformation of 59%. A porous structure with pore size of 100-500μm is found in the composite hydrogels by scanning electron microscopy (SEM), and the pore size and the swelling ratio in NaCl solution decrease by the addition of HNTs and the immersing of ethanol. Chitosan/HNTs composite hydrogels show low cytotoxicity towards MC3T3-E1 cells. Also, the composite hydrogels show a maximum drug entrapment efficiency of 45.7% for doxorubicin (DOX) which is much higher than that of pure chitosan hydrogel (27.5%). All the results illustrate that the chitosan/HNTs composite hydrogels show promising applications as biomaterials. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Occupational methaemoglobinaemia. Mechanisms of production, features, diagnosis and management including the use of methylene blue.

    Science.gov (United States)

    Bradberry, Sally M

    2003-01-01

    unreliable in the presence of methaemoglobinaemia. Arterial blood gas analysis is mandatory in severe poisoning and reveals normal partial pressures of oxygen (pO2) and carbon dioxide (pCO2,), a normal 'calculated' haemoglobin oxygen saturation, an increased methaemoglobin concentration and possibly a metabolic acidosis. Following decontamination, high-flow oxygen should be given to maximise oxygen carriage by remaining ferrous haem. No controlled trial of the efficacy of methylene blue has been performed but clinical experience suggests that methylene blue can increase the rate of methaemoglobin conversion to haemoglobin some 6-fold. Patients with features and/or methaemoglobin concentrations of 30-50%, should be administered methylene blue 1-2 mg/kg/bodyweight intravenously (the dose depending on the severity of the features), whereas those with methaemoglobin concentrations exceeding 50% should be given methylene blue 2 mg/kg intravenously. Symptomatic improvement usually occurs within 30 minutes and a second dose of methylene blue will be required in only very severe cases or if there is evidence of ongoing methaemoglobin formation. Methylene blue is less effective or ineffective in the presence of glucose-6-phosphate dehydrogenase deficiency since its antidotal action is dependent on nicotinamide-adenine dinucleotide phosphate (NADP+). In addition, methylene blue is most effective in intact erythrocytes; efficacy is reduced in the presence of haemolysis. Moreover, in the presence of haemolysis, high dose methylene blue (20-30 mg/kg) can itself initiate methaemoglobin formation. Supplemental antioxidants such as ascorbic acid (vitamin C), N-acetylcysteine and tocopherol (vitamin E) have been used as adjuvants or alternatives to methylene blue with no confirmed benefit. Exchange transfusion may have a role in the management of severe haemolysis or in G-6-P-D deficiency associated with life-threatening methaemoglobinaemia where methylene blue is relatively contraindicated.

  4. Studies on electrospun nylon-6/chitosan complex nanofiber interactions

    International Nuclear Information System (INIS)

    Zhang Haitao; Li Shubai; Branford White, Christopher J.; Ning Xin; Nie Huali; Zhu Limin

    2009-01-01

    Composite membranes of nylon-6/chitosan nanofibers with different weight ratio of nylon-6 to chitosan were fabricated successfully using electrospinning. Morphologies of the nanofibers were investigated by scanning electron microscopy (SEM) and the intermolecular interactions of the nylon-6/chitosan complex were evaluated by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), differential scanning calorimetry (DSC) as well as mechanical testing. We found that morphology and diameter of the nanofibers were influenced by the concentration of the solution and weight ratio of the blending component materials. Furthermore FT-IR analyses on interactions between components demonstrated an IR band frequency shift that appeared to be dependent on the amount of chitosan in the complex. Observations from XRD and DSC suggested that a new fraction of γ phase crystals appeared and increased with the increasing content of chitosan in blends, this indicated that intermolecular interactions occurred between nylon-6 and chitosan. Results from performance data in mechanical showed that intermolecular interactions varied with varying chitosan content in the fibers. It was concluded that a new composite product was created and the stability of this system was attributed to strong new interactions such as hydrogen bond formation between the nylon-6 polymers and chitosan structures.

  5. Recent advances in chitosan-based nanoparticulate pulmonary drug delivery

    Science.gov (United States)

    Islam, Nazrul; Ferro, Vito

    2016-07-01

    The advent of biodegradable polymer-encapsulated drug nanoparticles has made the pulmonary route of administration an exciting area of drug delivery research. Chitosan, a natural biodegradable and biocompatible polysaccharide has received enormous attention as a carrier for drug delivery. Recently, nanoparticles of chitosan (CS) and its synthetic derivatives have been investigated for the encapsulation and delivery of many drugs with improved targeting and controlled release. Herein, recent advances in the preparation and use of micro-/nanoparticles of chitosan and its derivatives for pulmonary delivery of various therapeutic agents (drugs, genes, vaccines) are reviewed. Although chitosan has wide applications in terms of formulations and routes of drug delivery, this review is focused on pulmonary delivery of drug-encapsulated nanoparticles of chitosan and its derivatives. In addition, the controversial toxicological effects of chitosan nanoparticles for lung delivery will also be discussed.

  6. Poly(Poly(Ethylene Glycol Methyl Ether Methacrylate Grafted Chitosan for Dye Removal from Water

    Directory of Open Access Journals (Sweden)

    Bryan Tsai

    2017-03-01

    Full Text Available As the demand for textile products and synthetic dyes increases with the growing global population, textile dye wastewater is becoming one of the most significant water pollution contributors. Azo dyes represent 70% of dyes used worldwide, and are hence a significant contributor to textile waste. In this work, the removal of a reactive azo dye (Reactive Orange 16 from water by adsorption with chitosan grafted poly(poly(ethylene glycol methyl ether methacrylate (CTS-GMA-g-PPEGMA was investigated. The chitosan (CTS was first functionalized with glycidyl methacrylate and then grafted with poly(poly(ethylene glycol methyl ether methacrylate using a nitroxide-mediated polymerization grafting to approach. Equilibrium adsorption experiments were carried out at different initial dye concentrations and were successfully fitted to the Langmuir and Freundlich adsorption isotherm models. Adsorption isotherms showed maximum adsorption capacities of CTS-g-GMA-PPEGMA and chitosan of 200 mg/g and 150 mg/g, respectively, while the Langmuir equations estimated 232 mg/g and 194 mg/g, respectively. The fundamental assumptions underlying the Langmuir model may not be applicable for azo dye adsorption, which could explain the difference. The Freundlich isotherm parameters, n and K, were determined to be 2.18 and 17.7 for CTS-g-GMA-PPEGMA and 0.14 and 2.11 for chitosan, respectively. An “n” value between one and ten generally indicates favorable adsorption. The adsorption capacities of a chitosan-PPEGMA 50/50 physical mixture and pure PPEGMA were also investigated, and both exhibited significantly lower adsorption capacities than pure chitosan. In this work, CTS-g-GMA-PPEGMA proved to be more effective than its parent chitosan, with a 33% increase in adsorption capacity.

  7. Conductivity enhancement via chemical modification of chitosan based green polymer electrolyte

    International Nuclear Information System (INIS)

    Mobarak, N.N.; Ahmad, A.; Abdullah, M.P.; Ramli, N.; Rahman, M.Y.A.

    2013-01-01

    The potential of carboxymethyl chitosan as a green polymer electrolyte has been explored. Chitosan produced from partial deacetylation of chitin was reacted with monochloroacetic acid to form carboxymethyl chitosan. A green polymer electrolyte based chitosan and carboxymethyl chitosan was prepared by solution-casting technique. The powder and films were characterized by reflection Fourier transform infrared (ATR-FTIR) spectroscopy, 1 H nuclear magnetic resonance, elemental analysis and X-ray diffraction, electrochemical impedance spectroscopy, and scanning electron microscopy. The shift of wavenumber that represents hydroxyl and amine stretching confirmed the polymer solvent complex formation. The XRD spectra results show that chemical modification of chitosan has improved amorphous properties of chitosan. The ionic conductivity was found to increase by two magnitudes higher with the chemical modification of chitosan. The highest conductivity achieved was 3.6 × 10 −6 S cm −1 for carboxymethyl chitosan at room temperature and 3.7 × 10 −4 S cm −1 at 60 °C

  8. A novel glucose biosensor based on phosphonic acid-functionalized silica nanoparticles for sensitive detection of glucose in real samples

    International Nuclear Information System (INIS)

    Zhao, Wenbo; Fang, Yi; Zhu, Qinshu; Wang, Kuai; Liu, Min; Huang, Xiaohua; Shen, Jian

    2013-01-01

    An effective strategy for preparation amperometric biosensor by using the phosphonic acid-functionalized silica nanoparticles (PFSi NPs) as special modified materials is proposed. In such a strategy, glucose oxidase (GOD) was selected as model protein to fabricate glucose biosensor in the presence of phosphonic acid-functionalized silica nanoparticles (PFSi NPs). The PFSi NPs were first modified on the surface of glassy carbon (GC) electrode, then, GOD was adsorbed onto the PFSi NPs film by drop-coating. The PFSi NPs were characterized by transmission electron microscopy (TEM) and nuclear magnetic resonance (NMR) spectra. The interaction of PFSi NPs with GOD was investigated by the circular dicroism spectroscopy (CD). The results showed PFSi NPs could essentially maintain the native conformation of GOD. The direct electron transfer of GOD on (PFSi NPs)/GCE electrode exhibited excellent electrocatalytic activity for the oxidation of glucose. The proposed biosensor modified with PFSi NPs displayed a fast amperometric response (5 s) to glucose, a good linear current–time relation over a wide range of glucose concentrations from 5.00 × 10 −4 to 1.87 × 10 −1 M, and a low detection limit of 2.44 × 10 −5 M (S/N = 3). Moreover, the biosensor can be used for assessment of the concentration of glucose in many real samples (relative error < 3%). The GOD biosensor modified with PFSi NPs will have essential meaning and practical application in future that attributed to the simple method of fabrication and good performance

  9. Sorption of technetium on composite chitosan-hydroxyapatite from aqueous solutions

    International Nuclear Information System (INIS)

    Pivarciova, L.; Rosskopfova, O.; Galambos, M.; Rajec, P.

    2013-01-01

    Biomaterials such as natural polymers (chitosan) and hydroxyapatite have an important application in material for bone replacement. Most of chitosan/hydroxyapatite composites are prepared by mixing hydroxyapatite particles with chitosan matrices. Another method of preparation of chitosan/hydroxyapatite composite is in-situ generation of nano-hydroxyapatite in chitosan matrix. The most common biomaterial used in the past years in hard tissue regeneration was hydroxyapatite, owing to its properties as biocompatibility, bioactivity, non-toxicity, non-immunogenicity etc. Chitosan is a polyaminosacharide, partially deacetylated product of chitin. Chitosan can be used in combination with other materials to enhance bone growth such as bone filling paste. The aims of this work were: the influence of the contact time on sorption of pertechnate anions on chitosan/hydroxyapatite composites; the effect of pH on sorption of pertechnate anions on chitosan/hydroxyapatite composites; the effect of foreign ions on sorption of pertechnate anions on chitosan/hydroxyapatite composites. The author concluded: the percentage of technetium sorption after 1 hour of contact time was > 97 %. In the initial pH range of 2.9-10.2, the percentage of technetium sorption on chitosan/hydroxyapatite composites CH/HA(A), CH/HA(B), CH/HA 30:70, ZCH was > 98 % and on CH/HA 50:50 was > 94%. The competition effect of Fe 2+ towards TcO 4 :- sorption is stronger than competition effect of other observed cations for all examined composites with the same weight ratio. The percentage of the technetium sorption was the same for all composites with the weight ratio of 30:70. (authors)

  10. Novel procedure to enhance PLA surface properties by chitosan irreversible immobilization

    Energy Technology Data Exchange (ETDEWEB)

    Stoleru, Elena; Dumitriu, Raluca Petronela [Petru Poni Institute of Macromolecular Chemistry, Grigore Ghica Voda Alley, 41A, 700487 Iasi (Romania); Munteanu, Bogdanel Silvestru [“Al. I. Cuza” University, Faculty of Physics, 11 Carol I Blvd., 700506 Iasi (Romania); Zaharescu, Traian [INCDIE ICPE CA, Bucharest (Romania); Tănase, Elisabeta Elena; Mitelut, Amalia [Industrial Biotechnology Department, Faculty of Biotechnology – USAMV Bucharest (Romania); Ailiesei, Gabriela-Liliana [Petru Poni Institute of Macromolecular Chemistry, Grigore Ghica Voda Alley, 41A, 700487 Iasi (Romania); Vasile, Cornelia, E-mail: cvasile@icmpp.ro [Petru Poni Institute of Macromolecular Chemistry, Grigore Ghica Voda Alley, 41A, 700487 Iasi (Romania)

    2016-03-30

    Graphical abstract: - Highlights: • PLA requires functionalization prior to surface attaching chitosan. • Chitosan with different molecular weights was grafted onto PLA surface. • Antibacterial, antifungal, antioxidant PLA-based materials are obtained. • Nano-fibers coatings obtained by electrospinning of high molecular weight chitosan. - Abstract: A novel two step procedure was applied for poly(lactic acid) (PLA) functionalization consisting in the exposure to cold radiofrequency plasma in nitrogen atmosphere or to gamma irradiation followed by “grafting to” of a chitosan layer using carbodiimide chemistry. The adhesion and stability of the deposited surface layer was assured by plasma/gamma irradiation treatment while the chitosan layer offers antifungal/antibacterial/antioxidant activities. Chitosan with different viscosities/deacetylation degree was deposited by electrospinning or immersion methods. Correlations between rheological behavior of chitosan solutions and chitosan layer deposition conditions are made. The PLA surface properties were investigated by water contact angle measurements, ATR-FTIR spectroscopy, AFM, chemiluminiscence, etc. It has been established that the surface roughness increases direct proportional with cold plasma duration and gamma irradiation dose and further increases by chitosan coating which at its turn depends on chitosan characteristics (viscosity and deacetylation degree) and method of deposition. Nano-fibers with relatively homogeneous and reproducible features are obtained by electrospinning of highly viscous chitosan while with the other two types of chitosan both microparticles and nano-fibers are formed. The chitosan coating obtained by immersion is more homogenous and compact and has a better antibacterial activity than the electrospun layer as fiber meshes.

  11. Viscometric studies of chitosan radiation degradation

    International Nuclear Information System (INIS)

    Rapado, M.; Ceausoglu, I.; Hunkeler, D.

    2001-01-01

    The paper presents the preliminary results, related to the viscometric studies on chitosan gamma radiation degradation. To follow the effects on the processes of chitosan transformations caused by irradiation in vacuum irradiated solutions changes of viscosity, and viscosity average molecular weight were measured The influence of absorbed dose on the chitosan molecular weight was studied using the Mark-Houwink-Sakurada equation. Various relationships for the for the determination of the intrinsic viscosity were made vias the Huggins, Kramer and Schulz- Blaschke models. The distinct decrease of intrinsic viscosity indicates that the main change scission was the dominating process

  12. Synthesis and Properties of a Novel Type of Acyclic Nucleoside Phosphonates: 2-(Purin-9-yl)ethoxyphenylphosphonic Acids

    Czech Academy of Sciences Publication Activity Database

    Hocková, Dana; Dračínský, Martin; Holý, Antonín

    -, č. 15 (2010), s. 2885-2892 ISSN 1434-193X R&D Projects: GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z40550506 Keywords : nucleotides * phosphonates * cross-coupling Subject RIV: CC - Organic Chemistry Impact factor: 3.206, year: 2010

  13. Chitosan-Based Polymer Blends: Current Status and applications

    International Nuclear Information System (INIS)

    Hefian, E.A.E.; Nasef, M.M.

    2014-01-01

    This paper reviews the latest developments in chitosan-based blends and their potential applications in various fields. Various blends together with other derivatives, such as composites and graft copolymers, have been developed to overcome chitosans disadvantages, including poor mechanical properties and to improve its functionality towards specific applications. The progress made in blending chitosan with synthetic and natural polymers is presented. The versatility and unique characteristics, such as hydrophilicity, film-forming ability, biodegradability, biocompatibility, antibacterial activity and non-toxicity of chitosan has contributed to the successful development of various blends for medical, pharmaceutical, agricultural and environmental applications. (author)

  14. Investigation of Galactosylated Low Molecular Weight Chitosan ...

    African Journals Online (AJOL)

    was coupled with low molecular weight chitosan (LMWC) using carbodiimide chemistry. .... High molecular weight chitosan (minimum 85% ..... membrane permeability of drug and mutual repulsion ... coating thickness and the lower solubility of.

  15. Chitosan-glycerol phosphate/blood implants elicit hyaline cartilage repair integrated with porous subchondral bone in microdrilled rabbit defects.

    Science.gov (United States)

    Hoemann, C D; Sun, J; McKee, M D; Chevrier, A; Rossomacha, E; Rivard, G-E; Hurtig, M; Buschmann, M D

    2007-01-01

    We have previously shown that microfractured ovine defects are repaired with more hyaline cartilage when the defect is treated with in situ-solidified implants of chitosan-glycerol phosphate (chitosan-GP) mixed with autologous whole blood. The objectives of this study were (1) to characterize chitosan-GP/blood clots in vitro, and (2) to develop a rabbit marrow stimulation model in order to determine the effects of the chitosan-GP/blood implant and of debridement on the formation of incipient cartilage repair tissue. Blood clots were characterized by histology and in vitro clot retraction tests. Bilateral 3.5 x 4 mm trochlear defects debrided into the calcified layer were pierced with four microdrill holes and filled with a chitosan-GP/blood implant or allowed to bleed freely as a control. At 1 day post-surgery, initial defects were characterized by histomorphometry (n=3). After 8 weeks of repair, osteochondral repair tissues between or through the drill holes were evaluated by histology, histomorphometry, collagen type II expression, and stereology (n=16). Chitosan-GP solutions structurally stabilized the blood clots by inhibiting clot retraction. Treatment of drilled defects with chitosan-GP/blood clots led to the formation of a more integrated and hyaline repair tissue above a more porous and vascularized subchondral bone plate compared to drilling alone. Correlation analysis of repair tissue between the drill holes revealed that the absence of calcified cartilage and the presence of a porous subchondral bone plate were predictors of greater repair tissue integration with subchondral bone (Phyaline and integrated repair tissue associated with a porous subchondral bone replete with blood vessels. Concomitant regeneration of a vascularized bone plate during cartilage repair could provide progenitors, anabolic factors and nutrients that aid in the formation of hyaline cartilage.

  16. Amino Groups of Chitosan Are Crucial for Binding to a Family 32 Carbohydrate Binding Module of a Chitosanase from Paenibacillus elgii*

    Science.gov (United States)

    Das, Subha Narayan; Wagenknecht, Martin; Nareddy, Pavan Kumar; Bhuvanachandra, Bhoopal; Niddana, Ramana; Balamurugan, Rengarajan; Swamy, Musti J.; Moerschbacher, Bruno M.; Podile, Appa Rao

    2016-01-01

    We report here the role and mechanism of specificity of a family 32 carbohydrate binding module (CBM32) of a glycoside hydrolase family 8 chitosanase from Paenibacillus elgii (PeCsn). Both the activity and mode of action of PeCsn toward soluble chitosan polymers were not different with/without the CBM32 domain of P. elgii (PeCBM32). The decreased activity of PeCsn without PeCBM32 on chitosan powder suggested that PeCBM32 increases the relative concentration of enzyme on the substrate and thereby enhanced enzymatic activity. PeCBM32 specifically bound to polymeric and oligomeric chitosan and showed very weak binding to chitin and cellulose. In isothermal titration calorimetry, the binding stoichiometry of 2 and 1 for glucosamine monosaccharide (GlcN) and disaccharide (GlcN)2, respectively, was indicative of two binding sites in PeCBM32. A three-dimensional model-guided site-directed mutagenesis and the use of defined disaccharides varying in the pattern of acetylation suggested that the amino groups of chitosan and the polar residues Glu-16 and Glu-38 of PeCBM32 play a crucial role for the observed binding. The specificity of CBM32 has been further elucidated by a generated fusion protein PeCBM32-eGFP that binds to the chitosan exposing endophytic infection structures of Puccinia graminis f. sp. tritici. Phylogenetic analysis showed that CBM32s appended to chitosanases are highly conserved across different chitosanase families suggesting their role in chitosan recognition and degradation. We have identified and characterized a chitosan-specific CBM32 useful for in situ staining of chitosans in the fungal cell wall during plant-fungus interaction. PMID:27405759

  17. In vivo evaluation of thiolated chitosan tablets for oral insulin delivery.

    Science.gov (United States)

    Millotti, Gioconda; Laffleur, Flavia; Perera, Glen; Vigl, Claudia; Pickl, Karin; Sinner, Frank; Bernkop-Schnürch, Andreas

    2014-10-01

    Chitosan-6-mercaptonicotinic acid (chitosan-6-MNA) is a thiolated chitosan with strong mucoadhesive properties and a pH-independent reactivity. This study aimed to evaluate the in vivo potential for the oral delivery of insulin. The comparison of the nonconjugated chitosan and chitosan-6-MNA was performed on several studies such as mucoadhesion, release, and in vivo studies. Thiolated chitosan formulations were both about 80-fold more mucoadhesive compared with unmodified ones. The thiolated chitosan tablets showed a sustained release for 5 h for the polymer of 20 kDa and 8 h for the polymer of 400 kDa. Human insulin was quantified in rats' plasma by means of ELISA specific for human insulin with no cross-reactivity with the endogenous insulin. In vivo results showed thiolation having a tremendous impact on the absorption of insulin. The absolute bioavailabilities were 0.73% for chitosan-6-MNA of 20 kDa and 0.62% for chitosan-6-MNA 400 kDa. The areas under the concentration-time curves (AUC) of chitosan-6-MNA formulations compared with unmodified chitosan were 4.8-fold improved for the polymer of 20 kDa and 21.02-fold improved for the polymer of 400 kDa. The improvement in the AUC with regard to the most promising aliphatic thiomer was up to 6.8-fold. Therefore, chitosan-6-MNA represents a promising excipient for the oral delivery of insulin. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

  18. The molecular understanding of interfacial interactions of functionalized graphene and chitosan

    International Nuclear Information System (INIS)

    Zhang, Hong-ping; Luo, Xue-gang; Lin, Xiao-yan; Lu, Xiong; Tang, Youhong

    2016-01-01

    Graphical abstract: The type of the functional groups can be used to modulating interactions between graphene sheet and chitosan. - Highlights: • Investigate interfacial interactions between chitosan and functionalized graphene by DFT. • Observe covalent linkages between COOH-modified graphene and chitosan units. • Multi-functionalized graphene regulates the interfacial interactions with chitosan. • It is useful for guiding the preparation of graphene/chitosan composites. - Abstract: Graphene-reinforced chitosan scaffolds have been extensively studied for several years as promising hard tissue replacements. However, the interfacial interactions between graphene and chitosan are strongly related to the solubility, processability, and mechanical properties of graphene-reinforced chitosan (G–C) composites. The functionalization of graphene is regarded as the most effective way to improve the abovementioned properties of the G–C composite. In this study, the interfacial interactions between chitosan and functionalized graphene sheets with carboxylization (COOH-), amination (NH 2 -), and hydroxylation (OH-) groups were systematically studied at the electronic level using the method of ab initio simulations based on quantum mechanics theory and the observations were compared with reported experimental results. The covalent linkages between COOH-modified graphene and the chitosan units were demonstrated and the combination of multi-functionalization on graphene could regulate the interfacial interactions between graphene and the chitosan. The interfacial interactions between chitosan and properly functionalized graphene are critical for the preparation of G–C-based composites for tissue engineering scaffolds and other applications.

  19. Nanotubo de carbono-chitosan en células HOS y THP-1 Carbon nanotubes-chitosan in HOS and THP-1 cells

    Directory of Open Access Journals (Sweden)

    John Jairo Castillo León

    2011-04-01

    Full Text Available Introducción: Los nanotubos de carbono (NTC son estructuras nanométricas utilizadas en el tratamiento de enfermedades, principalmente en la entrega de fármacos para terapias en cáncer. Objetivos: Estudiar la internalización de NTC acoplado a quitosan (NTC-Q en células de osteosarcoma humano (HOS y monocitos humanos de leucemia aguda (THP-1. Materiales y métodos: Los NTC solubilizados con quitosan 30% fueron caracterizados espectroscópicamente por UV-Vis, fluorescencia y Raman. Las células HOS y THP-1 fueron tratadas con NTC-Q y se evaluó la internalización por tinción de Giemsa en microscopio de luz y la citotóxicidad utilizando la prueba fluorométrica de Azul de Alamar. Resultados: Los espectros Raman y de fluorescencia mostraron la funcionalización de los NTC con quitosan. Los NTC fueron internalizados por las líneas celulares después de 24 h mostrando una ubicación citoplasmática sin presentar citotóxicidad en ninguna de las células evaluadas. Discusión: Las características presentadas por los NTC-Q les brinda la posibilidad de ser utilizados como transportadores de fármacos. Salud UIS 2011; 43(1: 21-26Introduction: Carbon nanotubes (CNT are nanometer-sized structures used in medicine in the treatment of diseases, mainly in drug delivery in therapies against cancer. Objectives: To Study the internalization of carbon nanotubes modified with chitosan (CNT-CH in human osteosarcom cells (HOS and human monocytes of acute leukemia (THP1. Materials and methods: The CNTs solubilized in chitosan 30% were characterized spectroscopically by UV-Vis, fluorescence and Raman. HOS cells and THP-1 were treated with CNT-CH, the internalization was evaluated by Giemsa staining with light microscopy, and cytotoxicity was determined using Alamar Blue assay. Results: Raman and fluorescence spectra showed the functionalization of the CNT with chitosan. After 24 h the NTC were internalized in the cell lines showing a cytoplasmic location and

  20. Highly Response and Sensitivity Chitosan-Polyvinyl alcohol Based Hexanal Sensors

    Directory of Open Access Journals (Sweden)

    Abd Wahab Nur Zuraihan

    2016-01-01

    Full Text Available This work is to study the sensing properties of chitosanpolyvinyl alcohol film sensors upon hexanal gas exposure using vapour sensing technique. The sensor fabrication process was done using electrochemical deposition method by deposit the sensing materials on the gold patterned electrode with chitosan/PVA. The response value of chitosan-PVA film sensors towards hexanal was taken as an output voltage using electrical testing method. In this study, 1.75% of chitosan with 5% of PVA were mixed with the ratio of (95:5 was tested upon exposure to hexanal gas. The concentration of the hexanal was varied as 10 ppm, 20 ppm, 30 ppm. It was found that the chitosan-PVA film sensors showed fast response, stable, good stability, good recovery, repeatable and good sensitivity towards hexanal exposure. The morphology of the pure chitosan and chitosan-PVA was analyzed by scanning electron microscope (SEM and the interaction between chitosan and PVA was examined by Fourier Transform Infrared Spectroscopy (FTIR. The FTIR results indicate the changes in characteristics of the spectral peaks due to the formation of the intermolecular bonds between chitosan and PVA. The SEM morphology of the composites showed flat smooth surface that be a sign of uniform distribution of chitosan and PVA mixture throughout the films.

  1. Fabrication and application of coaxial polyvinyl alcohol/chitosan nanofiber membranes

    Directory of Open Access Journals (Sweden)

    Kuo Ting-Yun

    2017-12-01

    Full Text Available It is difficult to fabricate chitosan-wrapped coaxial nanofibers, because highly viscous chitosan solutions might hinder the manufacturing process. To overcome this difficulty, our newly developed method, which included the addition of a small amount of gum arabic, was utilized to prepare much less viscous chitosan solutions. In this way, coaxial polyvinyl alcohol (PVA/chitosan (as core/shell nanofiber membranes were fabricated successfully by coaxial electrospinning. The core/shell structures were confirmed by TEM, and the existence of PVA and chitosan was also verified using FT-IR and TGA. The tensile strength of the nanofiber membranes was increased from 0.6-0.7 MPa to 0.8-0.9 MPa after being crosslinked with glutaraldehyde. The application potential of the PVA/chitosan nanofiber membranes was tested in drug release experiments by loading the core (PVA with theophylline as a model drug. The use of the coaxial PVA/chitosan nanofiber membranes in drug release extended the release time of theophylline from 5 minutes to 24 hours. Further, the release mechanisms could be described by the Korsmeyer-Peppas model. In summary, by combining the advantages of PVA and chitosan (good mechanical strength and good biocompatibility respectively, the coaxial PVA/chitosan nanofiber membranes are potential biomaterials for various biomedical applications.

  2. Study on growth-promotion of paddy plants treated with oligo chitosan

    International Nuclear Information System (INIS)

    Norhashidah Talip; Maznah Mahmud; Norzita Yacob; Kamaruddin Hashim; Khairul Zaman Mohd Dahlan

    2010-01-01

    Chitosan has been degraded to produced oligo chitosan with different molecular weight using gamma ray irradiation from a Co-60 source in solid state (powder form) and liquid state (aqueous solution). Study on growth promotion of paddy plants was done using oligo chitosan and conventional plant growth promoter as a comparison. Oligo chitosan was used with different molecular weight and different concentrations. Smaller molecular weight of oligo chitosan with smaller concentration showed better result than bigger molecular weight of oligo chitosan as a plant growth promoter. This study also showed that conventional growth promoter can be replaced with oligo chitosan as it is more effective as plant growth promoter as well as more environmental friendly. (author)

  3. Chitosan: An Update on Potential Biomedical and Pharmaceutical Applications

    Directory of Open Access Journals (Sweden)

    Randy Chi Fai Cheung

    2015-08-01

    Full Text Available Chitosan is a natural polycationic linear polysaccharide derived from chitin. The low solubility of chitosan in neutral and alkaline solution limits its application. Nevertheless, chemical modification into composites or hydrogels brings to it new functional properties for different applications. Chitosans are recognized as versatile biomaterials because of their non-toxicity, low allergenicity, biocompatibility and biodegradability. This review presents the recent research, trends and prospects in chitosan. Some special pharmaceutical and biomedical applications are also highlighted.

  4. Chitosan: An Update on Potential Biomedical and Pharmaceutical Applications

    Science.gov (United States)

    Cheung, Randy Chi Fai; Ng, Tzi Bun; Wong, Jack Ho; Chan, Wai Yee

    2015-01-01

    Chitosan is a natural polycationic linear polysaccharide derived from chitin. The low solubility of chitosan in neutral and alkaline solution limits its application. Nevertheless, chemical modification into composites or hydrogels brings to it new functional properties for different applications. Chitosans are recognized as versatile biomaterials because of their non-toxicity, low allergenicity, biocompatibility and biodegradability. This review presents the recent research, trends and prospects in chitosan. Some special pharmaceutical and biomedical applications are also highlighted. PMID:26287217

  5. Complications of Methylene Blue Dye in Breast Surgery: Case Reports and Review of the Literature

    Directory of Open Access Journals (Sweden)

    FJ Reyes, MB Noelck, C Valentino, L Grasso-LeBeau, JE Lang

    2011-01-01

    Full Text Available Introduction: Methylene blue dye has been used worldwide successfully with few complications in breast surgery. We present two different complications involving methylene blue: 1 skin and parenchymal necrosis when dye was injected in a subdermal fashion and 2 Mycoplasma infection caused by contaminated methylene blue in breast reduction surgery.Methods: We present two cases seen at the University of Arizona during 2008 and referred to a breast surgeon for management. We evaluated and managed complications of methylene blue dye injected by 2 referring surgeons for different indications. A review of the literature was performed.Results: The first case is a 67 year old female diagnosed with infiltrating ductal carcinoma of the left breast for which she was treated by her initial surgeon with left segmental mastectomy and sentinel node biopsy. The operating surgeon injected methylene blue in a subareolar subdermal fashion (distant from the primary tumor; unfortunately the patient suffered skin and breast necrosis requiring multiple surgical debridements and finally achieving delayed primary closure. The second case is a 45 year old female with infiltrating lobular carcinoma with a history of Mycoplasma infection secondary to methylene blue injected for breast reduction surgery. She required multiple debridements and had granulomas masquerading as cancer on MRI that confounded her extent of disease.Conclusions: The use of methylene blue dye in breast surgery is not without risk. In both cases methylene blue was responsible for complications requiring surgical debridement for local wound problems. In each case severe necrosis and infection were present. Methylene blue may cause not only significant morbidity, but may also produce cosmetically unsatisfactory results.

  6. Inhibition of hypoxanthine-guanine phosphoribosyltransferase by acyclic nucleoside phosphonates: A new class of antimalarial therapeutics

    Czech Academy of Sciences Publication Activity Database

    Keough, D. T.; Hocková, Dana; Holý, Antonín; Naesens, L.; Skinner-Adams, T. S.; de Jersey, J.; Guddat, L. W.

    2009-01-01

    Roč. 52, č. 14 (2009), s. 4391-4399 ISSN 0022-2623 R&D Projects: GA MŠk 1M0508; GA AV ČR 1QS400550501 Institutional research plan: CEZ:AV0Z40550506 Keywords : acyclic nucleoside phosphonates * phosphoribosyltransferase * enzyme inhibitors * Plasmodium falciparum Subject RIV: CC - Organic Chemistry Impact factor: 4.802, year: 2009

  7. Chitosan as a bioactive polymer: Processing, properties and applications.

    Science.gov (United States)

    Muxika, A; Etxabide, A; Uranga, J; Guerrero, P; de la Caba, K

    2017-12-01

    Chitin is one of the most abundant natural polysaccharides in the world and it is mainly used for the production of chitosan by a deacetylation process. Chitosan is a bioactive polymer with a wide variety of applications due to its functional properties such as antibacterial activity, non-toxicity, ease of modification, and biodegradability. This review summarizes the most common chitosan processing methods and highlights some applications of chitosan in various industrial and biomedical fields. Finally, environmental concerns of chitosan-based films, considering the stages from raw materials extraction up to the end of life after disposal, are also discussed with the aim of finding more eco-friendly alternatives. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. The production of fully deacetylated chitosan by compression method

    Directory of Open Access Journals (Sweden)

    Xiaofei He

    2016-03-01

    Full Text Available Chitosan’s activities are significantly affected by degree of deacetylation (DDA, while fully deacetylated chitosan is difficult to produce in a large scale. Therefore, this paper introduces a compression method for preparing 100% deacetylated chitosan with less environmental pollution. The product is characterized by XRD, FT-IR, UV and HPLC. The 100% fully deacetylated chitosan is produced in low-concentration alkali and high-pressure conditions, which only requires 15% alkali solution and 1:10 chitosan powder to NaOH solution ratio under 0.11–0.12 MPa for 120 min. When the alkali concentration varied from 5% to 15%, the chitosan with ultra-high DDA value (up to 95% is produced.

  9. A novel bio-degradable polymer stabilized Ag/TiO2 nanocomposites and their catalytic activity on reduction of methylene blue under natural sun light.

    Science.gov (United States)

    Geetha, D; Kavitha, S; Ramesh, P S

    2015-11-01

    In the present work we defined a novel method of TiO2 doped silver nanocomposite synthesis and stabilization using bio-degradable polymers viz., chitosan (Cts) and polyethylene glycol (PEG). These polymers are used as reducing agents. The instant formation of AgNPs was analyzed by visual observation and UV-visible spectrophotometer. TiO2 nanoparticles doped at different concentrations viz., 0.03, 0.06 and 0.09mM on PEG/Cts stabilized silver (0.04wt%) were successfully synthesized. This study presents a simple route for the in situ synthesis of both metal and polymer confined within the nanomaterial, producing ternary hybrid inorganic-organic nanomaterials. The results reveal that they have higher photocatalytic efficiencies under natural sun light. The synthesized TiO2 doped Ag nanocomposites (NCs) were characterized by SEM/EDS, TEM, XRD, FTIR and DLS with zeta potential. The stability of Ag/TiO2 nanocomposite is due to the high negative values of zeta potential and capping of constituents present in the biodegradable polymer which is evident from zeta potential and FT-IR studies. The XRD and EDS pattern of synthesized Ag/TiO2 NCs showed their crystalline structure, with face centered cubic geometry oriented in (111) plane. AFM and DLS studies revealed that the diameter of stable Ag/TiO2 NCs was approximately 35nm. Moreover the catalytic activity of synthesize Ag/TiO2 NCs in the reduction of methylene blue was studied by UV-visible spectrophotometer. The synthesized Ag/TiO2 NCs are observed to have a good catalytic activity on the reduction of methylene blue by bio-degradable which is confirmed by the decrease in absorbance maximum value of methylene blue with respect to time using UV-vis spectrophotometer. The significant enhancement in the photocatalytic activity of Ag/TiO2 nanocomposites under sun light irradiation can be ascribed to the effect of noble metal Ag by acting as electron traps in TiO2 band gap. Copyright © 2015. Published by Elsevier Inc.

  10. Label-free electrochemical analysis of chitosan and glucosamine-containing oligosaccharides

    Czech Academy of Sciences Publication Activity Database

    Paleček, Emil

    2016-01-01

    Roč. 187, JAN 1 2016 (2016), s. 375-380 ISSN 0013-4686 R&D Projects: GA ČR(CZ) GA15-15479S Institutional support: RVO:68081707 Keywords : Chitosan * Glucosamine-containing oligosaccharides * Alkaline deacetylation of N-acetylated glycans Subject RIV: BO - Biophysics Impact factor: 4.798, year: 2016

  11. Nuclear imaging evaluation of galactosylation of chitosan

    International Nuclear Information System (INIS)

    Jeong, Hwan Jeong; Kim, Eun Mi; Kim, Chang Guhn; Park, In Kyu; Cho, Chong Su; Bom, Hee Seung

    2004-01-01

    Chitosan has been studied as a non-viral gene delivery vector, drug delivery carrier, metal chelater, food additive, and radiopharmaceutical, among other things. Recently, galactose-graft chitosan was studied as a non-viral gene and drug delivery vector to target hepatocytes. The aim of this study was to investigate the usefulness of nuclear imaging for in vivo evaluation of targeting the hepatocyte by galactose grafting. Galactosyl methylated chitosan (GMC) was produced by methylation to lactobionic acid coupled chitosan Cytotoxicity of 99 mTc-GMC was determined by MTT assay. Rabbits were injected via their auricular vein with 99 mTc-GMC and 99 mTc-methylated chitosan (MC), the latter of which does not contain a galactose group, and images were acquired with a gamma camera equipped with a parallel hole collimator. The composition of the galactose group in galactosylated chitosan (GC), as well as the tri-, di-, or mono-methylation of GMC, was confirmed by NMR spectroscopy. The results of MTT assay indicated that 99 mTc-GMC was non-toxic. 99 mTc-GMC specifically accumulated in the liver within 10 minutes of injection and maintained high hepatic uptake. In contrast, 99 mTc-MC showed faint liver uptake. 99 mTc-GMC scintigraphy of rabbits showed that the galactose ligand principally targeted the liver while the chitosan functionalities led to excretion through the urinary system. Bioconjugation with a specific ligand endows some degree of targetability to an administered molecule or drug, as in the case of galactose for hepatocyte in vivo, and evaluating said targetability is a clear example of the great benefit proffered by nuclear imaging

  12. Chitosan microspheres in novel drug delivery systems.

    Science.gov (United States)

    Mitra, Analava; Dey, Baishakhi

    2011-07-01

    The main aim in the drug therapy of any disease is to attain the desired therapeutic concentration of the drug in plasma or at the site of action and maintain it for the entire duration of treatment. A drug on being used in conventional dosage forms leads to unavoidable fluctuations in the drug concentration leading to under medication or overmedication and increased frequency of dose administration as well as poor patient compliance. To minimize drug degradation and loss, to prevent harmful side effects and to increase drug bioavailability various drug delivery and drug targeting systems are currently under development. Handling the treatment of severe disease conditions has necessitated the development of innovative ideas to modify drug delivery techniques. Drug targeting means delivery of the drug-loaded system to the site of interest. Drug carrier systems include polymers, micelles, microcapsules, liposomes and lipoproteins to name some. Different polymer carriers exert different effects on drug delivery. Synthetic polymers are usually non-biocompatible, non-biodegradable and expensive. Natural polymers such as chitin and chitosan are devoid of such problems. Chitosan comes from the deacetylation of chitin, a natural biopolymer originating from crustacean shells. Chitosan is a biocompatible, biodegradable, and nontoxic natural polymer with excellent film-forming ability. Being of cationic character, chitosan is able to react with polyanions giving rise to polyelectrolyte complexes. Hence chitosan has become a promising natural polymer for the preparation of microspheres/nanospheres and microcapsules. The techniques employed to microencapsulate with chitosan include ionotropic gelation, spray drying, emulsion phase separation, simple and complex coacervation. This review focuses on the preparation, characterization of chitosan microspheres and their role in novel drug delivery systems.

  13. Evaluation of dose dependent antimicrobial activity of self-assembled chitosan, nano silver and chitosan-nano silver composite against several pathogens.

    Science.gov (United States)

    Tareq, Foysal Kabir; Fayzunnesa, Mst; Kabir, Md Shahariar; Nuzat, Musrat

    2018-01-01

    The aim of this investigation to preparation of silver nanoparticles organized chitosan nano polymer, which effective against microbial and pathogens, when apply to liquid medium and edible food products surface, will rescue the growth of microbes. Self-assembly approach used to synthesis of silver nanoparticles and silver nanoparticles organized chitosan nano polymer. Silver nanoparticles and silver nanoparticles organized chitosan nano polymer and film characterized using Ultra-violate visible spectrometer (UV-vis), X-ray diffraction (X-ray), and Scanning electronic microscope (SEM). The crystalline structured protein capped nano silver successfully synthesized at range of 12 nm-29 nm and organized into chitosan nano polymer. Antimicrobial ingredient in liquid medium and food product surface provide to rescue oxidative change and growth of microorganism to provide higher safety. The silver nanoparticles organized chitosan nano polymer caused the death of microorganism. The materials in nano scale synthesized successfully using self-assembly method, which showed good antimicrobial properties. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. A step-by-step approach to study the influence of N-acetylation on the adjuvanticity of N,N,N-trimethyl chitosan (TMC) in an intranasal nanoparticulate influenza virus vaccine.

    Science.gov (United States)

    Verheul, Rolf J; Hagenaars, Niels; van Es, Thomas; van Gaal, Ethlinn V B; de Jong, Pascal H J L F; Bruijns, Sven; Mastrobattista, Enrico; Slütter, Bram; Que, Ivo; Heldens, Jacco G M; van den Bosch, Han; Glansbeek, Harrie L; Hennink, Wim E; Jiskoot, Wim

    2012-03-12

    Recently we reported that reacetylation of N,N,N-trimethyl chitosan (TMC) reduced the adjuvant effect of TMC in mice after intranasal (i.n.) administration of whole inactivated influenza virus (WIV) vaccine. The aim of the present study was to elucidate the mechanism of this lack of adjuvanticity. Reacetylated TMC (TMC-RA, degree of acetylation 54%) was compared with TMC (degree of acetylation 17%) at six potentially critical steps in the induction of an immune response after i.n. administration in mice. TMC-RA was degraded in a nasal wash to a slightly larger extent than TMC. The local i.n. distribution and nasal clearance of WIV were similar for both TMC types. Fluorescently labeled WIV was taken up more efficiently by Calu-3 cells when formulated with TMC-RA compared to TMC and both TMCs significantly reduced transport of WIV over a Calu-3 monolayer. Murine bone-marrow derived dendritic cell activation was similar for plain WIV, and WIV formulated with TMC-RA or TMC. The inferior adjuvant effect in mice of TMC-RA over that of TMC might be caused by a slightly lower stability of TMC-RA-WIV in the nasal cavity, rather than by any of the other factors studied in this paper. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Inhibition of the Escherichia coli 6-oxopurine phosphoribosyltransferases by nucleoside phosphonates: potential for new antibacterial agents

    Czech Academy of Sciences Publication Activity Database

    Keough, D. T.; Hocková, Dana; Rejman, Dominik; Špaček, Petr; Vrbková, Silvie; Krečmerová, Marcela; Eng, W. S.; Jans, H.; West, N. P.; Naesens, L. M. J.; de Jersey, J.; Guddat, L. W.

    2013-01-01

    Roč. 56, č. 17 (2013), s. 6967-6984 ISSN 0022-2623 R&D Projects: GA ČR GAP207/11/0108 Institutional support: RVO:61388963 Keywords : nucleoside phosphonates * antibacterial agents * hypoxanthine-guanine phosphoribosyltransferase * state analog inhibitor * antimalarial chemotherapy Subject RIV: CC - Organic Chemistry Impact factor: 5.480, year: 2013

  16. Synthesis of PVA-Chitosan Hydrogels for Wound Dressing Using Gamma Irradiation. Part II: Antibacterial Activity of PVA/Chitosan Hydrogel Synthesized by Gamma Irradiation

    International Nuclear Information System (INIS)

    Mahlous, M.; Tahtat, D.; Benamer, S.; Nacer Khodja, A.; Larbi Youcef, S.

    2010-01-01

    Poly(vinyl alcohol) (PVA) is a synthetic polymer used in a large range of medical, commercial, industrial and food applications, manufacture of paper products, surgical threads, wound care, and food-contact applications. It was recently used as a coating for dietary supplements and pharmaceutical capsules. Cross-linked PVA microspheres are also used for controlled release of oral drugs. Chitin, a polysaccharide from which chitosan is derived, is the second most abundant natural polysaccharide after cellulose. Chitin is obtained from the exoskeletons (crab, shrimps and squid pen) fungi, insects, and some algae. Chitosan, a non toxic and biocompatible cationic polysaccharide, is produced by partial deacetylation of chitin; these properties of chitosan provide high potential for many applications. Chitosan has been widely used in vastly diverse fields, such as in biomedical applications drug delivery in agriculture metal ion sorption. The most important characteristic of chitosan is the deacetylation degree (DD) which influences its physical and chemical behaviors. Evaluation of DD can be carried out by FT-IR spectroscopy potentiometric titration, first derivative UV spectrophotometry, 1 H-NMR and X-ray diffraction. Chitosan extracted from squid pen chitin is inherently purer than crustacean chitosans, it does not contain large amounts of calcium carbonate, and it does contain large amounts of protein. The purity of squid pen chitosan makes it particularly suitable for medical and cosmetic application. Application of radiation for the formation of hydrogels for medical use offers a unique possibility to combine the formation and sterilization of the product in a single technological step. The main aim of this study is to synthesis poly(vinyl alcohol) hydrogels containing different moieties of chitosan by gamma irradiation at a dose of 25 kGy, and investigate the antibacterial effect of chitosan contained in the hydrogel

  17. Development of hydroxyapatite-chitosan gel sunscreen combating clinical multidrug-resistant bacteria

    Science.gov (United States)

    Morsy, Reda; Ali, Sameh S.; El-Shetehy, Mohamed

    2017-09-01

    The several harmful effects on infected human skin resulting from exposure to the sun's UV radiation generate an interest in the development of a multifunctional hydroxyapatite-chitosan (HAp-chitosan) gel that works as an antibacterial sunscreen agent for skin care. In this work, HAp-chitosan gel was synthesized via coprecipitation method by dissolving chitosan in phosphoric acid and adding HAp. The characteristics of HAp-chitosan composite were investigated by conventional techniques, such as XRD, FTIR, and SEM techniques, while its sunscreen property was investigated by UV-spectroscopy. In addition to the influence of the gel on bacterial cell morphology, the antibacterial activity of HAp-chitosan gel against clinical multidrug resistant skin pathogens, such as Staphylococcus aureus, Klebsiella pneumoniae, and Pseudomonas aeruginosa has been studied. The results revealed the formation of HAp-chitosan gel having nanosized particles, which confers protection against UV-radiation. The antibacterial activity records showed that chitosan-HAp gel exhibits a significant effect on the growth and ultrastructure of multi-drug resistant bacterial activities. Therefore, the chitosan-HAp gel is promising for skin health care as an antibacterial sunscreen.

  18. Toxicity tests, antioxidant activity, and antimicrobial activity of chitosan

    Science.gov (United States)

    Kurniasih, M.; Purwati; Dewi, R. S.

    2018-04-01

    Chitosan is a naturally occurring cationic biopolymer, obtained by alkaline deacetylation of chitin. This research aims to investigate the toxicity, antioxidant activity and antibacterial activity of chitosan from shrimp chitin. In this study, chitin extracted from shrimp waste material. Chitin is then deacetylation with 60% NaOH so that chitosan produced. Degrees of deacetylation, molecular weight, toxicity test, antioxidant activity and antimicrobial activity of chitosan then evaluated. Toxicity test using Brine Shrimp Lethality Test. The antioxidant analysis was performed using DPPH method (2, 2-diphenyl-1-picrylhydrazyl) and FTC method (ferric thiocyanate) in which the radical formed will reduce Ferro to Ferri resulting in a complex with thiocyanate. To determine the antibacterial activity of Staphylococcus aureus, antifungal in Candida albicans and Aspergillus niger by measuring antimicrobial effects and minimum inhibitory concentrations (MIC). Based on the result of research, the value of degrees of deacetylation, molecular weight, and LC50 values of chitosan synthesis was 94,32, 1052.93 g/mol and 1364.41 ppm, respectively. In general, the antioxidative activities increased as the concentration of chitosan increased. MIC value of chitosan against S. aureus, C. albicans, and A. niger was 10 ppm, 15.6 ppm, and 5 ppm, respectively.

  19. FTIR studies of chitosan acetate based polymer electrolytes

    International Nuclear Information System (INIS)

    Osman, Z.; Arof, A.K.

    2003-01-01

    Chitosan is the product when partially deacetylated chitin dissolves in dilute acetic acid. As such, depending on the degree of deacetylation, the carbonyl, C=O-NHR band can be observed at ∼1670 cm -1 and the amine, NH 2 band at 1590 cm -1 . When lithium triflate is added to chitosan to form a film of chitosan acetate-salt complex, the bands assigned to chitosan in the complex and the spectrum as a whole shift to lower wavenumbers. The carbonyl band is observed to shift to as low as 1645 cm -1 and the amine band to as low as 1560 cm -1 . These indicate chitosan-salt interactions. Also present are the bands due to lithium triflate i.e. ∼761, 1033, 1182 and 1263 cm -1 . When chitosan and ethylene carbonate (EC) are dissolved in acetic acid to form a film of plasticized chitosan acetate, the bands in the infrared spectrum of the films do not show any significant shift indicating that EC does not interact with chitosan. EC-LiCF 3 SO 3 interactions are indicated by the shifting of the C-O bending band from 718 cm -1 in the spectrum of EC to 725 cm -1 in the EC-salt spectrum. The Li + -EC is also evident in the ring breathing region at 893 cm -1 in the pure EC spectrum. This band has shifted to 898 cm -1 in the EC-salt spectrum. C=O stretching in the doublet observed at 1774 and 1803 cm -1 in the spectrum of pure EC has shifted to 1777 and 1808 cm -1 in the EC-salt spectrum

  20. Methylene Blue for Vasoplegia When on Cardiopulmonary Bypass During Double-Lung Transplantation.

    Science.gov (United States)

    Carley, Michelle; Schaff, Jacob; Lai, Terrance; Poppers, Jeremy

    2015-10-15

    Vasoplegia syndrome, characterized by hypotension refractory to fluid resuscitation or high-dose vasopressors, low systemic vascular resistance, and normal-to-increased cardiac index, is associated with increased morbidity and mortality after cardiothoracic surgery. Methylene blue inhibits inducible nitric oxide synthase and guanylyl cyclase, and has been used to treat vasoplegia during cardiopulmonary bypass. However, because methylene blue is associated with increased pulmonary vascular resistance, its use in patients undergoing lung transplantion has been limited. Herein, we report the use of methylene blue to treat refractory vasoplegia during cardiopulmonary bypass in a patient undergoing double-lung transplantation.

  1. Effect of time and deposition method on quality of phosphonic acid modifier self-assembled monolayers on indium zinc oxide

    Energy Technology Data Exchange (ETDEWEB)

    Sang, Lingzi [Department of Chemistry and Biochemistry, University of Arizona, Tucson, AZ 85721 (United States); Knesting, Kristina M. [Department of Chemistry, University of Washington, Seattle, WA 98195-1700 (United States); Bulusu, Anuradha [School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Sigdel, Ajaya K. [National Renewable Energy Laboratory, Golden, CO 80401 (United States); Giordano, Anthony J.; Marder, Seth R. [School of Chemistry and Biochemistry and Center for Organic Photonics and Electronics, Georgia Institute of Technology, Atlanta, GA 30332-0400 (United States); Berry, Joseph J. [National Renewable Energy Laboratory, Golden, CO 80401 (United States); Graham, Samuel [School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Ginger, David S. [Department of Chemistry, University of Washington, Seattle, WA 98195-1700 (United States); Pemberton, Jeanne E., E-mail: pembertn@email.arizona.edu [Department of Chemistry and Biochemistry, University of Arizona, Tucson, AZ 85721 (United States)

    2016-12-15

    Highlights: • Deposition of phosphonic acid monolayers on oxides from ethanol solutions occurs by rapid adsorption within 10 s with slower equilibration complete in 48 h. • The slower equilibration step involves molecular reorientation and vacancy filling on the oxide surface. • Soak-free deposition by spray coating and microcontact printing do not provide reproducible, fully-covered, uniform monolayers without substrate etching. • Adjustments to exposure time, substrate temperature, and solution/substrate contact efficiency are necessary to optimize soak-free methods. - Abstract: Phosphonic acid (PA) self-assembled monolayers (SAMs) are utilized at critical interfaces between transparent conductive oxides (TCO) and organic active layers in organic photovoltaic devices (OPVs). The effects of PA deposition method and time on the formation of close-packed, high-quality monolayers is investigated here for SAMs fabricated by solution deposition, micro-contact printing, and spray coating. The solution deposition isotherm for pentafluorinated benzylphosphonic acid (F{sub 5}BnPA) on indium-doped zinc oxide (IZO) is studied using polarization modulation-infrared reflection-absorption spectroscopy (PM-IRRAS) at room temperature as a model PA/IZO system. Fast surface adsorption occurs within the first min; however, well-oriented high-quality SAMs are reached only after ∼48 h, presumably through a continual process of molecular adsorption/desorption and monolayer filling accompanied by molecular reorientation. Two other rapid, soak-free deposition techniques, micro-contact printing and spray coating, are also explored. SAM quality is compared for deposition of phenyl phosphonic acid (PPA), F{sub 13}-octylphosphonic acid (F{sub 13}OPA), and pentafluorinated benzyl phosphonic acid (F{sub 5}BnPA) by solution deposition, micro-contact printing and spray coating using PM-IRRAS. In contrast to micro-contact printing and spray coating techniques, 48–168 h solution

  2. Solid polymer electrolyte from phosphorylated chitosan

    Energy Technology Data Exchange (ETDEWEB)

    Fauzi, Iqbal, E-mail: arcana@chem.itb.ac.id; Arcana, I Made, E-mail: arcana@chem.itb.ac.id [Inorganic and Physical Chemistry Research Groups, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132 (Indonesia)

    2014-03-24

    Recently, the need of secondary battery application continues to increase. The secondary battery which using a liquid electrolyte was indicated had some weakness. A solid polymer electrolyte is an alternative electrolytes membrane which developed in order to replace the liquid electrolyte type. In the present study, the effect of phosphorylation on to polymer electrolyte membrane which synthesized from chitosan and lithium perchlorate salts was investigated. The effect of the component’s composition respectively on the properties of polymer electrolyte, was carried out by analyzed of it’s characterization such as functional groups, ion conductivity, and thermal properties. The mechanical properties i.e tensile resistance and the morphology structure of membrane surface were determined. The phosphorylation processing of polymer electrolyte membrane of chitosan and lithium perchlorate was conducted by immersing with phosphoric acid for 2 hours, and then irradiated on a microwave for 60 seconds. The degree of deacetylation of chitosan derived from shrimp shells was obtained around 75.4%. Relative molecular mass of chitosan was obtained by viscometry method is 796,792 g/mol. The ionic conductivity of chitosan membrane was increase from 6.33 × 10{sup −6} S/cm up to 6.01 × 10{sup −4} S/cm after adding by 15 % solution of lithium perchlorate. After phosphorylation, the ionic conductivity of phosphorylated lithium chitosan membrane was observed 1.37 × 10{sup −3} S/cm, while the tensile resistance of 40.2 MPa with a better thermal resistance. On the strength of electrolyte membrane properties, this polymer electrolyte membrane was suggested had one potential used for polymer electrolyte in field of lithium battery applications.

  3. PLA/chitosan/keratin composites for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Tanase, Constantin Edi, E-mail: etanase@live.com [Faculty of Medical Bioengineering, ‘Grigore T. Popa’ University of Medicine and Pharmacy, 9-13 Kogalniceanu Street, 700454 Iasi (Romania); Spiridon, Iuliana [“Petru Poni” Institute of Macromolecular Chemistry, 41A Grigore Ghica Voda Alley, 700487 Iasi (Romania)

    2014-07-01

    Novel composites based on PLA, chitosan and keratin was obtained via blend preparation. The goal of this contribution was to evaluate mechanical and in vitro behavior of the composites. The results point out composites with improved Young modulus and decreased tensile strength, significant increase in hardness (compared to PLA) and a good uptake of the surface properties. Biological assessments using human osteosarcoma cell line on these composites indicate a good viability/proliferation outcome. Hence preliminary results regarding mechanical behavior and in vitro osteoblast response suggest that these composites might have prospective application in medical field. - Highlights: • PLA, chitosan and keratin composites are prepared by blend preparation. • PLA, chitosan and keratin composites present improved mechanical properties and water uptake compare to PLA. • PLA, chitosan and keratin composites present good in vitro behavior.

  4. PLA/chitosan/keratin composites for biomedical applications

    International Nuclear Information System (INIS)

    Tanase, Constantin Edi; Spiridon, Iuliana

    2014-01-01

    Novel composites based on PLA, chitosan and keratin was obtained via blend preparation. The goal of this contribution was to evaluate mechanical and in vitro behavior of the composites. The results point out composites with improved Young modulus and decreased tensile strength, significant increase in hardness (compared to PLA) and a good uptake of the surface properties. Biological assessments using human osteosarcoma cell line on these composites indicate a good viability/proliferation outcome. Hence preliminary results regarding mechanical behavior and in vitro osteoblast response suggest that these composites might have prospective application in medical field. - Highlights: • PLA, chitosan and keratin composites are prepared by blend preparation. • PLA, chitosan and keratin composites present improved mechanical properties and water uptake compare to PLA. • PLA, chitosan and keratin composites present good in vitro behavior

  5. Development of Chitosan Acetate Films for Transdermal Delivery of ...

    African Journals Online (AJOL)

    Erah

    Methods: Chitosan acetate was chemically modified with acetaldehyde and the solution was prepared ... from solution [3]. In this regard possibilities for the potential use of chitosan as an absorption enhancer in the more basic environment of the large intestine, colon and ..... impregnation of ophthalmic drugs on chitosan.

  6. Lactic acid demineralization of shrimp shell and chitosan synthesis

    Directory of Open Access Journals (Sweden)

    Alewo Opuada AMEH

    2015-05-01

    Full Text Available The use of lactic acid was compared to hydrochloric acid for shrimp shell demineralization in chitosan synthesis. Five different acid concentrations were considered for the study: 1.5M, 3.0M, 4.5M, 6.0M and 7.5M. After demineralization, the shrimp shell were deproteinized and subsequently deacetylated to produce chitosan using sodium hydroxide solution. The synthesized chitosan samples were characterized using solubility, FTIR, SEM, XRD and viscosity. The SEM, FTIR and XRD analysis indicated that chitosan was synthesized with a high degree of deacetylation (83.18±2.11 when lactic acid was used and 84.2±5.00 when HCl was used. The degree of deacetylation and the molecular weight of the chitosan samples were also estimated. ANOVA analysis (at 95% confidence interval indicated that acid type and concentration did not significantly affect the solubility, degree of deacetylation, viscosity and molecular weight of the chitosan within the range considered.

  7. Fabrication and Characteristics of Chitosan Sponge as a Tissue Engineering Scaffold

    Directory of Open Access Journals (Sweden)

    Takeshi Ikeda

    2014-01-01

    Full Text Available Cells, growth factors, and scaffolds are the three main factors required to create a tissue-engineered construct. After the appearance of bovine spongiform encephalopathy (BSE, considerable attention has therefore been focused on nonbovine materials. In this study, we examined the properties of a chitosan porous scaffold. A porous chitosan sponge was prepared by the controlled freezing and lyophilization of different concentrations of chitosan solutions. The materials were examined by scanning electron microscopy, and the porosity, tensile strength, and basic fibroblast growth factor (bFGF release profiles from chitosan sponge were examined in vitro. The morphology of the chitosan scaffolds presented a typical microporous structure, with the pore size ranging from 50 to 200 μm. The porosity of chitosan scaffolds with different concentrations was approximately 75–85%. A decreasing tendency for porosity was observed as the concentration of the chitosan increased. The relationship between the tensile properties and chitosan concentration indicated that the ultimate tensile strength for the sponge increased with a higher concentration. The in vitro bFGF release study showed that the higher the concentration of chitosan solution became, the longer the releasing time of the bFGF from the chitosan sponge was.

  8. Novel procedure to enhance PLA surface properties by chitosan irreversible immobilization

    Science.gov (United States)

    Stoleru, Elena; Dumitriu, Raluca Petronela; Munteanu, Bogdanel Silvestru; Zaharescu, Traian; Tănase, Elisabeta Elena; Mitelut, Amalia; Ailiesei, Gabriela-Liliana; Vasile, Cornelia

    2016-03-01

    A novel two step procedure was applied for poly(lactic acid) (PLA) functionalization consisting in the exposure to cold radiofrequency plasma in nitrogen atmosphere or to gamma irradiation followed by ;grafting to; of a chitosan layer using carbodiimide chemistry. The adhesion and stability of the deposited surface layer was assured by plasma/gamma irradiation treatment while the chitosan layer offers antifungal/antibacterial/antioxidant activities. Chitosan with different viscosities/deacetylation degree was deposited by electrospinning or immersion methods. Correlations between rheological behavior of chitosan solutions and chitosan layer deposition conditions are made. The PLA surface properties were investigated by water contact angle measurements, ATR-FTIR spectroscopy, AFM, chemiluminiscence, etc. It has been established that the surface roughness increases direct proportional with cold plasma duration and gamma irradiation dose and further increases by chitosan coating which at its turn depends on chitosan characteristics (viscosity and deacetylation degree) and method of deposition. Nano-fibers with relatively homogeneous and reproducible features are obtained by electrospinning of highly viscous chitosan while with the other two types of chitosan both microparticles and nano-fibers are formed. The chitosan coating obtained by immersion is more homogenous and compact and has a better antibacterial activity than the electrospun layer as fiber meshes.

  9. Structural coloration of chitosan-cationized cotton fabric using photonic crystals

    Science.gov (United States)

    Yavuz, G.; Zille, A.; Seventekin, N.; Souto, A. P.

    2017-10-01

    In this work, poly (styrene-methyl methacrylate-acrylic acid) P(St-MMA-AA) composite nanospheres were deposited onto chitosan-cationized woven cotton fabrics followed by a second layer of chitosan. The deposited photonic crystals (PCs) on the fabrics were evaluated for coating efficiency and resistance, chemical analysis and color variation by optical and SEM microscopy, ATR-FTIR, diffuse reflectance spectroscopy and washing fastness. Chitosan deposition on cotton fabric provided cationic groups on the fiber surface promoting electrostatic interaction with photonic crystals. SEM images of the washed samples indicate that the PCs are firmly coated on the cotton surface only in the chitosan treated sample. The photonic nanospheres show an average diameter of 280 nm and display a face-centered cubic closepacking structure with an average thickness of 10 μm. A further chitosan post-treatment enhances color yield of the samples due to the chitosan transparent covering layer that induce bright reflections where the angles of incidence and reflection are the same. After washing, no photonic crystal can be detected on control fabric surface. However, the sample that received a chitosan post-treatment showed a good washing fastness maintaining a reasonable degree of iridescence. Chitosan fills the spaces between the polymer spheres in the matrix stabilizing the photonic structure. Sizeable variations in lattice spacing will allow color variations using more flexible non-close-packed photonic crystal arrays in chitosan hydrogels matrices.

  10. Enhancement of Cunninghamella elegans UCP/WFCC 0542 Biomass and Chitosan with Amino Acid Supply

    Directory of Open Access Journals (Sweden)

    Galba M. Campos-Takaki

    2013-08-01

    Full Text Available Studies were carried out with Cunninghamella elegans UCP/WFCC 0542 to evaluate the effects of an abundant supply of amino acids, asparagine and corn steep liquor associated with sucrose on the production of biomass and chitosan by submerged fermentation. The concentrations of the components of the culture medium which were determined by a 23 full factorial design evaluated the interactions and effects of the independent variables of the sucrose, asparagine and corn steep liquor in relation to carbon and nitrogen sources, on the production of chitosan regarding biomass. The best results were observed at the central point [asparagine 0.025%, sucrose 0.15% and 0.45% of corn steep liquor, ratio C:N=2:6], and produced maximum yields of 16.95 g/L biomass and 2.14 g/L chitosan, after 96 h of submerged fermentation. However, the lowest level of sucrose, asparagine and corn steep liquor produced a low amount of biomass (10.83 g/L and chitosan (0.60g/L. The infrared spectrum absorption of the chitosan produced by C. elegans showed bands regarding OH-axial stretching between 3406 and 3432 cm−1, superimposed on the NH stretching band with axial deformation of the amide C=O group at about 1639 cm−1, NH angular deformation at approximately 1560 cm−1; axial deformation of amide-CN at around 1421 cm−1, symmetrical angular deformation in CH3 at 1379 cm−1, -CN axial deformation of amino groups from 1125 to 1250 cm−1 and polysaccharide structure bands in the range of between 890–1150 cm−1. The crystallinity index of chitosan was 60.92%, and its degree of deacetylation was 75.25%. A low percentage of a supply of sucrose and asparagine with corn steep liquor offered higher yields of biomass and chitosan production at low cost.

  11. Obtaining and characterization of chitosan biocomposites / HAP for application as biomaterial

    International Nuclear Information System (INIS)

    Leal, R.C.A.; Nascimento, I.V.S.R.; Fook, M.V.L.; Furtado, G.T.F.S.

    2011-01-01

    The hydroxyapatite is one of the most biocompatible materials known by encouraging bone growth. However, the main drawback it is the poor mechanical strength. A method to overcome this problem is the addition of the biopolymer chitosan, suitable for applications as biomaterials. In this study was obtained a hydroxyapatite - chitosan biocomposites for application as a biomaterial. In the FTIR analysis it was identified characteristic bands of hydroxyapatite and a possible overlap of the amino group of chitosan by carbonate. XRD analysis showed that there was no change in the profile of HA after chitosan incorporation. In SEM analysis of the biocomposites HA / chitosan, it is observed that there wasn't a complete dispersion of HA particles in the chitosan. In the image of calcined biocomposite, it was found that after heat treatment at 900 ° C chitosan was eliminated, resulting in a porous material. The analysis has shown that the presence of chitosan did not cause significant changes in the phase of hydroxyapatite. (author)

  12. Synthesis and characterization of Chitosan-CuO-MgO polymer nanocomposites

    Science.gov (United States)

    Praffulla, S. R.; Bubbly, S. G.

    2018-05-01

    In the present work, we have synthesized Chitosan-CuO-MgO nanocomposites by incorporating CuO and MgO nanoparticles in chitosan matrix. Copper oxide and magnesium oxide nanoparticles synthesized by precipitation method were characterized by X-ray diffraction and the diffraction patterns confirmed the monoclinic and cubic crystalline structures of CuO and MgO nanoparticles respectively. Chitosan-CuO-MgO composite films were prepared using solution- cast method with different concentrations of CuO and MgO nanoparticles (15 - 50 wt % with respect to chitosan) and characterized by XRD, FTIR and UV-Vis spectroscopy. The X-ray diffraction pattern shows that the crystallinity of the chitosan composite increases with increase in nanoparticle concentration. FTIR spectra confirm the chemical interaction between chitosan and metal oxide nanoparticles (CuO and MgO). UV absorbance of chitosan nanocomposites were up to 17% better than pure chitosan, thus confirming its UV shielding properties. The mechanical and electrical properties of the prepared composites are in progress.

  13. Application of radiation degraded CM-chitosan for preservation of fresh fruits

    International Nuclear Information System (INIS)

    Quynh, Tran Minh; Hien, Nuguyen Quoc; Yoshii, Fumio; Nagasawa, Naotsugu; Kume, Tamikazu

    2003-01-01

    CM-chitosan was irradiated with various doses in powder state and solution using Co 60 gamma source. The changes of viscosity in solution as well as molecular weight were also measured. The molecular weight reduced with increasing of radiation dose. The antimicrobial activity of CM-chitosan and irradiated CM-chitosan in solution against E.coli was investigated. In this studies, the sensitivity of E.coli depended on the concentration of CM-chitosan supplemented into medium and the antimicrobial activity of irradiated CM-chitosan was found to increase with radiation dose and reached to maximum with dose of 100 kGy. The 2% aqueous solutions prepared from CM-chitosan and 100 kGy irradiated CM-chitosan as mentioned above were applied for apple preservation. All coating fruits have significantly reduced the weight loss, spoilage ratio compared with control. Chemical and sensory quality of coated fruits were evaluated and compared, the best results were achieved with fruit coated using irradiated CM-chitosan. (author)

  14. Degradation of chitosan by gamma ray with presence of hydrogen peroxide

    Energy Technology Data Exchange (ETDEWEB)

    Mahmud, Maznah; Yacob, Norzita; Talip, Norhashidah; Abdullah, Zahid [Malaysian Nuclear Agency, Radiation Technology Division, Bangi, 43000 Kajang, Selangor (Malaysia); Naziri, Muhammad Ihsan [University of Malaya, 50603 Kuala Lumpur (Malaysia)

    2014-02-12

    The radiation degraded chitosan samples were prepared by swelling the chitosan powder in water and exposed for gamma irradiation. The ratio chitosan to water was 1:6 with the presence of hydrogen peroxide (H{sub 2}O{sub 2}), 1%–5%. These chitosan-water mixtures were irradiated at 6kGy, which is the lowest irradiation dose that facility can offered. All samples were purified and proceed with characterization. The molecular weight (MW) study was monitored by size exclusion chromatography-multi angle laser light scattering (SEC-MALLS). Results showed that MW of chitosan reduced as the dose increased. Application of H{sub 2}O{sub 2} enhanced the degradation rate of chitosan even at very low irradiation dose. Homogenous degradation also occurred during treatment with H{sub 2}O{sub 2}based on the polydispersity index (PDI) derived from the calculation of weight average molecular weight over number average molecular weight (Mw/Mn). Mechanism of chitosan radiation degradation with and without hydrogen peroxide was also discussed in this paper. Structure of degraded products was characterized with Fourier-transform infrared spectra. The degree of deacetylation (DDA) values of the samples was determined by acid-base titration. Solubility test results showed that, chitosan powder even at low Mw was insoluble in water even at low pH water. Chitosan as well as irradiated chitosan powder are soluble in strong and weak acid solution. Further discussion on behaviours of radiation degraded chitosan will be elaborated more in this paper.

  15. Degradation of chitosan by gamma ray with presence of hydrogen peroxide

    Science.gov (United States)

    Mahmud, Maznah; Naziri, Muhammad Ihsan; Yacob, Norzita; Talip, Norhashidah; Abdullah, Zahid

    2014-02-01

    The radiation degraded chitosan samples were prepared by swelling the chitosan powder in water and exposed for gamma irradiation. The ratio chitosan to water was 1:6 with the presence of hydrogen peroxide (H2O2), 1%-5%. These chitosan-water mixtures were irradiated at 6kGy, which is the lowest irradiation dose that facility can offered. All samples were purified and proceed with characterization. The molecular weight (MW) study was monitored by size exclusion chromatography-multi angle laser light scattering (SEC-MALLS). Results showed that MW of chitosan reduced as the dose increased. Application of H2O2 enhanced the degradation rate of chitosan even at very low irradiation dose. Homogenous degradation also occurred during treatment with H2O2based on the polydispersity index (PDI) derived from the calculation of weight average molecular weight over number average molecular weight (Mw/Mn). Mechanism of chitosan radiation degradation with and without hydrogen peroxide was also discussed in this paper. Structure of degraded products was characterized with Fourier-transform infrared spectra. The degree of deacetylation (DDA) values of the samples was determined by acid-base titration. Solubility test results showed that, chitosan powder even at low Mw was insoluble in water even at low pH water. Chitosan as well as irradiated chitosan powder are soluble in strong and weak acid solution. Further discussion on behaviours of radiation degraded chitosan will be elaborated more in this paper.

  16. Improving effects of chitosan nanofiber scaffolds on osteoblast proliferation and maturation

    Science.gov (United States)

    Ho, Ming-Hua; Liao, Mei-Hsiu; Lin, Yi-Ling; Lai, Chien-Hao; Lin, Pei-I; Chen, Ruei-Ming

    2014-01-01

    Osteoblast maturation plays a key role in regulating osteogenesis. Electrospun nanofibrous products were reported to possess a high surface area and porosity. In this study, we developed chitosan nanofibers and examined the effects of nanofibrous scaffolds on osteoblast maturation and the possible mechanisms. Macro- and micro observations of the chitosan nanofibers revealed that these nanoproducts had a flat surface and well-distributed fibers with nanoscale diameters. Mouse osteoblasts were able to attach onto the chitosan nanofiber scaffolds, and the scaffolds degraded in a time-dependent manner. Analysis by scanning electron microscopy further showed mouse osteoblasts adhered onto the scaffolds along the nanofibers, and cell–cell communication was also detected. Mouse osteoblasts grew much better on chitosan nanofiber scaffolds than on chitosan films. In addition, human osteoblasts were able to adhere and grow on the chitosan nanofiber scaffolds. Interestingly, culturing human osteoblasts on chitosan nanofiber scaffolds time-dependently increased DNA replication and cell proliferation. In parallel, administration of human osteoblasts onto chitosan nanofibers significantly induced osteopontin, osteocalcin, and alkaline phosphatase (ALP) messenger (m)RNA expression. As to the mechanism, chitosan nanofibers triggered runt-related transcription factor 2 mRNA and protein syntheses. Consequently, results of ALP-, alizarin red-, and von Kossa-staining analyses showed that chitosan nanofibers improved osteoblast mineralization. Taken together, results of this study demonstrate that chitosan nanofibers can stimulate osteoblast proliferation and maturation via runt-related transcription factor 2-mediated regulation of osteoblast-associated osteopontin, osteocalcin, and ALP gene expression. PMID:25246786

  17. Corrosion protective performance of amino trimethylene phosphonic acid-metal complex layers fabricated on the cold-rolled steel substrate via one-step assembly

    Science.gov (United States)

    Yan, Ru; He, Wei; Zhai, Tianhua; Ma, Houyi

    2018-06-01

    Seeing that amino trimethylene phosphonic acid (ATMP) possesses very strong complexation ability to metal ions and the phosphonic acid group has good affinity for the oxidized iron surface, herein a simple and rapid film-forming method (one-step assembly method) was developed to construct the ATMP-Zn complex conversion layers (ATMP-Zn layers for short) on the cold-rolled steel (CRS) substrate. Zinc ions were found to participate in the formation process of ATMP-based composite film, which made the Zn-containing ATMP film significantly different in appearance, thickness, microstructure and film-forming mechanisms from the Zn-free ATMP film. There was mainly iron (ш) phosphonate in the Zn-free ATMP film, whereas there were Zn2+-ATMP complex and a certain amount of ZnO in the ATMP-Zn composite film. In addition, electrochemical test results clearly indicate that corrosion resistance of ATMP-Zn composite film was greatly enhanced due to the presence of Zn component. Moreover, the corrosion resistance performance could be controlled by adjusting film-forming time, pH and ATMP concentration in the film-forming solutions. The present study provides a new method for the design and fabrication of high-quality environmentally-friendly conversion layers.

  18. Characterization and obtainment of thin films based on N,N,N-trimethyl chitosan and heparin through the technical layer-by-layer; Caracterizacao e obtencao de filmes finos de N,N,N-trimetil quitosana e heparina atraves da tecnica layer-by-layer

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2011-07-01

    Thin films of Heparin (HP) and N,N,N-trimethyl chitosan (TMC) with a high degree of quaternization (DQ) were obtained at pH 7.4 through the layer-by-layer (LbL) technique. Polystyrene (PS) was oxidized with aqueous solution of sodium persulfate and subsequently employed as substrate. The characterization of TMC and the respective determination of DQ were performed through {sup 1}H NMR spectroscopy. The thin films de TMC/HP were characterized by FTIR-ATR and AFM. Both techniques confirmed the adsorption of TMC and HP in surface of the PS. The increasing of the bilayers provides a decrease of the projections and/or roughness, further of minimizing the depressions at the surface of the films. Studies of thin films the base of TMC/HP prepared from the LbL technique has not been reported in the literature. It is expected that the thin films of TMC/HP present anti-adhesive and antimicrobial properties. (author)

  19. Chitosan-containing hydrogel wound dressings prepared by radiation technique

    International Nuclear Information System (INIS)

    Mozalewska, Wiktoria; Czechowska-Biskup, Renata; Olejnik, Alicja K.; Wach, Radoslaw A.; Ulański, Piotr; Rosiak, Janusz M.

    2017-01-01

    The aim of the study was to develop an antimicrobial hydrogel wound dressing by means of radiation-initiated crosslinking of hydrophilic polymers, i.e. by well-established technology comprising gel manufacturing and its sterilization in one process. The approach included admixture of chitosan of relatively low molecular weight dissolved in lactic acid (LA) into the initial regular components of the conventional hydrogel dressing based on poly(N-vinyl pyrrolidone) (PVP) and agar. Molecular weight of chitosan was regulated by radiation-initiated degradation in the range of 39–132 kg mol −1 . Optimum total concentration of LA in the resultant hydrogel dressing was evaluated as 0.05 mol dm −3 , that is ca. 0.5%. Presence of LA in the system influenced essential radiation and technological parameters of hydrogel manufacturing. The setting temperature of the pre-hydrogel mixture, resulting from agar ability to congeal, was reduced with LA concentration, yet remained significantly above the room temperature. 0.5% of chitosan was effectively dissolved in aqueous solution of lactic acid due to its pH (lower than 5.5). Radiation parameters of PVP crosslinking in the presence of LA, as determined with generalized Charlesby–Pinner equation, were reflected in slight reduction of the maximum gel fraction and increase in gelation dose and in the factor comparing yields of scission to crosslinking. Nevertheless, essentially physical characteristics of the hydrogel was not affected, except for somewhat increased water uptake capacity, what in turn improves functionality of the dressing as extensive exudate for the wound can be efficiently absorbed. Preliminary microbiological studies showed antimicrobial character of the chitosan-containing hydrogel towards Gram-positive bacterial strain. - Highlights: • Radiation synthesis of bioactive hydrogel wound dressing based on PVP. • Sol-gel analysis, radiation yield of crosslinking and degradation, gel fraction.

  20. Films, Buckypapers and Fibers from Clay, Chitosan and Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Marc in het Panhuis

    2011-04-01

    Full Text Available The mechanical and electrical characteristics of films, buckypapers and fiber materials from combinations of clay, carbon nanotubes (CNTs and chitosan are described. The rheological time-dependent characteristics of clay are maintained in clay–carbon nanotube–chitosan composite dispersions. It is demonstrated that the addition of chitosan improves their mechanical characteristics, but decreases electrical conductivity by three-orders of magnitude compared to clay–CNT materials. We show that the electrical response upon exposure to humid atmosphere is influenced by clay-chitosan interactions, i.e., the resistance of clay–CNT materials decreases, whereas that of clay–CNT–chitosan increases.