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Sample records for chemical peptide synthesis

  1. Synthesis, chemical and biological quality control of radioiodinated peptides

    International Nuclear Information System (INIS)

    Rafii, H.; Khalaj, A.; Beiki, D.; Motameidi, F.; Maloobi, M.; Karimian-dehghan, M.; Keshavarrzi, F.

    2002-01-01

    Iodinated compounds with I-131, 125 and 123 have been widely used for biochemical function studies. In conjunction with SPECT, [I-123] labelled proteins have various diagnostic and therapeutic applications in nuclear medicine. Preparation of some radioiodinated peptides with tyrosine and/or lysine groups on their main chain molecules can be carried out with both direct and indirect methods, but lack of these groups in molecule cause the molecule dose not lend itself for direct radioiodination. In this study, human IgG and Formyl-Methyl-Leucyl-Phenylalanine, FMLF, have been chosen as a model compounds for direct and indirect radioiodination respectively. Here, we will describe the labelling procedure of [I-125] IgG using chloramine-T as a suitable oxidant agent and [I-125 and I-131] FMLF by indirect method using ATE/SIB as a prosthetic group in multi-step reactions. The obtained results for chemical quality control of intermediate radioiodinated SIB by HPLC and two labelled IgG and FMLF will be also discussed. Biological results, biodistribution studies and SPECT scans on mice per-injected labelled FMLF show a low uptake of thyroid but a high at urine and bladder, perhaps because of low molecular weight of FMLF. In this case, it seems to be better to separate the reaction mixture of labelled FMLF by BPLC than Sephadex-G50 gel filtration. (Author)

  2. Development of a method for environmentally friendly chemical peptide synthesis in water using water-dispersible amino acid nanoparticles

    Directory of Open Access Journals (Sweden)

    Fukumori Yoshinobu

    2011-08-01

    Full Text Available Abstract Due to the vast importance of peptides in biological processes, there is an escalating need for synthetic peptides to be used in a wide variety of applications. However, the consumption of organic solvent is extremely large in chemical peptide syntheses because of the multiple condensation steps in organic solvents. That is, the current synthesis method is not environmentally friendly. From the viewpoint of green sustainable chemistry, we focused on developing an organic solvent-free synthetic method using water, an environmentally friendly solvent. Here we described in-water synthesis technology using water-dispersible protected amino acids.

  3. Catalytic chemical amide synthesis at room temperature: one more step toward peptide synthesis.

    Science.gov (United States)

    Mohy El Dine, Tharwat; Erb, William; Berhault, Yohann; Rouden, Jacques; Blanchet, Jérôme

    2015-05-01

    An efficient method has been developed for direct amide bond synthesis between carboxylic acids and amines via (2-(thiophen-2-ylmethyl)phenyl)boronic acid as a highly active bench-stable catalyst. This catalyst was found to be very effective at room temperature for a large range of substrates with slightly higher temperatures required for challenging ones. This methodology can be applied to aliphatic, α-hydroxyl, aromatic, and heteroaromatic acids as well as primary, secondary, heterocyclic, and even functionalized amines. Notably, N-Boc-protected amino acids were successfully coupled in good yields with very little racemization. An example of catalytic dipeptide synthesis is reported.

  4. Chemo-enzymatic peptide synthesis : bioprocess engineering aspects

    NARCIS (Netherlands)

    Vossenberg, P.

    2012-01-01

    Peptides, in particular oligopeptides, play an important role in the fields of health care, nutrition and cosmetics. Chemical synthesis is currently the most mature technique for the synthesis of peptides that range in length from 5 to 80 amino acids. Chemical synthesis is, however,

  5. Role of manganese oxides in peptide synthesis: implication in chemical evolution

    Science.gov (United States)

    Bhushan, Brij; Nayak, Arunima; Kamaluddin

    2017-10-01

    During the course of chemical evolution the role of metal oxides may have been very significant in catalysing the polymerization of biomonomers. The peptide bond formation of alanine (ala) and glycine (gly) in the presence of various oxides of manganese were performed for a period of 35 days at three different temperatures 50, 90 and 120°C without applying drying/wetting cycling. The reaction was monitored every week. The products formed were characterized by high-performance liquid chromatography and electrospray ionization-mass spectrometry techniques. Trace amount of oligomers was observed at 50°C. Maximum yield of peptides was found after 35 days at 90°C. It is important to note that very high temperatures of 120°C favoured the formation of diketopiperazine derivatives. Different types of manganese oxides [manganosite (MnO), bixbyite (Mn2O3), hausmannite (Mn3O4) and pyrolusite (MnO2)] were used as catalyst. The MnO catalysed glycine to cyclic (Gly)2, (Gly)2 and (Gly)3, and alanine, to cyclic (Ala)2 and (Ala)2. Mn3O4 also produced the same products but in lesser yield, while Mn2O3 and MnO2 produced cyclic anhydride of glycine and alanine with a trace amount of dimers and trimmers. Manganese of lower oxidation state is much more efficient in propagating the reaction than higher oxidation states. The possible mechanism of these reactions and the relevance of the results for the prebiotic chemistry are discussed.

  6. Automated solid-phase peptide synthesis to obtain therapeutic peptides

    Directory of Open Access Journals (Sweden)

    Veronika Mäde

    2014-05-01

    Full Text Available The great versatility and the inherent high affinities of peptides for their respective targets have led to tremendous progress for therapeutic applications in the last years. In order to increase the drugability of these frequently unstable and rapidly cleared molecules, chemical modifications are of great interest. Automated solid-phase peptide synthesis (SPPS offers a suitable technology to produce chemically engineered peptides. This review concentrates on the application of SPPS by Fmoc/t-Bu protecting-group strategy, which is most commonly used. Critical issues and suggestions for the synthesis are covered. The development of automated methods from conventional to essentially improved microwave-assisted instruments is discussed. In order to improve pharmacokinetic properties of peptides, lipidation and PEGylation are described as covalent conjugation methods, which can be applied by a combination of automated and manual synthesis approaches. The synthesis and application of SPPS is described for neuropeptide Y receptor analogs as an example for bioactive hormones. The applied strategies represent innovative and potent methods for the development of novel peptide drug candidates that can be manufactured with optimized automated synthesis technologies.

  7. A new class of HIV-1 protease inhibitor: the crystallographic structure, inhibition and chemical synthesis of an aminimide peptide isostere.

    Science.gov (United States)

    Rutenber, E E; McPhee, F; Kaplan, A P; Gallion, S L; Hogan, J C; Craik, C S; Stroud, R M

    1996-09-01

    The essential role of HIV-1 protease (HIV-1 PR) in the viral life cycle makes it an attractive target for the development of substrate-based inhibitors that may find efficacy as anti-AIDS drugs. However, resistance has arisen to potent peptidomimetic drugs necessitating the further development of novel chemical backbones for diversity based chemistry focused on probing the active site for inhibitor interactions and binding modes that evade protease resistance. AQ148 is a potent inhibitor of HIV-1 PR and represents a new class of transition state analogues incorporating an aminimide peptide isostere. A 3-D crystallographic structure of AQ148, a tetrapeptide isostere, has been determined in complex with its target HIV-1 PR to a resolution of 2.5 A and used to evaluate the specific structural determinants of AQ148 potency and to correlate structure-activity relationships within the class of related compounds. AQ148 is a competitive inhibitor of HIV-1 PR with a Ki value of 137 nM. Twenty-nine derivatives have been synthesized and chemical modifications have been made at the P1, P2, P1', and P2' sites. The atomic resolution structure of AQ148 bound to HIV-1 PR reveals both an inhibitor binding mode that closely resembles that of other peptidomimetic inhibitors and specific protein/inhibitor interactions that correlate with structure-activity relationships. The structure provides the basis for the design, synthesis and evaluation of the next generation of hydroxyethyl aminimide inhibitors. The aminimide peptide isostere is a scaffold with favorable biological properties well suited to both the combinatorial methods of peptidomimesis and the rational design of potent and specific substrate-based analogues.

  8. Solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Jensen, Knud Jørgen

    2013-01-01

    This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective.......This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective....

  9. Chemical Methods for Peptide and Protein Production

    Directory of Open Access Journals (Sweden)

    Istvan Toth

    2013-04-01

    Full Text Available Since the invention of solid phase synthetic methods by Merrifield in 1963, the number of research groups focusing on peptide synthesis has grown exponentially. However, the original step-by-step synthesis had limitations: the purity of the final product decreased with the number of coupling steps. After the development of Boc and Fmoc protecting groups, novel amino acid protecting groups and new techniques were introduced to provide high quality and quantity peptide products. Fragment condensation was a popular method for peptide production in the 1980s, but unfortunately the rate of racemization and reaction difficulties proved less than ideal. Kent and co-workers revolutionized peptide coupling by introducing the chemoselective reaction of unprotected peptides, called native chemical ligation. Subsequently, research has focused on the development of novel ligating techniques including the famous click reaction, ligation of peptide hydrazides, and the recently reported a-ketoacid-hydroxylamine ligations with 5-oxaproline. Several companies have been formed all over the world to prepare high quality Good Manufacturing Practice peptide products on a multi-kilogram scale. This review describes the advances in peptide chemistry including the variety of synthetic peptide methods currently available and the broad application of peptides in medicinal chemistry.

  10. Chemical methods for peptide and protein production.

    Science.gov (United States)

    Chandrudu, Saranya; Simerska, Pavla; Toth, Istvan

    2013-04-12

    Since the invention of solid phase synthetic methods by Merrifield in 1963, the number of research groups focusing on peptide synthesis has grown exponentially. However, the original step-by-step synthesis had limitations: the purity of the final product decreased with the number of coupling steps. After the development of Boc and Fmoc protecting groups, novel amino acid protecting groups and new techniques were introduced to provide high quality and quantity peptide products. Fragment condensation was a popular method for peptide production in the 1980s, but unfortunately the rate of racemization and reaction difficulties proved less than ideal. Kent and co-workers revolutionized peptide coupling by introducing the chemoselective reaction of unprotected peptides, called native chemical ligation. Subsequently, research has focused on the development of novel ligating techniques including the famous click reaction, ligation of peptide hydrazides, and the recently reported α-ketoacid-hydroxylamine ligations with 5-oxaproline. Several companies have been formed all over the world to prepare high quality Good Manufacturing Practice peptide products on a multi-kilogram scale. This review describes the advances in peptide chemistry including the variety of synthetic peptide methods currently available and the broad application of peptides in medicinal chemistry.

  11. Matrix-assisted peptide synthesis on nanoparticles.

    Science.gov (United States)

    Khandadash, Raz; Machtey, Victoria; Weiss, Aryeh; Byk, Gerardo

    2014-09-01

    We report a new method for multistep peptide synthesis on polymeric nanoparticles of differing sizes. Polymeric nanoparticles were functionalized via their temporary embedment into a magnetic inorganic matrix that allows multistep peptide synthesis. The matrix is removed at the end of the process for obtaining nanoparticles functionalized with peptides. The matrix-assisted synthesis on nanoparticles was proved by generating various biologically relevant peptides. Copyright © 2014 European Peptide Society and John Wiley & Sons, Ltd.

  12. Chemical Synthesis and In Vitro Evaluation of a Phage Display-Derived Peptide Active against Infectious Salmon Anemia Virus.

    Science.gov (United States)

    Ojeda, Nicolás; Cárdenas, Constanza; Guzmán, Fanny; Marshall, Sergio H

    2016-04-01

    pathogen has made prophylactic control extremely difficult. The identified antiviral peptide efficiently impairs ISAV infection in vitro by specifically blocking hemagglutinin-esterase, a pivotal surface protein of this virus. Peptide synthesis could further modify the primary structure of the identified peptide to improve specific activity and stability. The present results form the foundation for developing a new pharmacological treatment against ISAV. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

  13. Effects of the substitution of amino acid residues, through chemical synthesis, on the conformation and activity of antimicrobial peptides

    Directory of Open Access Journals (Sweden)

    Regina C. Adão

    2012-06-01

    Full Text Available Antimicrobial peptides make up an assorted group of molecules which contain from 12 to 50 amino acid residues and which may be produced by microorganisms, plants and animals. From the discovery that these biomolecules are lethal to bacteria, inhibiting the pathogenic organism’s growth, and are also related to innate and adapted defense mechanisms, the investigation of such molecules came to be an emergent research field, in which more than 1800 antimicrobial peptides have so far been discovered throughout the last three decades. These molecules are potential representatives of a new generation of antibiotic agents and the main motivation for such use is their activity against a wide variety of pathogens, including Gram-positive and Gram-negative bacteria as well as fungi and viruses. An important class of comprising some of these peptides may be found in anurans, from which it has been isolated, a considerable number of antimicrobial peptides with diverse sequences and structures, including linear and dimeric ones. In this work monomeric chains (CH1 e CH2 of the heterodimeric antimicrobial peptide distinctin (isolated in 1999 from Phyllomedusa distincta anurans, as well as its mutated monomers (CH1-S and CH2-S and the heterodimer itself were synthesized. The distinctin is the peptide with two chains of different sequences (Table 1 bound each other by disulfide bond from the cystein residues constituting the heterodimer. To investigate the effects on the biological activity by amino acids substitution at normal distinctin CH1 and CH2 chains, both were synthesized as well as their similar chains (CH1-S and CH2-S in which the cystein (Fig.1 a residues of each chain were changed by serin residues (Fig. 1 b. The new chains were named mutants. The synthesis was carried out in solid phase, using Fmoc strategy. The heterodimer distinctin was obtained from CH1 and CH2 chains coupling through cystein residues air oxidation. The results from HPLC

  14. Modern methods for the synthesis of peptide-oligonucleotide conjugates

    International Nuclear Information System (INIS)

    Zubin, Evgenii M; Oretskaya, Tat'yana S; Romanova, Elena A

    2002-01-01

    The published data on the methods of chemical solution and solid-phase synthesis of peptide-oligonucleotide conjugates are reviewed. The known methods are systematised and their advantages and disadvantages are considered. The approaches to the solution synthesis of peptide-oligonucleotide conjugates are systematised according to the type of chemical bonds between the fragments, whereas those to the solid-phase synthesis are classified according to the procedure used for the preparation of conjugates, viz., stepwise elongation of oligonucleotide and peptide chains on the same polymeric support or solid-phase condensation of two presynthesised fragments. The bibliography includes 141 references.

  15. Synthesis of Mikto-Arm Star Peptide Conjugates.

    Science.gov (United States)

    Koo, Jin Mo; Su, Hao; Lin, Yi-An; Cui, Honggang

    2018-01-01

    Mikto-arm star peptide conjugates are an emerging class of self-assembling peptide-based structural units that contain three or more auxiliary segments of different chemical compositions and/or functionalities. This group of molecules exhibit interesting self-assembly behavior in solution due to their chemically asymmetric topology. Here we describe the detailed procedure for synthesis of an ABC Mikto-arm star peptide conjugate in which two immiscible entities (a saturated hydrocarbon and a hydrophobic and lipophobic fluorocarbon) are conjugated onto a short β-sheet forming peptide sequence, GNNQQNY, derived from the Sup35 prion, through a lysine junction. Automated and manual Fmoc-solid phase synthesis techniques are used to synthesize the Mikto-arm star peptide conjugates, followed by HPLC purification. We envision that this set of protocols can afford a versatile platform to synthesize a new class of peptidic building units for diverse applications.

  16. Tidbits for the synthesis of bis(2-sulfanylethyl)amido (SEA) polystyrene resin, SEA peptides and peptide thioesters.

    Science.gov (United States)

    Ollivier, Nathalie; Raibaut, Laurent; Blanpain, Annick; Desmet, Rémi; Dheur, Julien; Mhidia, Reda; Boll, Emmanuelle; Drobecq, Hervé; Pira, Silvain L; Melnyk, Oleg

    2014-02-01

    Protein total chemical synthesis enables the atom-by-atom control of the protein structure and therefore has a great potential for studying protein function. Native chemical ligation of C-terminal peptide thioesters with N-terminal cysteinyl peptides and related methodologies are central to the field of protein total synthesis. Consequently, methods enabling the facile synthesis of peptide thioesters using Fmoc-SPPS are of great value. Herein, we provide a detailed protocol for the preparation of bis(2-sulfanylethyl)amino polystyrene resin as a starting point for the synthesis of C-terminal bis(2-sulfanylethyl)amido peptides and of peptide thioesters derived from 3-mercaptopropionic acid. Copyright © 2013 European Peptide Society and John Wiley & Sons, Ltd.

  17. Synthesis of peptide .alpha.-thioesters

    Science.gov (United States)

    Camarero, Julio A [Livermore, CA; Mitchell, Alexander R [Livermore, CA; De Yoreo, James J [Clayton, CA

    2008-08-19

    Disclosed herein is a new method for the solid phase peptide synthesis (SPPS) of C-terminal peptide .alpha. thioesters using Fmoc/t-Bu chemistry. This method is based on the use of an aryl hydrazine linker, which is totally stable to conditions required for Fmoc-SPPS. When the peptide synthesis has been completed, activation of the linker is achieved by mild oxidation. The oxidation step converts the acyl-hydrazine group into a highly reactive acyl-diazene intermediate which reacts with an .alpha.-amino acid alkylthioester (H-AA-SR) to yield the corresponding peptide .alpha.-thioester in good yield. A variety of peptide thioesters, cyclic peptides and a fully functional Src homology 3 (SH3) protein domain have been successfully prepared.

  18. Radiation chemical synthesis

    International Nuclear Information System (INIS)

    Zagoretz, P.A.; Poluetkov, V.A.; Shostenko, A.G.

    1986-01-01

    The authors consider processes in radiation chemical synthesis which are being developed in various scientific-research organizations. The important advantages of radiation chlorination, viz. the lower temperature compared with the thermal method and the absence of dehydrochlorination products are discussed. The authors examine the liquid-phase chlorination of trifluorochloroethyltrichloromethyl ether to obtain the pentachloro-contining ether, trifluorodichloroethyltrichloromethyl ether. The authors discuss radiation synthesis processes that have be used formulated kinetic equations on which models have been based. It is concluded that the possibilities of preparative (micro- and low-tonnage) radiation synthesis are promising

  19. Chemical Synthesis of Circular Proteins*

    Science.gov (United States)

    Tam, James P.; Wong, Clarence T. T.

    2012-01-01

    Circular proteins, once thought to be rare, are now commonly found in plants. Their chemical synthesis, once thought to be difficult, is now readily achievable. The enabling methodology is largely due to the advances in entropic chemical ligation to overcome the entropy barrier in coupling the N- and C-terminal ends of large peptide segments for either intermolecular ligation or intramolecular ligation in end-to-end cyclization. Key elements of an entropic chemical ligation consist of a chemoselective capture step merging the N and C termini as a covalently linked O/S-ester intermediate to permit the subsequent step of an intramolecular O/S-N acyl shift to form an amide. Many ligation methods exploit the supernucleophilicity of a thiol side chain at the N terminus for the capture reaction, which makes cysteine-rich peptides ideal candidates for the entropy-driven macrocyclization. Advances in desulfurization and modification of the thiol-containing amino acids at the ligation sites to other amino acids add extra dimensions to the entropy-driven ligation methods. This minireview describes recent advances of entropy-driven ligation to prepare circular proteins with or without a cysteinyl side chain. PMID:22700959

  20. Chemical reactions directed Peptide self-assembly.

    Science.gov (United States)

    Rasale, Dnyaneshwar B; Das, Apurba K

    2015-05-13

    Fabrication of self-assembled nanostructures is one of the important aspects in nanoscience and nanotechnology. The study of self-assembled soft materials remains an area of interest due to their potential applications in biomedicine. The versatile properties of soft materials can be tuned using a bottom up approach of small molecules. Peptide based self-assembly has significant impact in biology because of its unique features such as biocompatibility, straight peptide chain and the presence of different side chain functionality. These unique features explore peptides in various self-assembly process. In this review, we briefly introduce chemical reaction-mediated peptide self-assembly. Herein, we have emphasised enzymes, native chemical ligation and photochemical reactions in the exploration of peptide self-assembly.

  1. R. Bruce Merrifield and Solid-Phase Peptide Synthesis: A Historical Assessment

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R

    2007-12-04

    Bruce Merrifield, trained as a biochemist, had to address three major challenges related to the development and acceptance of solid-phase peptide synthesis (SPPS). The challenges were (1) to reduce the concept of peptide synthesis on a insoluble support to practice, (2) overcome the resistance of synthetic chemists to this novel approach, and (3) establish that a biochemist had the scientific credentials to effect the proposed revolutionary change in chemical synthesis. How these challenges were met is discussed in this article.

  2. Synthesis of radioiodinated labeled peptides

    International Nuclear Information System (INIS)

    Matloobi, M.; Rafii, H.; Beigi, D.; Khalaj, A.; Kamali-Dehghan, M.

    2003-01-01

    Optimization of radioiodination of peptides is covered by both a direct method in which a constituent tyrosine residue is labeled and indirect method by using an iodinated derivative (SIB) of N succinimidyl 3-(tri-n-butylstannyl) benzoate (ATE) as the intermediate. Radioiodination of IgG and FMLF were performed by direct method using Chloramine-T as an oxidant but since Formyl-Methyl-Leucyl-Phenylalanine, FMLF, does not lend itself for direct radioiodination we performed labeling of FMLF by indirect method via radioiodined SIB at different pH. (author)

  3. Encoded libraries of chemically modified peptides.

    Science.gov (United States)

    Heinis, Christian; Winter, Greg

    2015-06-01

    The use of powerful technologies for generating and screening DNA-encoded protein libraries has helped drive the development of proteins as pharmaceutical ligands. However the development of peptides as pharmaceutical ligands has been more limited. Although encoded peptide libraries are typically several orders of magnitude larger than classical chemical libraries, can be more readily screened, and can give rise to higher affinity ligands, their use as pharmaceutical ligands is limited by their intrinsic properties. Two of the intrinsic limitations include the rotational flexibility of the peptide backbone and the limited number (20) of natural amino acids. However these limitations can be overcome by use of chemical modification. For example, the libraries can be modified to introduce topological constraints such as cyclization linkers, or to introduce new chemical entities such as small molecule ligands, fluorophores and photo-switchable compounds. This article reviews the chemistry involved, the properties of the peptide ligands, and the new opportunities offered by chemical modification of DNA-encoded peptide libraries. Copyright © 2015. Published by Elsevier Ltd.

  4. SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

    African Journals Online (AJOL)

    SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

  5. Green chemistry for chemical synthesis

    OpenAIRE

    Li, Chao-Jun; Trost, Barry M.

    2008-01-01

    Green chemistry for chemical synthesis addresses our future challenges in working with chemical processes and products by inventing novel reactions that can maximize the desired products and minimize by-products, designing new synthetic schemes and apparati that can simplify operations in chemical productions, and seeking greener solvents that are inherently environmentally and ecologically benign.

  6. Green chemistry for chemical synthesis.

    Science.gov (United States)

    Li, Chao-Jun; Trost, Barry M

    2008-09-09

    Green chemistry for chemical synthesis addresses our future challenges in working with chemical processes and products by inventing novel reactions that can maximize the desired products and minimize by-products, designing new synthetic schemes and apparati that can simplify operations in chemical productions, and seeking greener solvents that are inherently environmentally and ecologically benign.

  7. Chemical synthesis on SU-8

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Taveras, Kennedy; Thastrup, Ole

    2011-01-01

    In this paper we describe a highly effective surface modification of SU-8 microparticles, the attachment of appropriate linkers for solid-supported synthesis, and the successful chemical modification of these particles via controlled multi-step organic synthesis leading to molecules attached...

  8. CLEAN CHEMICAL SYNTHESIS IN WATER

    Science.gov (United States)

    Newer green chemistry approach to accomplish chemical synthesis in water is summarized. Recent global developments pertaining to C-C bond forming reactions using metallic reagents and direct use of the renewable materials such as carbohydrates without derivatization are described...

  9. Protein chemical synthesis by α-ketoacid-hydroxylamine ligation.

    Science.gov (United States)

    Harmand, Thibault J; Murar, Claudia E; Bode, Jeffrey W

    2016-06-01

    Total chemical synthesis of proteins allows researchers to custom design proteins without the complex molecular biology that is required to insert non-natural amino acids or the biocontamination that arises from methods relying on overexpression in cells. We describe a detailed procedure for the chemical synthesis of proteins with the α-ketoacid-hydroxylamine (KAHA ligation), using (S)-5-oxaproline (Opr) as a key building block. This protocol comprises two main parts: (i) the synthesis of peptide fragments by standard fluorenylmethoxycarbonyl (Fmoc) chemistry and (ii) the KAHA ligation between fragments containing Opr and a C-terminal peptide α-ketoacid. This procedure provides an alternative to native chemical ligation (NCL) that could be valuable for the synthesis of proteins, particularly targets that do not contain cysteine residues. The ligation conditions-acidic DMSO/H2O or N-methyl-2-pyrrolidinone (NMP)/H2O-are ideally suited for solubilizing peptide segments, including many hydrophobic examples. The utility and efficiency of the protocol is demonstrated by the total chemical synthesis of the mature betatrophin (also called ANGPTL8), a 177-residue protein that contains no cysteine residues. With this protocol, the total synthesis of the betatrophin protein has been achieved in around 35 working days on a multimilligram scale.

  10. Preparation of peptide thioesters through fmoc-based solid-phase peptide synthesis by using amino thioesters

    DEFF Research Database (Denmark)

    Stuhr-Hansen, N.; Wilbek, T.S.; Strømgaard, K.

    2013-01-01

    protected peptide thioester, which was globally deprotected to afford the desired unprotected peptide thioester. The method is compatible with labile groups such as phosphoryl and glycosyl moieties. The synthesis of peptide alkyl thioesters by 9-fluorenylmethoxycarbonyl (Fmoc) solid-phase peptide synthesis...

  11. Apparatus for chemical synthesis

    Science.gov (United States)

    Kong, Peter C [Idaho Falls, ID; Herring, J Stephen [Idaho Falls, ID; Grandy, Jon D [Idaho Falls, ID

    2011-05-10

    A method and apparatus for forming a chemical hydride is described and which includes a pseudo-plasma-electrolysis reactor which is operable to receive a solution capable of forming a chemical hydride and which further includes a cathode and a movable anode, and wherein the anode is moved into and out of fluidic, ohmic electrical contact with the solution capable of forming a chemical hydride and which further, when energized produces an oxygen plasma which facilitates the formation of a chemical hydride in the solution.

  12. Microwave heating in solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg; Shelton, Anne Pernille Tofteng; Malik, Leila

    2012-01-01

    synthesis, precise microwave irradiation to heat the reaction mixture during coupling and N(a)-deprotection has become increasingly popular. It has often provided dramatic reductions in synthesis times, accompanied by an increase in the crude peptide purity. Microwave heating has been proven especially...... relevant for sequences which might form ß-sheet type structures and for sterically difficult couplings. The beneficial effect of microwave heating appears so far to be due to the precise nature of this type of heating, rather than a peptide-specific microwave effect. However, microwave heating...... in microwave heating for peptide synthesis, with a focus on systematic studies and general protocols, as well as important applications. The assembly of ß-peptides, peptoids and pseudopeptides are also evaluated in this critical review (254 references)....

  13. The synthesis and coupling of photoreactive collagen-based peptides to restore integrin reactivity to an inert substrate, chemically-crosslinked collagen

    Science.gov (United States)

    Malcor, Jean-Daniel; Bax, Daniel; Hamaia, Samir W.; Davidenko, Natalia; Best, Serena M.; Cameron, Ruth E.; Farndale, Richard W.; Bihan, Dominique

    2016-01-01

    Collagen is frequently advocated as a scaffold for use in regenerative medicine. Increasing the mechanical stability of a collagen scaffold is widely achieved by cross-linking using 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-hydroxysuccinimide (NHS). However, this treatment consumes the carboxylate-containing amino acid sidechains that are crucial for recognition by the cell-surface integrins, abolishing cell adhesion. Here, we restore cell reactivity to a cross-linked type I collagen film by covalently linking synthetic triple-helical peptides (THPs), mimicking the structure of collagen. These THPs are ligands containing an active cell-recognition motif, GFOGER, a high-affinity binding site for the collagen-binding integrins. We end-stapled peptide strands containing GFOGER by coupling a short diglutamate-containing peptide to their N-terminus, improving the thermal stability of the resulting THP. A photoreactive Diazirine group was grafted onto the end-stapled THP to allow covalent linkage to the collagen film upon UV activation. Such GFOGER-derivatized collagen films showed restored affinity for the ligand-binding I domain of integrin α2β1, and increased integrin-dependent cell attachment and spreading of HT1080 and Rugli cell lines, expressing integrins α2β1 and α1β1, respectively. The method we describe has wide application, beyond collagen films or scaffolds, since the photoreactive diazirine will react with many organic carbon skeletons. PMID:26854392

  14. Total chemical synthesis of histones and their analogs, assisted by native chemical ligation and palladium complexes.

    Science.gov (United States)

    Maity, Suman Kumar; Jbara, Muhammad; Mann, Guy; Kamnesky, Guy; Brik, Ashraf

    2017-11-01

    Chemical synthesis of histones allows precise control of the installation of post-translational modifications via the coupling of derivatized amino acids. Shortcomings of other approaches for obtaining modified histones for epigenetic studies include heterogeneity of the obtained product and difficulties in incorporating multiple modifications on the same histone. In this protocol, unprotected peptide fragments are prepared by Fmoc solid-phase synthesis and coupled in aqueous buffers via native chemical ligation (NCL; in NCL, a peptide bond is formed between a peptide with an N-terminal Cys and another peptide having a C-terminal thioester). This task is challenging, with obstacles relating to the preparation and ligation of hydrophobic peptides, as well as the requirement for multiple purification steps due to protecting-group manipulations during the polypeptide assembly process. To address this, our approach uses an easily removable solubilizing tag for the synthesis and ligation of hydrophobic peptides, as well as a more efficient and better-yielding method to remove Cys-protecting groups that uses palladium chemistry (specifically [Pd(allyl)Cl] 2 and PdCl 2 complexes). The utility of this approach is demonstrated in the syntheses of ubiquitinated H2B at Lys34, phosphorylated H2A at Tyr57 and unmodified H4. Each of these analogs can be prepared in milligram quantities within ∼20-30 d.

  15. Practical multipeptide synthesis: dedicated software for the definition of multiple, overlapping peptides covering polypeptide sequences.

    Science.gov (United States)

    Heegaard, P M; Holm, A; Hagerup, M

    1993-01-01

    A personal computer program for the conversion of linear amino acid sequences to multiple, small, overlapping peptide sequences has been developed. Peptide lengths and "jumps" (the distance between two consecutive overlapping peptides) are defined by the user. To facilitate the use of the program for parallel solid-phase chemical peptide syntheses for the synchronous production of multiple peptides, amino acids at each acylation step are laid out by the program in a convenient standard multi-well setup. Also, the total number of equivalents, as well as the derived amount in milligrams (depend-ending on user-defined equivalent weights and molar surplus), of each amino acid are given. The program facilitates the implementation of multipeptide synthesis, e.g., for the elucidation of polypeptide structure-function relationships, and greatly reduces the risk of introducing mistakes at the planning step. It is written in Pascal and runs on any DOS-based personal computer. No special graphic display is needed.

  16. Novel Antimicrobial Peptides That Inhibit Gram Positive Bacterial Exotoxin Synthesis

    Science.gov (United States)

    Merriman, Joseph A.; Nemeth, Kimberly A.; Schlievert, Patrick M.

    2014-01-01

    Gram-positive bacteria, such as Staphylococcus aureus, cause serious human illnesses through combinations of surface virulence factors and secretion of exotoxins. Our prior studies using the protein synthesis inhibitor clindamycin and signal transduction inhibitors glycerol monolaurate and α-globin and β-globin chains of hemoglobin indicate that their abilities to inhibit exotoxin production by S. aureus are separable from abilities to inhibit growth of the organism. Additionally, our previous studies suggest that inhibition of exotoxin production, in absence of ability to kill S. aureus and normal flora lactobacilli, will prevent colonization by pathogenic S. aureus, while not interfering with lactobacilli colonization. These disparate activities may be important in development of novel anti-infective agents that do not alter normal flora. We initiated studies to explore the exotoxin-synthesis-inhibition activity of hemoglobin peptides further to develop potential agents to prevent S. aureus infections. We tested synthesized α-globin chain peptides, synthetic variants of α-globin chain peptides, and two human defensins for ability to inhibit exotoxin production without significantly inhibiting S. aureus growth. All of these peptides were weakly or not inhibitory to bacterial growth. However, the peptides were inhibitory to exotoxin production with increasing activity dependent on increasing numbers of positively-charged amino acids. Additionally, the peptides could be immobilized on agarose beads or have amino acid sequences scrambled and still retain exotoxin-synthesis-inhibition. The peptides are not toxic to human vaginal epithelial cells and do not inhibit growth of normal flora L. crispatus. These peptides may interfere with plasma membrane signal transduction in S. aureus due to their positive charges. PMID:24748386

  17. Chemical protein synthesis: Inventing synthetic methods to decipher how proteins work.

    Science.gov (United States)

    Kent, Stephen

    2017-09-15

    Total chemical synthesis of proteins has been rendered practical by the chemical ligation principle: chemoselective condensation of unprotected peptide segments equipped with unique, mutually reactive functional groups, enabled by formation of a non-native replacement for the peptide bond. Ligation chemistries are briefly described, including native chemical ligation - thioester-mediated, amide-forming reaction at Xaa-Cys sites - and its extensions. Case studies from the author's own works are used to illustrate the utility and applications of chemical protein synthesis. Selected recent developments in the field are briefly discussed. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. ‘Umpolung’ Reactivity in Semiaqueous Amide and Peptide Synthesis

    Science.gov (United States)

    Shen, Bo; Makley, Dawn M.; Johnston, Jeffrey N.

    2010-01-01

    The amide functional group is one of Nature’s key functional and structural elements, most notably within peptides. Amides are also key intermediates in the preparation of a diverse range of therapeutic small molecules. Its construction using available methods focuses principally upon dehydrative approaches, although oxidative and radical-based methods are representative alternatives. During the carbon-nitrogen bond forming step in most every example, the carbon and nitrogen bear electrophilic and nucleophilic character, respectively. Here we show that activation of amines and nitroalkanes with an electrophilic iodine source in wet THF can lead directly to amide products. Preliminary observations support a mechanistic construct in which reactant polarity is reversed (umpolung) during C-N bond formation relative to traditional approaches. The use of nitroalkanes as acyl anion equivalents provides a conceptually innovative approach to amide and peptide synthesis, and one that might ultimately provide for efficient peptide synthesis that is fully reliant on enantioselective methods. PMID:20577205

  19. Standardized chemical synthesis of Pseudomonas aeruginosa pyocyanin

    Directory of Open Access Journals (Sweden)

    Rajkumar Cheluvappa

    2014-01-01

    As we have extracted pyocyanin both from P. aeruginosa cultures, and via chemical synthesis; we know the procedural and product-quality differences. We endorse the relative ease, safety, and convenience of using the chemical synthesis described here. Crucially, our “naturally endotoxin-free” pyocyanin can be extracted easily without using infectious bacteria.

  20. Synthesis of mutual azo prodrugs of anti-inflammatory agents and peptides facilitated by α-aminoisobutyric acid.

    Science.gov (United States)

    Kennedy, David A; Vembu, Nagarajan; Fronczek, Frank R; Devocelle, Marc

    2011-12-02

    Reported is the synthesis of azo mutual prodrugs of the nonsteroidal anti-inflammatory agents (NSAIDs) 4-aminophenylacetic acid (4-APAA) or 5-aminosalicylic acid (5-ASA) with peptides, including an antibiotic peptide temporin analogue modified at the amino terminal by an α-aminoisobutyric acid (Aib) residue. These prodrugs are designed for colonic delivery of two agents to treat infection and inflammation by the bacterial pathogen Clostridium difficile . © 2011 American Chemical Society

  1. Immobilization methods for the rapid total chemical synthesis of proteins on microtiter plates.

    Science.gov (United States)

    Zitterbart, Robert; Krumrey, Michael; Seitz, Oliver

    2017-07-01

    The chemical synthesis of proteins typically involves the solid-phase peptide synthesis of unprotected peptide fragments that are stitched together in solution by native chemical ligation (NCL). The process is slow, and throughput is limited because of the need for repeated high performance liquid chromatography purification steps after both solid-phase peptide synthesis and NCL. With an aim to provide faster access to functional proteins and to accelerate the functional analysis of synthetic proteins by parallelization, we developed a method for the high performance liquid chromatography-free synthesis of proteins on the surface of microtiter plates. The method relies on solid-phase synthesis of unprotected peptide fragments, immobilization of the C-terminal fragment and on-surface NCL with an unprotected peptide thioester in crude form. Herein, we describe the development of a suitable immobilization chemistry. We compared (i) formation of nickel(II)-oligohistidine complexes, (ii) Cu-based [2 + 3] alkine-azide cycloaddition and (iii) hydrazone ligation. The comparative study identified the hydrazone ligation as most suitable. The sequence of immobilization via hydrazone ligation, on-surface NCL and radical desulfurization furnished the targeted SH3 domains in near quantitative yield. The synthetic proteins were functional as demonstrated by an on-surface fluorescence-based saturation binding analysis. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd.

  2. Chemical synthesis of membrane proteins by the removable backbone modification method.

    Science.gov (United States)

    Tang, Shan; Zuo, Chao; Huang, Dong-Liang; Cai, Xiao-Ying; Zhang, Long-Hua; Tian, Chang-Lin; Zheng, Ji-Shen; Liu, Lei

    2017-12-01

    Chemical synthesis can produce membrane proteins bearing specifically designed modifications (e.g., phosphorylation, isotope labeling) that are difficult to obtain through recombinant protein expression approaches. The resulting homogeneously modified synthetic membrane proteins are valuable tools for many advanced biochemical and biophysical studies. This protocol describes the chemical synthesis of membrane proteins by condensation of transmembrane peptide segments through native chemical ligation. To avoid common problems encountered due to the poor solubility of transmembrane peptides in almost any solvent, we describe an effective procedure for the chemical synthesis of membrane proteins through the removable-backbone modification (RBM) strategy. Two key steps of this protocol are: (i) installation of solubilizing Arg4-tagged RBM groups into the transmembrane peptides at any primary amino acid through Fmoc (9-fluorenylmethyloxycarbonyl) solid-phase peptide synthesis and (ii) native ligation of the full-length sequence, followed by removal of the RBM tags by TFA (trifluoroacetic acid) cocktails to afford the native protein. The installation of RBM groups is achieved by using 4-methoxy-5-nitrosalicyladehyde by reduction amination to incorporate an activated O-to-N acyl transfer auxiliary. The Arg4-tag-modified membrane-spanning peptide segments behave like water-soluble peptides to facilitate their purification, ligation and mass characterization.

  3. Stereocontrolled Synthesis of Methyl Silanediol Peptide Mimics

    DEFF Research Database (Denmark)

    Nielsen, Lone; Lindsay, Karl; Faber, Jesper

    2007-01-01

     The treatment of chiral sulfinimines with (methyldiphenylsilyl)lithium gives R-(methyldiphenylsilyl)-sulfinamides with excellent diastereoselectivity, and in good yield. The presence of α-protons on the imines is also well tolerated. The sulfinamide auxiliary is easily removed via treatment with...... corresponding bis-TMS siloxane via protection with TMSCl, and converted back to the desired silanediol via hydrolysis with aqueous KOH. Efforts to apply this approach to biologically relevant silanediol peptide mimics, with a view to protease inhibition, are described....

  4. Purification and use of E. coli peptide deformylase for peptide deprotection in chemoenzymatic peptide synthesis

    NARCIS (Netherlands)

    Di Toma, Claudia; Sonke, Theo; Quaedflieg, Peter J.; Janssen, Dick B.

    Peptide deformylases (PDFs) catalyze the removal of the formyl group from the N-terminal methionine residue in nascent polypeptide chains in prokaryotes. Its deformylation activity makes PDF an attractive candidate for the biocatalytic deprotection of formylated peptides that are used in

  5. Semi-automated microwave assisted solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Pedersen, Søren Ljungberg

    with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

  6. Total synthesis of cytochrome b562 by native chemical ligation using a removable auxiliary

    Science.gov (United States)

    Low, Donald W.; Hill, Michael G.; Carrasco, Michael R.; Kent, Stephen B. H.; Botti, Paolo

    2001-01-01

    We have completed the total chemical synthesis of cytochrome b562 and an axial ligand analogue, [SeMet7]cyt b562, by thioester-mediated chemical ligation of unprotected peptide segments. A novel auxiliary-mediated native chemical ligation that enables peptide ligation to be applied to protein sequences lacking cysteine was used. A cleavable thiol-containing auxiliary group, 1-phenyl-2-mercaptoethyl, was added to the α-amino group of one peptide segment to facilitate amide bond-forming ligation. The amine-linked 1-phenyl-2-mercaptoethyl auxiliary was stable to anhydrous hydrogen fluoride used to cleave and deprotect peptides after solid-phase peptide synthesis. Following native chemical ligation with a thioester-containing segment, the auxiliary group was cleanly removed from the newly formed amide bond by treatment with anhydrous hydrogen fluoride, yielding a full-length unmodified polypeptide product. The resulting polypeptide was reconstituted with heme and folded to form the functional protein molecule. Synthetic wild-type cyt b562 exhibited spectroscopic and electrochemical properties identical to the recombinant protein, whereas the engineered [SeMet7]cyt b562 analogue protein was spectroscopically and functionally distinct, with a reduction potential shifted by ≈45 mV. The use of the 1-phenyl-2-mercaptoethyl removable auxiliary reported here will greatly expand the applicability of total protein synthesis by native chemical ligation of unprotected peptide segments. PMID:11390992

  7. Synthesis of hydrophobic peptides : An Fmoc “Solubilising Tail” method

    NARCIS (Netherlands)

    Choma, Christin T.; Robillard, George T.; Englebretsen, Darren R.

    1998-01-01

    The development of an Fmoc method for synthesis and purification of hydrophobic peptides using a “solubihsing tail” strategy is described. Peptide-constructs of the form hydrophobic peptide-[CHmb ester]-solubilising peptide were synthesised. Procedures for forming the 4-Hmb ester linkage, and

  8. Linkers, resins, and general procedures for solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

    2013-01-01

    and linkers for solid-phase synthesis is a key parameter for successful peptide synthesis. This chapter provides an overview of the most common and useful resins and linkers for the synthesis of peptides with C-terminal amides, carboxylic acids, and more. The chapter finishes with robust protocols for general...

  9. Tools for chemical synthesis in microsystems

    OpenAIRE

    Jensen, Klavs F.; Newman, Stephen G.; Reizman, Brandon Jacob

    2014-01-01

    Chemical synthesis in microsystems has evolved from simple proof-of-principle examples to become a general technique in academia and industry. Numerous such “flow chemistry” applications are now found in pharmaceutical and fine chemical synthesis. Much of the development has been based on systems employing macroscopic flow components and tubes, rather than the integrated chip technology envisioned by the lab-on-a-chip community. We review the major developments in systems for flow chemistry a...

  10. Optimization of synthesis and quality control procedures for the preparation of 18F-labelled peptides

    International Nuclear Information System (INIS)

    Amartey, J.K.

    2002-01-01

    Radiohalogenation via prosthetic groups has provided a useful route for labelling proteins, peptides and drug molecules. This method is the only option available as far as molecules that are not amenable to the classical radiohalogenation reactions are concerned. This pertains to proteins and peptides lacking tyrosyl groups in their structure. More importantly, radiofluorination by electrophilic method has not been developed for labelling these macromolecules. The need to optimize methods and techniques to enable efficient labelling and fully exploit the potential biochemical application of these molecules prompted this investigation. Reaction conditions were optimized to prepare ethyl 4-[ 18 F]-benzoate from an ammonium precursor, ethyl 4-trimethylammoniumbenzoate.triflate in excellent yield. The fluorinated ester was hydrolyzed quantitatively to the acid. The acid was then converted to the activated N-succinimidylfluorobenzoate (SFB) using O- (Nsuccinimidyl)- tetramethyluroniumtetrafluoroborate also typically in greater than 90% radiochemical yield. The activated ester was purified either by HPLC or SEPPAK cartridge and was conjugated to a potent chemotactic peptide (Formyl-Nle-Leu-Phe-Nle-Tyr-Lys) as a model in acetonitrile. The conjugate was purified chromatographically or by SEPPAK cartridges. To ascertain the retention of biological activity of the peptide after these chemical manipulations, the superoxide production assay was employed. The purified [ 19 F]-peptide conjugate specifically bound and activated human polymorphonuclear leukocytes to generate superoxide in a dose dependent manner. Biodistribution in normal mice showed that the conjugated peptide did not suffer any significant dehalogenation in vivo. This was indicated by the low uptake of activity in bone. The methodology developed with the chemotactic peptide was used to label RC-160 (cyclic-D-Phe-Cys-Tyr-D-Trp-Lys (Boc)- Val-Cys-Trp-NH2) a SST analog. The conjugate peptide inhibited the growth of

  11. A Photolabile Linker for the Solid-Phase Synthesis of Peptide Hydrazides and Heterocycles

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Komnatnyy, Vitaly V.; Nielsen, Thomas Eiland

    2014-01-01

    A photolabile hydrazine linker for the solid-phase synthesis of peptide hydrazides and hydrazine-derived heterocycles is presented. The developed protocols enable the efficient synthesis of structurally diverse peptide hydrazides derived from the standard amino adds, including those with side......-chain protected residues at the C-terminal of the resulting peptide hydrazide, and are useful for the synthesis of dihydropyrano[2,3-c]pyrazoles. The linker is compatible with most commonly used coupling reagents and protecting groups for solid-phase peptide synthesis....

  12. Studies in Solid Phase Peptide Synthesis: A Personal Perspective

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R

    2007-06-01

    By the early 1970s it had became apparent that the solid phase synthesis of ribonuclease A could not be generalized. Consequently, virtually every aspect of solid phase peptide synthesis (SPPS) was reexamined and improved during the decade of the 1970s. The sensitive detection and elimination of possible side reactions (amino acid insertion, N{sup {alpha}}-trifluoroacetylation, N{sup {alpha}{var_epsilon}}-alkylation) was examined. The quantitation of coupling efficiency in SPPS as a function of chain length was studied. A new and improved support for SPPS, the 'PAM-resin', was prepared and evaluated. These and many other studies from the Merrifield laboratory and elsewhere increased the general acceptance of SPPS leading to the 1984 Nobel Prize in Chemistry for Bruce Merrifield.

  13. Carbohydrate protease conjugates: Stabilized proteases for peptide synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Wartchow, C.A.; Wang, Peng; Bednarski, M.D.; Callstrom, M.R. [Ohio State Univ., Columbus, OH (United States)]|[Lawrence Berkeley Lab., CA (United States)

    1995-12-31

    The synthesis of oligopeptides using stable carbohydrate protease conjugates (CPCs) was examined in acetonitrile solvent systems. CPC[{alpha}-chymotrypsin] was used for the preparation of peptides containing histidine, phenylalanine, tryptophan in the P{sub 1} position in 60-93% yield. The CPC[{alpha}-chymotrypsin]-catalyzed synthesis of octamer Z-Gly-Gly-Phe-Gly-Gly-Phe-Gly-Gly-OEt from Z-Gly-Gly-Phe-Gly-Gly-Phe-OMe was achieved in 71% yield demonstrating that synthesis peptides containing both hydrophylic and hydrophobic amino acids. The P{sub 2} specificity of papain for aromatic residues was utilized for the 2 + 3 coupling of Z-Tyr-Gly-OMe to H{sub 2}N-Gly-Phe-Leu-OH to generate the leucine enkephalin derivative in 79% yield. Although papain is nonspecific for the hydrolysis of N-benzyloxycarbonyl amino acid methyl esters in aqueous solution, the rates of synthesis for these derivitives with nucleophile leucine tert-butyl ester differed by nearly 2 orders of magnitude. CPC[thermolysin] was used to prepare the aspartame precursor Z-Asp-Phe-OMe in 90% yield. The increased stability of CPCs prepared from periodate-modified poly(2-methacryl- amido-2-deoxy-D-glucose), poly(2-methacrylamido-2-deoxy-D-galactose), and poly(5-methacryl-amido-5-deoxy-D-ribose), carbohydrate materials designed to increase the aldehyde concentration in aqueous solution, suggests that the stability of CPCs is directly related to the aldehyde concentration of the carbohydrate material. Periodate oxidation of poly(2-methacrylamido-2-deoxy-D-glucose) followed by covalent attachment to {alpha}-chymotrypsin gave a CPC with catalytic activity in potassium phosphate buffer at 90{degrees}C for 2 h. 1 fig., 1 tab., 40 refs.

  14. ANALYTICAL SYNTHESIS OF CHEMICAL REACTOR CONTROL SYSTEM

    Directory of Open Access Journals (Sweden)

    Alexander Labutin

    2017-02-01

    Full Text Available The problem of the analytical synthesis of the synergetic control system of chemical reactor for the realization of a complex series-parallel exothermal reaction has been solved. The synthesis of control principles is performed using the analytical design method of aggregated regulators. Synthesized nonlinear control system solves the problem of stabilization of the concentration of target component at the exit of reactor and also enables one to automatically transfer to new production using the equipment.

  15. Methanol synthesis beyond chemical equilibrium

    NARCIS (Netherlands)

    van Bennekom, J. G.; Venderbosch, R. H.; Winkelman, J. G. M.; Wilbers, E.; Assink, D.; Lemmens, K. P. J.; Heeres, H. J.

    2013-01-01

    In commercial methanol production from syngas, the conversion is thermodynamically limited to 0.3-0.7 leading to large recycles of non-converted syngas. This problem can be overcome to a significant extent by in situ condensation of methanol during its synthesis which is possible nowadays due to the

  16. Total chemical synthesis and X-ray structure of kaliotoxin by racemic protein crystallography.

    Science.gov (United States)

    Pentelute, Brad L; Mandal, Kalyaneswar; Gates, Zachary P; Sawaya, Michael R; Yeates, Todd O; Kent, Stephen B H

    2010-11-21

    Here we report the total synthesis of kaliotoxin by 'one pot' native chemical ligation of three synthetic peptides. A racemic mixture of D- and L-kaliotoxin synthetic protein molecules gave crystals in the centrosymmetric space group P1 that diffracted to atomic-resolution (0.95 Å), enabling the X-ray structure of kaliotoxin to be determined by direct methods.

  17. Phospholyl(borane) Amino Acids and Peptides: Stereoselective Synthesis and Fluorescent Properties with Large Stokes Shift.

    Science.gov (United States)

    Arribat, Mathieu; Rémond, Emmanuelle; Clément, Sébastien; Lee, Arie Van Der; Cavelier, Florine

    2018-01-24

    The synthesis of phospholyl(borane) amino acids was stereoselectively achieved by reaction of phospholide anion with iodo α-amino ester derived from l-aspartic acid or l-serine, followed by in situ complexation with borane. Phospholyl(borane) amino acids are easy to store and can be subjected to direct transformation into the corresponding free phospholyl, gold complex, oxide or sulfur derivatives as well as phospholinium salts, thus offering a variety of side chains. After selective deprotection of carboxylic function or amine, C- or N- peptide coupling with an alanine moiety proved the possible incorporation into peptides. Such phospholyl amino acid and peptide derivatives exhibit fluorescent properties with a large Stokes shift (160 nm) and fluorescence up to 535 nm, depending on the phosphole aromaticity and the chemical environment. These phospholyl(borane) amino acids constitute a new class of unnatural amino acids useful for structure-activities relationship studies and appear to be promising fluorophores for the development of labeled peptides.

  18. MICROWAVE TECHNOLOGY CHEMICAL SYNTHESIS APPLICATIONS

    Science.gov (United States)

    Microwave-accelerated chemical syntheses in various solvents as well as under solvent-free conditions have witnessed an explosive growth. The technique has found widespread application predominantly exploiting the inexpensive unmodified household microwave (MW) ovens although th...

  19. Use of Modern Chemical Protein Synthesis and Advanced Fluorescent Assay Techniques to Experimentally Validate the Functional Annotation of Microbial Genomes

    Energy Technology Data Exchange (ETDEWEB)

    Kent, Stephen [University of Chicago

    2012-07-20

    The objective of this research program was to prototype methods for the chemical synthesis of predicted protein molecules in annotated microbial genomes. High throughput chemical methods were to be used to make large numbers of predicted proteins and protein domains, based on microbial genome sequences. Microscale chemical synthesis methods for the parallel preparation of peptide-thioester building blocks were developed; these peptide segments are used for the parallel chemical synthesis of proteins and protein domains. Ultimately, it is envisaged that these synthetic molecules would be ‘printed’ in spatially addressable arrays. The unique ability of total synthesis to precision label protein molecules with dyes and with chemical or biochemical ‘tags’ can be used to facilitate novel assay technologies adapted from state-of-the art single molecule fluorescence detection techniques. In the future, in conjunction with modern laboratory automation this integrated set of techniques will enable high throughput experimental validation of the functional annotation of microbial genomes.

  20. Synthesis and screening of peptide libraries with free C-termini.

    Science.gov (United States)

    Wang, Yen-Chih; Distefano, Mark D

    2014-01-01

    Peptide libraries are useful tools to investigate the relationship between structure and function of proteins. The creation of peptide libraries with free C-termini presents unique synthetic challenges. In this review, methods for creating peptide libraries using either solid-phase peptide synthesis or phage display are described. Methods for screening such libraries and their application in studying several important biological problems are also reported.

  1. SYNTHESIS, PHYSICO-CHEMICAL AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

    userpc

    -125. Byeong G. Chae D., Hae N., Hyung K. C. and. Yong K. C. (1996); Synthesis and characterization of schiff base derived 2- hydroxy napthaldehyde and aliphatic diammines. Bulletin Korean Chemical. Society 17(8): 687-693. Hassan S. W. ...

  2. The Chemical Synthesis of Discodermolide

    Science.gov (United States)

    Paterson, I.; Florence, G. J.

    The marine sponge-derived polyketide discodermolide is a potent antimitotic agent that represents a promising natural product lead structure in the treatment of cancer. Discodermolide shares the same microtubule-stabilising mechanism of action as Taxol®, inhibits the growth of solid tumours in animal models and shows synergy with Taxol. The pronounced cytotoxicity of discodermolide, which is maintained against cancer cell lines that display resistance to Taxol and other drugs, combined with its scarce availability from its natural source, has fuelled significant academic and industrial interest in devising a practical total synthesis as a means of ensuring a sustainable supply for drug development. This chapter surveys the various total syntheses of discodermolide that have been completed over the period 1993-2007, focusing on the strategies employed for introduction of the multiple stereocentres and achieving control over the alkene geometry, along with the various methods used for realising the pivotal fragment couplings to assemble progressively the full carbon skeleton. This dedicated synthetic effort has triumphed in removing the supply problem for discodermolide, providing sufficient material for extensive biological studies and enabling its early stage clinical development, as well as facilitating SAR studies for lead optimisation.

  3. Speciality chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Lin, J.J.; Knifton, J.F. (Shell Development Company, Houston, TX (USA))

    1992-04-01

    Texaco has undertaken research to investigate the use of carbon monoxide and hydrogen as building blocks for the manufacture of amidocarbonylation products. The amidocarbonylation reaction offers a convenient method to construct two functionalities - amido and carboxylate - simultaneously. Texaco has extended this chemistry to make a variety of speciality chemicals by tailoring cobalt catalysts. Products which have been made including: surface active agents such as the C{sub 14} - C{sub 16} alkyl amidoacids; surfactants; intermediates for sweeteners like aspartame; food additives like glutamic acid; and chelating agents such as polyamidoacids. 20 refs., 10 figs., 1 tab.

  4. Alternative Fuels and Chemicals from Synthesis Gas

    Energy Technology Data Exchange (ETDEWEB)

    None, None

    1998-12-02

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  5. Alternative fuels and chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-08-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  6. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1999-01-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  7. Alternative Fuels and Chemicals From Synthesis Gas

    Energy Technology Data Exchange (ETDEWEB)

    none

    1998-07-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  8. Chemoselective synthesis and analysis of naturally occurring phosphorylated cysteine peptides

    Science.gov (United States)

    Bertran-Vicente, Jordi; Penkert, Martin; Nieto-Garcia, Olaia; Jeckelmann, Jean-Marc; Schmieder, Peter; Krause, Eberhard; Hackenberger, Christian P. R.

    2016-09-01

    In contrast to protein O-phosphorylation, studying the function of the less frequent N- and S-phosphorylation events have lagged behind because they have chemical features that prevent their manipulation through standard synthetic and analytical methods. Here we report on the development of a chemoselective synthetic method to phosphorylate Cys side-chains in unprotected peptides. This approach makes use of a reaction between nucleophilic phosphites and electrophilic disulfides accessible by standard methods. We achieve the stereochemically defined phosphorylation of a Cys residue and verify the modification using electron-transfer higher-energy dissociation (EThcD) mass spectrometry. To demonstrate the use of the approach in resolving biological questions, we identify an endogenous Cys phosphorylation site in IICBGlc, which is known to be involved in the carbohydrate uptake from the bacterial phosphotransferase system (PTS). This new chemical and analytical approach finally allows further investigating the functions and significance of Cys phosphorylation in a wide range of crucial cellular processes.

  9. Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

    Science.gov (United States)

    Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

    2015-09-01

    A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

  10. Laminin peptide YIGSR induces collagen synthesis in Hs27 human dermal fibroblasts

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Jong Hyuk; Kim, Jaeyoon; Lee, Hyeongjoo [NovaCell Technology Inc., Pohang, Kyungbuk 790-784 (Korea, Republic of); Kim, So Young [Department of Dermatology, Chung-Ang University College of Medicine, Seoul 156-756 (Korea, Republic of); Department of Convergence Medicine and Pharmaceutical Biosciences, Graduate School, Chung-Ang University, Seoul 156-756 (Korea, Republic of); Jang, Hwan-Hee [Functional Food and Nutrition Division, Department of Agrofood Resources, Rural Development Administration, Suwon 441-853 (Korea, Republic of); Ryu, Sung Ho [Division of Integrative Biosciences and Biotechnology, Pohang University of Science and Technology (POSTECH), Pohang, Kyungbuk 790-784 (Korea, Republic of); Kim, Beom Joon [Department of Dermatology, Chung-Ang University College of Medicine, Seoul 156-756 (Korea, Republic of); Department of Convergence Medicine and Pharmaceutical Biosciences, Graduate School, Chung-Ang University, Seoul 156-756 (Korea, Republic of); Lee, Taehoon G., E-mail: taehoon@novacelltech.com [NovaCell Technology Inc., Pohang, Kyungbuk 790-784 (Korea, Republic of)

    2012-11-23

    Highlights: Black-Right-Pointing-Pointer We identify a function of the YIGSR peptide to enhance collagen synthesis in Hs27. Black-Right-Pointing-Pointer YIGSR peptide enhanced collagen type 1 synthesis both of gene and protein levels. Black-Right-Pointing-Pointer There were no changes in cell proliferation and MMP-1 level in YIGSR treatment. Black-Right-Pointing-Pointer The YIGSR effect on collagen synthesis mediated activation of FAK, pyk2 and ERK. Black-Right-Pointing-Pointer The YIGSR-induced FAK and ERK activation was modulated by FAK and MEK inhibitors. -- Abstract: The dermal ECM is synthesized from fibroblasts and is primarily compromised of fibrillar collagen and elastic fibers, which support the mechanical strength and resiliency of skin, respectively. Laminin, a major glycoprotein located in the basement membrane, promotes cell adhesion, cell growth, differentiation, and migration. The laminin tyrosine-isoleucine-glycine-serine-arginine (YIGSR) peptide, corresponding to the 929-933 sequence of the {beta}1 chain, is known to be a functional motif with effects on the inhibition of tumor metastasis, the regulation of sensory axonal response and the inhibition of angiogenesis through high affinity to the 67 kDa laminin receptor. In this study, we identified a novel function of the YIGSR peptide to enhance collagen synthesis in human dermal fibroblasts. To elucidate this novel function regarding collagen synthesis, we treated human dermal fibroblasts with YIGSR peptide in both a time- and dose-dependent manner. According to subsequent experiments, we found that the YIGSR peptide strongly enhanced collagen type 1 synthesis without changing cell proliferation or cellular MMP-1 level. This YIGSR peptide-mediated collagen type 1 synthesis was modulated by FAK inhibitor and MEK inhibitor. This study clearly reveals that YIGSR peptide plays a novel function on the collagen type 1 synthesis of dermal fibroblasts and also suggests that YIGSR is a strong candidate

  11. Laminin peptide YIGSR induces collagen synthesis in Hs27 human dermal fibroblasts

    International Nuclear Information System (INIS)

    Yoon, Jong Hyuk; Kim, Jaeyoon; Lee, Hyeongjoo; Kim, So Young; Jang, Hwan-Hee; Ryu, Sung Ho; Kim, Beom Joon; Lee, Taehoon G.

    2012-01-01

    Highlights: ► We identify a function of the YIGSR peptide to enhance collagen synthesis in Hs27. ► YIGSR peptide enhanced collagen type 1 synthesis both of gene and protein levels. ► There were no changes in cell proliferation and MMP-1 level in YIGSR treatment. ► The YIGSR effect on collagen synthesis mediated activation of FAK, pyk2 and ERK. ► The YIGSR-induced FAK and ERK activation was modulated by FAK and MEK inhibitors. -- Abstract: The dermal ECM is synthesized from fibroblasts and is primarily compromised of fibrillar collagen and elastic fibers, which support the mechanical strength and resiliency of skin, respectively. Laminin, a major glycoprotein located in the basement membrane, promotes cell adhesion, cell growth, differentiation, and migration. The laminin tyrosine-isoleucine-glycine-serine-arginine (YIGSR) peptide, corresponding to the 929–933 sequence of the β1 chain, is known to be a functional motif with effects on the inhibition of tumor metastasis, the regulation of sensory axonal response and the inhibition of angiogenesis through high affinity to the 67 kDa laminin receptor. In this study, we identified a novel function of the YIGSR peptide to enhance collagen synthesis in human dermal fibroblasts. To elucidate this novel function regarding collagen synthesis, we treated human dermal fibroblasts with YIGSR peptide in both a time- and dose-dependent manner. According to subsequent experiments, we found that the YIGSR peptide strongly enhanced collagen type 1 synthesis without changing cell proliferation or cellular MMP-1 level. This YIGSR peptide-mediated collagen type 1 synthesis was modulated by FAK inhibitor and MEK inhibitor. This study clearly reveals that YIGSR peptide plays a novel function on the collagen type 1 synthesis of dermal fibroblasts and also suggests that YIGSR is a strong candidate peptide for the treatment of skin aging and wrinkles.

  12. Chemical Reduction Synthesis of Iron Aluminum Powders

    Science.gov (United States)

    Zurita-Méndez, N. N.; la Torre, G. Carbajal-De; Ballesteros-Almanza, L.; Villagómez-Galindo, M.; Sánchez-Castillo, A.; Espinosa-Medina, M. A.

    In this study, a chemical reduction synthesis method of iron aluminum (FeAl) nano-dimensional intermetallic powders is described. The process has two stages: a salt reduction and solvent evaporation by a heat treatment at 1100°C. The precursors of the synthesis are ferric chloride, aluminum foil chips, a mix of Toluene/THF in a 75/25 volume relationship, and concentrated hydrochloric acid as initiator of the reaction. The reaction time was 20 days, the product obtained was dried at 60 °C for 2 h and calcined at 400, 800, and 1100 °C for 4 h each. To characterize and confirm the obtained synthesis products, X-Ray Diffraction (XRD), and Scanning Electron Microscopy (SEM) techniques were used. The results of morphology and chemical characterization of nano-dimensional powders obtained showed a formation of agglomerated particles of a size range of approximately 150 nm to 1.0 μm. Composition of powders was identified as corundum (Al2O3), iron aluminide (FeAl3), and iron-aluminum oxides (Fe0. 53Al0. 47)2O3 phases. The oxide phases formation were associated with the reaction of atmospheric concentration-free oxygen during synthesis and sintering steps, reducing the concentration of the iron aluminum phase.

  13. Environmentally benign chemical synthesis and processing

    International Nuclear Information System (INIS)

    Hancock, K.G.

    1992-01-01

    A new era of university-industry-government partnership is required to address the intertwined problems of industrial economic competitiveness and environmental quality. Chemicals that go up the stacks and down the drains are simultaneously a serious detriment to the environment, a waste of natural resources, and a threat to industrial profitability. Recently, the NSF Divisions of Chemistry and chemical and Thermal Systems have joined with the Council for Chemical research in a new grant program to reduce pollution at the source by underwriting research aimed at environmentally benign chemical synthesis and processing. Part of a broader NSF initiative on environmental science research, this new program serves as a model for university-industry-government joint action and technology transfer. Other features of this program and related activities will be described in this paper

  14. Opportunities for Merging Chemical and Biological Synthesis

    Science.gov (United States)

    Wallace, Stephen; Balskus, Emily P.

    2014-01-01

    Organic chemists and metabolic engineers use largely orthogonal technologies to access small molecules like pharmaceuticals and commodity chemicals. As the use of biological catalysts and engineered organisms for chemical production grows, it is becoming increasingly evident that future efforts for chemical manufacture will benefit from the integration and unified expansion of these two fields. This review will discuss approaches that combine chemical and biological synthesis for small molecule production. We highlight recent advances in combining enzymatic and non-enzymatic catalysis in vitro, discuss the application of design principles from organic chemistry for engineering non-biological reactivity into enzymes, and describe the development of biocompatible chemistry that can be interfaced with microbial metabolism. PMID:24747284

  15. Efficient and Selective Chemical Labeling of Electrochemically Generated Peptides Based on Spirolactone Chemistry

    NARCIS (Netherlands)

    Zhang, Tao; Niu, Xiaoyu; Yuan, Tao; Tessari, Marco; de Vries, Marcel P.; Permentier, Hjalmar P.; Bischoff, Rainer

    2016-01-01

    Specific digestion of proteins is an essential step for mass spectrometry-based proteomics, and the chemical labeling of the resulting peptides is often used for peptide enrichment or the introduction of desirable tags. Cleavage of the peptide bond following electrochemical oxidation of Tyr or Trp

  16. Isolation, structure, synthesis, and activity of a new member of the calcitonin gene-related peptide family from frog skin and molecular cloning of its precursor.

    Science.gov (United States)

    Seon, A A; Pierre, T N; Redeker, V; Lacombe, C; Delfour, A; Nicolas, P; Amiche, M

    2000-02-25

    Calcitonin gene-related peptide has been extracted from the skin exudate of a single living specimen of the frog Phyllomedusa bicolor and purified to homogeneity by a two-step protocol. A total volume of 250 microl of exudate yielded 380 microg of purified peptide. Mass spectrometric analysis and gas phase sequencing of the purified peptide as well as chemical synthesis and cDNA analysis were consistent with the structure SCDTSTCATQRLADFLSRSGGIGSPDFVPTDVSANSF amide and the presence of a disulfide bridge linking Cys(2) and Cys(7). The skin peptide, named skin calcitonin gene-related peptide, differs significantly from all other members of the calcitonin gene-related peptide family of peptides at nine positions but binds with high affinity to calcitonin gene-related peptide receptors in the rat brain and acts as an agonist in the rat vas deferens bioassay with potencies equal to those of human CGRP. Reverse transcriptase-polymerase chain reaction coupled with cDNA cloning and sequencing demonstrated that skin calcitonin gene-related peptide isolated in the skin is identical to that present in the frog's central and enteric nervous systems. These data, which indicate for the first time the existence of calcitonin gene-related peptide in the frog skin, add further support to the brain-skin-gut triangle hypothesis as a useful tool in the identification and/or isolation of mammalian peptides that are present in the brain and other tissues in only minute quantities.

  17. Development and use of engineered peptide deformylase in chemoenzymatic peptide synthesis

    NARCIS (Netherlands)

    Di Toma, Claudia

    2012-01-01

    Deze thesis beschrijft het onderzoek naar potentieel van het gebruik van het peptide deformylase (PDF) in chemo enzymatische peptide synthese. PDF is geschikt voor selective N terminale deformylatie van bepaalde N-formyl-peptides zonder gelijktijdige hydrolyse van de peptide binding. Door de

  18. Synthesis and evaluation of amphiphilic peptides as nanostructures and drug delivery tools

    Science.gov (United States)

    Sayeh, Naser Ali

    systems can affect the drug delivery efficiency. The result of this work provided insights about optimizing the amphiphilic cyclic-linear trizaolyl peptides can be used to design compounds with more efficient drug delivery capabilities. Chapter 3. MANUSCRIPT II. The objective of this Chapter was to synthesize a different series of amphiphilic peptides for different objectives. First, the amphiphilic trizaolyl peptides in Chapter I were systematically modified by increasing the number of arginine and tryptophan sequence in cyclic and linear peptides. The rationale for the modification was to enhance the possibility of interaction with the cell membrane and therefore improving the cellular uptake process. Moreover, a new class of amphiphilic peptides consist of tryptophan and glutamic acid were conjugated with a peptide containing arginine and lysine residues using Fmoc chemistry. These peptides have an amide bond that generates more flexibility compared to a triazole ring. The chemical and biological properties will be evaluated in future and compared with amphiphilic triazolyl peptides. Finally, additional fatty acids with different length chains were conjugated with positively charged peptides to be evaluated as antibacterial agents. Stearic acid (C16) and myristic acid (C14) were conjugated with a peptides consisting of arginine azide and lysine amino acids to enhance the antibacterial activity. In summary, the work in this dissertation provided insights about the synthesis and characterization of a new class of amphiphilic triazolyl peptides as drug delivery carriers and amphiphilic peptides as antibacterial agents. Molecular modeling was used to explain why triazolyl peptides were unable to enhance the delivery of small molecule drugs compared to the previously synthesized cyclic peptides [WR]4 (Chapter 2) Modification of synthesized peptides in Chapter 1, by addition of more positively charged amino acids or reducing the rigidity by incorporating amide bonds instead

  19. Role of leader peptide synthesis in tryptophanase operon expression in Escherichia coli K-12.

    OpenAIRE

    Stewart, V; Yanofsky, C

    1986-01-01

    We used site-directed mutagenesis to replace the Escherichia coli tryptophanase (tna) operon leader peptide start codon with AUC. This change greatly decreased the uninduced rate of tna operon expression, and it also lowered the response to inducer. We conclude that leader peptide synthesis plays an essential role in tna operon expression.

  20. Synthesis, properties, and application in peptide chemistry of a magnetically separable and reusable biocatalyst

    Science.gov (United States)

    Liria, Cleber W.; Ungaro, Vitor A.; Fernandes, Raphaella M.; Costa, Natália J. S.; Marana, Sandro R.; Rossi, Liane M.; Machini, M. Teresa

    2014-11-01

    Enzyme-catalyzed chemical processes are selective, very productive, and generate little waste. Nevertheless, they may be optimized using enzymes bound to solid supports, which are particularly important for protease-mediated reactions since proteases undergo fast autolysis in solution. Magnetic nanoparticles are suitable supports for this purpose owing to their high specific surface area and to be easily separated from reaction media. Here we describe the immobilization of bovine α-chymotrypsin (αCT) on silica-coated superparamagnetic nanoparticles (Fe3O4@silica) and the characterization of the enzyme-nanoparticle hybrid (Fe3O4@silica-αCT) in terms of protein content, properties, recovery from reaction media, application, and reuse in enzyme-catalyzed peptide synthesis. The results revealed that (i) full acid hydrolysis of the immobilized protease followed by amino acid analysis of the hydrolyzate is a reliable method to determine immobilization yield; (ii) despite showing lower amidase activity and a lower K cat/ K m value for a specific substrate than free αCT, the immobilized enzyme is chemically and thermally more stable, magnetically recoverable from reaction media, and can be consecutively reused for ten cycles to catalyze the amide bond hydrolysis and ester hydrolysis of the protected dipeptide Z-Ala-Phe-OMe. Altogether, these properties indicate the potential of Fe3O4@silica-αCT to act as an efficient, suitably stable, and reusable catalyst in amino acid, peptide, and protein chemistry as well as in proteomic studies.

  1. Wet chemical synthesis of soluble gold nanogaps

    DEFF Research Database (Denmark)

    Jain, Titoo; Tang, Qingxin; Bjørnholm, Thomas

    2014-01-01

    NRs) in aqueous solution. Through controlled end-to-end assembly of the AuNRs into dimers or chains, facilitated via target molecules, they can be used as electrical contacts. In this way, the preparation of AuNR-molecule-AuNR junctions by wet chemical methods may afford a large number of identical devices...... with little variation in the interface between molecule and electrode (AuNR). In this Account, we highlight recent progress in using chemically synthesized AuNRs as building blocks for molecular electronic applications. We outline the general synthesis and properties of AuNRs and describe the aqueous growth...... in the nanogaps lets us spectroscopically characterize the molecules via surface-enhanced Raman scattering. We discuss the incorporation of oligopeptides functionalized with acetylene units having uniquely identifiable vibrational modes. This acetylene moiety allows chemical reactions to be performed in the gaps...

  2. Screening And Optimizing Antimicrobial Peptides By Using SPOT-Synthesis

    Science.gov (United States)

    López-Pérez, Paula M.; Grimsey, Elizabeth; Bourne, Luc; Mikut, Ralf; Hilpert, Kai

    2017-04-01

    Peptide arrays on cellulose are a powerful tool to investigate peptide interactions with a number of different molecules, for examples antibodies, receptors or enzymes. Such peptide arrays can also be used to study interactions with whole cells. In this review, we focus on the interaction of small antimicrobial peptides with bacteria. Antimicrobial peptides (AMPs) can kill multidrug-resistant (MDR) human pathogenic bacteria and therefore could be next generation antibiotics targeting MDR bacteria. We describe the screen and the result of different optimization strategies of peptides cleaved from the membrane. In addition, screening of antibacterial activity of peptides that are tethered to the surface is discussed. Surface-active peptides can be used to protect surfaces from bacterial infections, for example implants.

  3. Mapping student thinking in chemical synthesis

    Science.gov (United States)

    Weinrich, Melissa

    In order to support the development of learning progressions about central ideas and practices in different disciplines, we need detailed analyses of the implicit assumptions and reasoning strategies that guide students' thinking at different educational levels. In the particular case of chemistry, understanding how new chemical substances are produced (chemical synthesis) is of critical importance. Thus, we have used a qualitative research approach based on individual interviews with first semester general chemistry students (n = 16), second semester organic chemistry students (n = 15), advanced undergraduates (n = 9), first year graduate students (n = 15), and PhD candidates (n = 16) to better characterize diverse students' underlying cognitive elements (conceptual modes and modes of reasoning) when thinking about chemical synthesis. Our results reveal a great variability in the cognitive resources and strategies used by students with different levels of training in the discipline to make decisions, particularly at intermediate levels of expertise. The specific nature of the task had a strong influence on the conceptual sophistication and mode of reasoning that students exhibited. Nevertheless, our data analysis has allowed us to identify common modes of reasoning and assumptions that seem to guide students' thinking at different educational levels. Our results should facilitate the development of learning progressions that help improve chemistry instruction, curriculum, and assessment.

  4. Recent Progress in the Chemical Synthesis of Class II and S-Glycosylated Bacteriocins

    Directory of Open Access Journals (Sweden)

    François Bédard

    2018-05-01

    Full Text Available A wide variety of antimicrobial peptides produced by lactic acid bacteria (LAB have been identified and studied in the last decades. Known as bacteriocins, these ribosomally synthesized peptides inhibit the growth of a wide range of bacterial species through numerous mechanisms and show a great variety of spectrum of activity. With their great potential as antimicrobial additives and alternatives to traditional antibiotics in food preservation and handling, animal production and in veterinary and medical medicine, the demand for bacteriocins is rapidly increasing. Bacteriocins are most often produced by fermentation but, in several cases, the low isolated yields and difficulties associated with their purification seriously limit their use on a large scale. Chemical synthesis has been proposed for their production and recent advances in peptide synthesis methodologies have allowed the preparation of several bacteriocins. Moreover, the significant cost reduction for peptide synthesis reagents and building blocks has made chemical synthesis of bacteriocins more attractive and competitive. From a protein engineering point of view, the chemical approach offers many advantages such as the possibility to rapidly perform amino acid substitution, use unnatural or modified residues, and make backbone and side chain modifications to improve potency, modify the activity spectrum or increase the stability of the targeted bacteriocin. This review summarized synthetic approaches that have been developed and used in recent years to allow the preparation of class IIa bacteriocins and S-linked glycopeptides from LAB. Synthetic strategies such as the use of pseudoprolines, backbone protecting groups, microwave irradiations, selective disulfide bridge formation and chemical ligations to prepare class II and S-glycosylsated bacteriocins are discussed.

  5. An optimized chemical synthesis of human relaxin-2.

    Science.gov (United States)

    Barlos, Kostas K; Gatos, Dimitrios; Vasileiou, Zoe; Barlos, Kleomenis

    2010-04-01

    Human gene 2 relaxin (RLX) is a member of the insulin superfamily and is a multi-functional factor playing a vital role in pregnancy, aging, fibrosis, cardioprotection, vasodilation, inflammation, and angiogenesis. RLX is currently applied in clinical trials to cure among others acute heart failure, fibrosis, and preeclampsia. The synthesis of RLX by chemical methods is difficult because of the insolubility of its B-chain and the required laborious and low yielding site-directed combination of its A (RLXA) and B (RLXB) chains. We report here that oxidation of the Met(25) residue of RLXB improves its solubility, allowing its effective solid-phase synthesis and application in random interchain combination reactions with RLXA. Linear Met(O)(25)-RLX B-chain (RLXBO) reacts with a mixture of isomers of bicyclic A-chain (bcRLXA) giving exclusively the native interchain combination. Applying this method Met(O)(25)-RLX (RLXO) was obtained in 62% yield and was easily converted to RLX in 78% yield, by reduction with ammonium iodide. Copyright (c) 2010 European Peptide Society and John Wiley & Sons, Ltd.

  6. chemical shift tensors in helical peptides by dipolar-modulated chemical shift recoupling NMR

    International Nuclear Information System (INIS)

    Yao Xiaolan; Yamaguchi, Satoru; Hong Mei

    2002-01-01

    The Cα chemical shift tensors of proteins contain information on the backbone conformation. We have determined the magnitude and orientation of the Cα chemical shift tensors of two peptides with α-helical torsion angles: the Ala residue in G*AL (φ=-65.7 deg., ψ=-40 deg.), and the Val residue in GG*V (φ=-81.5 deg., ψ=-50.7 deg.). The magnitude of the tensors was determined from quasi-static powder patterns recoupled under magic-angle spinning, while the orientation of the tensors was extracted from Cα-Hα and Cα-N dipolar modulated powder patterns. The helical Ala Cα chemical shift tensor has a span of 36 ppm and an asymmetry parameter of 0.89. Its σ 11 axis is 116 deg. ± 5 deg. from the Cα-Hα bond while the σ 22 axis is 40 deg. ± 5 deg. from the Cα-N bond. The Val tensor has an anisotropic span of 25 ppm and an asymmetry parameter of 0.33, both much smaller than the values for β-sheet Val found recently (Yao and Hong, 2002). The Val σ 33 axis is tilted by 115 deg. ± 5 deg. from the Cα-Hα bond and 98 deg. ± 5 deg. from the Cα-N bond. These represent the first completely experimentally determined Cα chemical shift tensors of helical peptides. Using an icosahedral representation, we compared the experimental chemical shift tensors with quantum chemical calculations and found overall good agreement. These solid-state chemical shift tensors confirm the observation from cross-correlated relaxation experiments that the projection of the Cα chemical shift tensor onto the Cα-Hα bond is much smaller in α-helices than in β-sheets

  7. Enzymatic synthesis of tRNA-peptide conjugates and spectroscopic studies of fluorine-modified RNA

    International Nuclear Information System (INIS)

    Graber, D.

    2010-01-01

    The research presented in this thesis concerns the enzymatic synthesis of artificially modified tRNA, in particular the preparation of non-hydrolysable tRNA-peptide conjugates. Another focus is on NMR-spectroscopic investigations of fluorine-modified RNA. In both projects, chemical methods were developed to address specific RNA-biological research questions. In the first part of this thesis the preparation of tRNA-peptide conjugates with a non-hydrolysable 3'-amide linkage is presented. These molecules are of high relevance for the characterization of ribosomal processes that occur in the peptidyl transferase center (such as peptide bond formation, peptide release, or translocation) using X-ray crystallography and biochemical methods. First, a novel concept to prepare chemically modified ('labeled') tRNA was elaborated based on the combination of solid-phase synthesis and enzymatic ligation. Thereby, a variety of differently labeled tRNAs was achieved. Moreover, the most successful high-yield ligation sites were identified to be situated within the TΨ C-loop. Optimization of the synthesis and the corresponding HPLC-purification of the conjugates were initially conducted with puromycin derivatized tRNA. In the course of this project, also two tRNAs with a ribose 3'-amino group at the terminal adenosine A76 were synthesized. For that purpose a protection group pattern had to be developed to obtain a functionalized solid-support bound to 3'-amino-3'-deoxyadenosine which was appropriate for RNA solid-phase synthesis. The successful preparation of tRNA-peptide conjugates was accomplished in cooperation with Holger Moroder and Jessica Steger (Micura group) who contributed short synthetic RNA-peptide conjugates. These fragments represented the tRNA 3'-termini that were required for exploring the new ligation strategies for non-hydrolisable tRNA - a main aim of this thesis. If the 5'-fragments are synthesized by solid-phase synthesis or in vitro transcription they do not

  8. Synthesis of lucifensin by native chemical ligation and characteristics of its isomer having different disulfide bridge pattern

    Czech Academy of Sciences Publication Activity Database

    Stanchev, Stancho; Zawada, Zbigniew; Monincová, Lenka; Bednárová, Lucie; Slaninová, Jiřina; Fučík, Vladimír; Čeřovský, Václav

    2014-01-01

    Roč. 20, č. 9 (2014), s. 725-735 ISSN 1075-2617 Institutional support: RVO:61388963 Keywords : lucifensin * native chemical ligation * solid-phase peptide synthesis * antimicrobial activity * CD spectroscopy * DTT reduction Subject RIV: CE - Biochemistry Impact factor: 1.546, year: 2014

  9. Glutamic Acid Selective Chemical Cleavage of Peptide Bonds.

    Science.gov (United States)

    Nalbone, Joseph M; Lahankar, Neelam; Buissereth, Lyssa; Raj, Monika

    2016-03-04

    Site-specific hydrolysis of peptide bonds at glutamic acid under neutral aqueous conditions is reported. The method relies on the activation of the backbone amide chain at glutamic acid by the formation of a pyroglutamyl (pGlu) imide moiety. This activation increases the susceptibility of a peptide bond toward hydrolysis. The method is highly specific and demonstrates broad substrate scope including cleavage of various bioactive peptides with unnatural amino acid residues, which are unsuitable substrates for enzymatic hydrolysis.

  10. The self-assembly of redox active peptides: Synthesis and electrochemical capacitive behavior.

    Science.gov (United States)

    Piccoli, Julia P; Santos, Adriano; Santos-Filho, Norival A; Lorenzón, Esteban N; Cilli, Eduardo M; Bueno, Paulo R

    2016-05-01

    The present work reports on the synthesis of a redox-tagged peptide with self-assembling capability aiming applications in electrochemically active capacitive surfaces (associated with the presence of the redox centers) generally useful in electroanalytical applications. Peptide containing ferrocene (fc) molecular (redox) group (Ac-Cys-Ile-Ile-Lys(fc)-Ile-Ile-COOH) was thus synthesized by solid phase peptide synthesis (SPPS). To obtain the electrochemically active capacitive interface, the side chain of the cysteine was covalently bound to the gold electrode (sulfur group) and the side chain of Lys was used to attach the ferrocene in the peptide chain. After obtaining the purified redox-tagged peptide, the self-assembly and redox capability was characterized by cyclic voltammetry (CV) and electrochemical impedance-based capacitance spectroscopy techniques. The obtained results confirmed that the redox-tagged peptide was successfully attached by forming an electroactive self-assembled monolayer onto gold electrode. The design of redox active self-assembly ferrocene-tagged peptide is predictably useful in the development of biosensor devices precisely to detect, in a label-free platform, those biomarkers of clinical relevance. © 2016 Wiley Periodicals, Inc. Biopolymers (Pept Sci) 106: 357-367, 2016. © 2016 Wiley Periodicals, Inc.

  11. Plant natriuretic peptides control of synthesis and systemic effects

    KAUST Repository

    Wang, Yuhua; Donaldson, Lara Elizabeth; Gehring, Christoph A; Irving, Helen R.

    2011-01-01

    Plant natriuretic peptides (PNPs) are signaling molecules that are secreted into the apoplast particularly under conditions of biotic and abiotic stress. At the local level, PNPs modulate their own expression via feed forward and feedback loops

  12. Peptide Macrocycles Featuring a Backbone Secondary Amine: A Convenient Strategy for the Synthesis of Lipidated Cyclic and Bicyclic Peptides on Solid Support

    DEFF Research Database (Denmark)

    Oddo, Alberto; Münzker, Lena; Hansen, Paul Robert

    2015-01-01

    A convenient strategy for the on-resin synthesis of macrocyclic peptides (3- to 13-mers) via intramolecular halide substitution by a diamino acid is described. The method is compatible with standard Fmoc/tBu SPPS and affords a tail-to-side-chain macrocyclic peptide featuring an endocyclic secondary...

  13. Total synthesis, structure, and oral absorption of a thiazole cyclic peptide, sanguinamide A

    DEFF Research Database (Denmark)

    Nielsen, Daniel S; Hoang, Huy N; Lohman, Rink-Jan

    2012-01-01

    The first total synthesis and three-dimensional solution structure are reported for sanguinamide A, a thiazole-containing cyclic peptide from the sea slug H. sanguineus. Solution phase fragment synthesis, solid phase fragment assembly, and solution macrocyclization were combined to give (1) in 10......% yield. Spectral properties were identical for the natural product, requiring revision of its structure from (2) to (1). Intramolecular transannular hydrogen bonds help to bury polar atoms, which enables oral absorption from the gut....

  14. Solid-phase synthesis of head and tail bis-acridinylated peptides

    Czech Academy of Sciences Publication Activity Database

    Šebestík, Jaroslav; Matějka, P.; Hlaváček, Jan; Stibor, I.

    2004-01-01

    Roč. 45, č. 6 (2004), s. 1203-1205 ISSN 0040-4039 R&D Projects: GA ČR GA203/02/1379 Institutional research plan: CEZ:AV0Z4055905 Keywords : 9-amino acridine * solid phase synthesis * head and tail peptide conjugates Subject RIV: CC - Organic Chemistry Impact factor: 2.484, year: 2004

  15. Synthesis of water-soluble scaffolds for peptide cyclization, labeling, and ligation

    NARCIS (Netherlands)

    Smeenk, L.E.J.; Dailly, N.; Hiemstra, H.; van Maarseveen, J.H.; Timmerman, P.

    2012-01-01

    The synthesis and applications of water-soluble scaffolds that conformationally constrain side chain unprotected linear peptides containing two cysteines are described. These scaffolds contain a functionality with orthogonal reactivity to be used for labeling and ligation. This is illustrated by the

  16. Oxygenated base chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Roeper, M.

    1984-11-01

    Methyl formate, a syngas based intermediate, is already today produced on large scale by base catalyzed methanol carbonylation. An alternative synthesis, based on methanol dehydrogenation, seems to be ready for commercialization, whereas other routes including direct carbon monoxide hydrogenation, formaldehyde disproportionation or methanol oxydehydrogenation are less advanced. Besides being used as a solvent or an insect control agent, methyl formate serves as a feedstock for e.g. formic acid, formamide, N,N-dimethylformamide, and N-formyl morpholine. Newer formic acid processes are based on direct hydrolysis of methyl formate, and appear to replace the traditional indirect formamide based route. Future use of methyl formate could include the production of pure carbon monoxide, methanol, dimethyl carbonate, diphosgene, ethylene glycol via methyl glycolate, acetic acid, and methyl propionate. All these processes either avoid the use of high purity carbon monoxide or proceed under milder conditions than conventional routes. They could gain interest, if syngas and methanol become available at a large scale as competitive feedstocks for the chemical industry.

  17. Computational Chemical Synthesis Analysis and Pathway Design

    Directory of Open Access Journals (Sweden)

    Fan Feng

    2018-06-01

    Full Text Available With the idea of retrosynthetic analysis, which was raised in the 1960s, chemical synthesis analysis and pathway design have been transformed from a complex problem to a regular process of structural simplification. This review aims to summarize the developments of computer-assisted synthetic analysis and design in recent years, and how machine-learning algorithms contributed to them. LHASA system started the pioneering work of designing semi-empirical reaction modes in computers, with its following rule-based and network-searching work not only expanding the databases, but also building new approaches to indicating reaction rules. Programs like ARChem Route Designer replaced hand-coded reaction modes with automatically-extracted rules, and programs like Chematica changed traditional designing into network searching. Afterward, with the help of machine learning, two-step models which combine reaction rules and statistical methods became the main stream. Recently, fully data-driven learning methods using deep neural networks which even do not require any prior knowledge, were applied into this field. Up to now, however, these methods still cannot replace experienced human organic chemists due to their relatively low accuracies. Future new algorithms with the aid of powerful computational hardware will make this topic promising and with good prospects.

  18. Chemical reactor development : from laboratory synthesis to industrial production

    NARCIS (Netherlands)

    Thoenes, D.

    1998-01-01

    Chemical Reactor Development is written primarily for chemists and chemical engineers who are concerned with the development of a chemical synthesis from the laboratory bench scale, where the first successful experiments are performed, to the design desk, where the first commercial reactor is

  19. Recent Progress in Chemical and Chemoenzymatic Synthesis of Carbohydrates

    Science.gov (United States)

    Muthana, Saddam; Cao, Hongzhi; Chen, Xi

    2011-01-01

    Summary The important roles that carbohydrates play in biological processes and their potential application in diagnosis, therapeutics, and vaccine development have made them attractive synthetic targets. Despite ongoing challenges, tremendous progresses have been made in recent years for the synthesis of carbohydrates. The chemical glycosylation methods have become more sophisticated and the synthesis of oligosaccharides has become more predictable. Simplified one-pot glycosylation strategy and automated synthesis are increasingly used to obtain biologically important glycans. On the other hand, chemoenzymatic synthesis continues to be a powerful alternative for obtaining complex carbohydrates. This review highlights recent progress in chemical and chemoenzymatic synthesis of carbohydrates with a particular focus on the methods developed for the synthesis of oligosaccharides, polysaccharides, glycolipids, and glycosylated natural products. PMID:19833544

  20. Multi-line split DNA synthesis: a novel combinatorial method to make high quality peptide libraries

    Directory of Open Access Journals (Sweden)

    Ueno Shingo

    2004-09-01

    Full Text Available Abstract Background We developed a method to make a various high quality random peptide libraries for evolutionary protein engineering based on a combinatorial DNA synthesis. Results A split synthesis in codon units was performed with mixtures of bases optimally designed by using a Genetic Algorithm program. It required only standard DNA synthetic reagents and standard DNA synthesizers in three lines. This multi-line split DNA synthesis (MLSDS is simply realized by adding a mix-and-split process to normal DNA synthesis protocol. Superiority of MLSDS method over other methods was shown. We demonstrated the synthesis of oligonucleotide libraries with 1016 diversity, and the construction of a library with random sequence coding 120 amino acids containing few stop codons. Conclusions Owing to the flexibility of the MLSDS method, it will be able to design various "rational" libraries by using bioinformatics databases.

  1. Prebiotic Peptide (Amide) Bond Synthesis Accelerated by Glycerol and Bicarbonate Under Neutral to Alkaline Dry-Down Conditions

    Science.gov (United States)

    Forsythe, J. G.; Weber, A. L.

    2017-01-01

    Past studies of prebiotic peptide bond synthesis have generally been carried out in the acidic to neutral pH range [1, 2]. Here we report a new process for peptide bond (amide) synthesis in the neutral to alkaline pH range that involves simple dry-down heating of amino acids in the presence of glycerol and bicarbonate. Glycerol was included in the reaction mixture as a solvent and to provide hydroxyl groups for possible formation of ester intermediates previously implicated in peptide bond synthesis under acidic to neutral conditions [1]. Bicarbonate was added to raise the reaction pH to 8-9.

  2. Synthesis and in vitro evaluation of PNA-peptide-DETA conjugates as potential cell penetrating artificial ribonucleases.

    Science.gov (United States)

    Petersen, Lene; de Koning, Martijn C; van Kuik-Romeijn, Petra; Weterings, Jimmy; Pol, Christine J; Platenburg, Gerard; Overhand, Mark; van der Marel, Gijsbert A; van Boom, Jacques H

    2004-01-01

    We report the synthesis of novel artificial ribonucleases with potentially improved cellular uptake. The design of trifunctional conjugates 1a and 1b is based on the specific RNA-recognizing properties of PNA, the RNA-cleaving abilities of diethylenetriamine (DETA), and the peptide (KFF)(3)K for potential uptake into E. coli. The conjugates were assembled in a convergent synthetic route involving native chemical ligation of a PNA, containing an N-terminal cysteine, with the C-terminal thioester of the cell-penetrating (KFF)(3)K peptide to give 12a and 12b. These hybrids contained a free cysteine side-chain, which was further functionalized with an RNA-hydrolyzing diethylenetriamine (DETA) moiety. The trifunctional conjugates (1a, 1b) were evaluated for RNA-cleaving properties in vitro and showed efficient degradation of the target RNA at two major cleavage sites. It was also established that the cleavage efficiency strongly depended on the type of spacer connecting the PNA and the peptide.

  3. Plant natriuretic peptides control of synthesis and systemic effects

    KAUST Repository

    Wang, Yuhua

    2011-10-01

    Plant natriuretic peptides (PNPs) are signaling molecules that are secreted into the apoplast particularly under conditions of biotic and abiotic stress. At the local level, PNPs modulate their own expression via feed forward and feedback loops to enable tuning of the response at the transcript and protein level and to prevent overexpression. PNPs also employ a systemic signal, possibly electrical, to rapidly alter photosynthesis and respiration not only in treated leaves but also in upper and lower leaves thereby modulating and integrating physiological responses at the level of the whole plant. © 2011 Landes Bioscience.

  4. Synthesis and antioxidant activity of peptide-based ebselen analogues.

    Science.gov (United States)

    Satheeshkumar, Kandhan; Mugesh, Govindasamy

    2011-04-18

    A series of di- and tripeptide-based ebselen analogues has been synthesized. The compounds were characterized by (1)H, (13)C, and (77)Se NMR spectroscopy and mass spectral techniques. The glutathione peroxidase (GPx)-like antioxidant activity has been studied by using H(2)O(2) , tert-butyl hydroperoxide (tBuOOH), and cumene hydroperoxide (Cum-OOH) as substrates, and glutathione (GSH) as a cosubstrate. Although all the peptide-based compounds have a selenazole ring similar to that of ebselen, the GPx activity of these compounds highly depends on the nature of the peptide moiety attached to the nitrogen atom of the selenazole ring. It was observed that the introduction of a phenylalanine (Phe) amino acid residue in the N-terminal reduces the activity in all three peroxide systems. On the other hand, the introduction of aliphatic amino acid residues such as valine (Val) significantly enhances the GPx activity of the ebselen analogues. The difference in the catalytic activity of dipeptide-based ebselen derivatives can be ascribed mainly to the change in the reactivity of these compounds toward GSH and peroxide. Although the presence of the Val-Ala-CO(2) Me moiety facilitates the formation of a catalytically active selenol species, the reaction of ebselen analogues that has a Phe-Ile-CO(2) Me residue with GSH does not generate the corresponding selenol. To understand the antioxidant activity of the peptide-based ebselen analogues in the absence of GSH, these compounds were studied for their ability to inhibit peroxynitrite (PN)-mediated nitration of bovine serum albumin (BSA) and oxidation of dihydrorhodamine 123. In contrast to the GPx activity, the PN-scavenging activity of the Phe-based peptide analogues was found to be comparable to that of the Val-based compounds. However, the introduction of an additional Phe residue to the ebselen analogue that had a Val-Ala dipeptide significantly reduced the potency of the parent compound in PN-mediated nitration. Copyright

  5. Highly efficient synthetic method onpyroacm resin using the boc SPPS protocol for C-terminal cysteine peptide synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Juvekar, Vinayak; Kim, Kang Tae; Gong, Young Dae [Innovative Drug Library Research Center, Dept. of Chemistry, College of Science, Dongguk University, Seoul (Korea, Republic of)

    2017-01-15

    A very effective process on Pyroacm resin was developed for solid-phase peptide synthesis (SPPS) of C-terminal cysteine and cysteine ester peptides. The process uses cysteine side chain anchoring to the Pyroacm resin and the Boc protocol for SPPS. The Pyroacm resin showed remarkable stability under standard trifluoromethanesulfonic acid (TFMSA) cleavage condition. TFMSA cleavage of protecting groups generates a peptide-linked resin, which can be subjected to peptide modification reactions. Finally, the peptide can be cleaved from the resin using methoxycarbonylsulfenyl chloride. The utility of this protocol was demonstrated by its applications to the synthesis of model peptides, key intermediates in the preparation of natural products riparin 1.2 and a-factor.

  6. Importance of asparagine on the conformational stability and chemical reactivity of selected anti-inflammatory peptides

    Energy Technology Data Exchange (ETDEWEB)

    Soriano-Correa, Catalina, E-mail: csorico@comunidad.unam.mx [Química Computacional, Facultad de Estudios Superiores (FES)-Zaragoza, Universidad Nacional Autónoma de México (UNAM), Iztapalapa, C.P. 09230 México, D.F. (Mexico); Barrientos-Salcedo, Carolina [Laboratorio de Química Médica y Quimiogenómica, Facultad de Bioanálisis Campus Veracruz-Boca del Río, Universidad Veracruzana, C.P. 91700 Veracruz (Mexico); Campos-Fernández, Linda; Alvarado-Salazar, Andres [Química Computacional, Facultad de Estudios Superiores (FES)-Zaragoza, Universidad Nacional Autónoma de México (UNAM), Iztapalapa, C.P. 09230 México, D.F. (Mexico); Esquivel, Rodolfo O. [Departamento de Química, Universidad Autónoma Metropolitana-Iztapalapa (UAM-Iztapalapa), C.P. 09340 México, D.F. (Mexico)

    2015-08-18

    Highlights: • Asparagine plays an important role to anti-inflammatory effect of peptides. • The electron-donor substituent groups favor the formation of the hydrogen bonds, which contribute in the structural stability of peptides. • Chemical reactivity and the physicochemical features are crucial in the biological functions of peptides. - Abstract: Inflammatory response events are initiated by a complex series of molecular reactions that generate chemical intermediaries. The structure and properties of peptides and proteins are determined by the charge distribution of their side chains, which play an essential role in its electronic structure and physicochemical properties, hence on its biological functionality. The aim of this study was to analyze the effect of changing one central amino acid, such as substituting asparagine for aspartic acid, from Cys–Asn–Ser in aqueous solution, by assessing the conformational stability, physicochemical properties, chemical reactivity and their relationship with anti-inflammatory activity; employing quantum-chemical descriptors at the M06-2X/6-311+G(d,p) level. Our results suggest that asparagine plays a more critical role than aspartic acid in the structural stability, physicochemical features, and chemical reactivity of these tripeptides. Substituent groups in the side chain cause significant changes on the conformational stability and chemical reactivity, and consequently on their anti-inflammatory activity.

  7. Amino acid substrates impose polyamine, eIF5A, or hypusine requirement for peptide synthesis.

    Science.gov (United States)

    Shin, Byung-Sik; Katoh, Takayuki; Gutierrez, Erik; Kim, Joo-Ran; Suga, Hiroaki; Dever, Thomas E

    2017-08-21

    Whereas ribosomes efficiently catalyze peptide bond synthesis by most amino acids, the imino acid proline is a poor substrate for protein synthesis. Previous studies have shown that the translation factor eIF5A and its bacterial ortholog EF-P bind in the E site of the ribosome where they contact the peptidyl-tRNA in the P site and play a critical role in promoting the synthesis of polyproline peptides. Using misacylated Pro-tRNAPhe and Phe-tRNAPro, we show that the imino acid proline and not tRNAPro imposes the primary eIF5A requirement for polyproline synthesis. Though most proline analogs require eIF5A for efficient peptide synthesis, azetidine-2-caboxylic acid, a more flexible four-membered ring derivative of proline, shows relaxed eIF5A dependency, indicating that the structural rigidity of proline might contribute to the requirement for eIF5A. Finally, we examine the interplay between eIF5A and polyamines in promoting translation elongation. We show that eIF5A can obviate the polyamine requirement for general translation elongation, and that this activity is independent of the conserved hypusine modification on eIF5A. Thus, we propose that the body of eIF5A functionally substitutes for polyamines to promote general protein synthesis and that the hypusine modification on eIF5A is critically important for poor substrates like proline. Published by Oxford University Press on behalf of Nucleic Acids Research 2017.

  8. Customized Peptide Biomaterial Synthesis via an Environment-Reliant Auto-Programmer Stigmergic Approach

    Directory of Open Access Journals (Sweden)

    Ravindra V. Badhe

    2018-04-01

    Full Text Available Stigmergy, a form of self-organization, was employed here to engineer a self-organizing peptide capable of forming a nano- or micro-structure and that can potentially be used in various drug delivery and biomedical applications. These self-assembling peptides exhibit several desirable qualities for drug delivery, tissue engineering, cosmetics, antibiotics, food science, and biomedical surface engineering. In this study, peptide biomaterial synthesis was carried out using an environment-reliant auto-programmer stigmergic approach. A model protein, α-gliadin (31, 36, and 38 kD, was forced to attain a primary structure with free –SH groups and broken down enzymatically into smaller fragments using chymotrypsin. This breakdown was carried out at different environment conditions (37 and 50 °C, and the fragments were allowed to self-organize at these temperatures. The new peptides so formed diverged according to the environmental conditions. Interestingly, two peptides (with molecular weights of 13.8 and 11.8 kD were isolated when the reaction temperature was maintained at 50 °C, while four peptides with molecular weights of 54, 51, 13.8, and 12.8 kD were obtained when the reaction was conducted at 37 °C. Thus, at a higher temperature (50 °C, the peptides formed, compared to the original protein, had lower molecular weights, whereas, at a lower temperature (37 °C, two peptides had higher molecular weights and two had lower molecular weights.

  9. 2-Methyltetrahydrofuran and cyclopentyl methyl ether for green solid-phase peptide synthesis.

    Science.gov (United States)

    Jad, Yahya E; Acosta, Gerardo A; Khattab, Sherine N; de la Torre, Beatriz G; Govender, Thavendran; Kruger, Hendrik G; El-Faham, Ayman; Albericio, Fernando

    2016-02-01

    2-MeTHF and CPME were evaluated as greener alternatives for the most employed solvents in peptide synthesis. The ability of these solvents to dissolve amino acid derivatives and a range of coupling reagents were evaluated as well as the swelling of polystyrene and polyethylene glycol resins. In addition, racemization and coupling efficiencies were also determined. We concluded that the use of 2-MeTHF with combination of DIC/OxymaPure gave the lowest racemization level during stepwise synthesis of Z-Phg-Pro-NH2 and the highest purity during SPPS of Aib-enkephalin pentapeptide (H-Tyr-Aib-Aib-Phe-Leu-NH2).

  10. Hydroxyapatite, a biomaterial: Its chemical synthesis ...

    Indian Academy of Sciences (India)

    The surface area and particle size of HAP powder prepared by chemical precipitation route, were also ... chemical precipitation method (Jarcho 1978). The powders .... den snail shell, Helix aspersa, was done by taking tris-HCl buffer solution.

  11. C-peptide prevents SMAD3 binding to alpha promoters to inhibit collagen type IV synthesis.

    Science.gov (United States)

    Li, Yanning; Zhong, Yan; Gong, Wenjian; Gao, Xuehan; Qi, Huanli; Liu, Kun; Qi, Jinsheng

    2018-07-01

    Activation of transforming growth factor β1 (TGFB1)/SMAD3 signaling may lead to additional synthesis of collagen type IV (COL4), which is a major contributor to extracellular matrix (ECM) accumulation in diabetic nephropathy (DN). C-peptide can attenuate fibrosis to have unique beneficial effects in DN. However, whether and how C-peptide affects TGFB1/SMAD3-activated COL4 synthesis is unclear. In this study, pathological changes, expression of COL4 a1-a5 chains ( Col4a1-a5 ), COL4 distribution and protein and TGFB1 and SMAD3 protein were first assessed in a rat model of diabetes. Then, rat mesangial cells were treated with high glucose (HG) and/or C-peptide to investigate the underlying mechanism. Col4a1-a5 expression, COL4 protein and secretion, TGFB1 protein, SMAD3 nuclear translocation and binding of SMAD3 to its cognate sites in the promoters of Col4a1a2 , Col4a3a4 and Col4a5 were measured. It was found that C-peptide attenuated glomerular pathological changes and suppressed renal Col4a1 -a5 mRNA expression, COL4 protein content and TGFB1 protein content. C-peptide had a dose-dependent effect to inhibit Col4a1-a5 mRNA expression, COL4 protein content and secretion, in HG-stimulated mesangial cells. In addition, the HG-induced increase in TGFB1 protein content was significantly reduced by C-peptide. Although not apparently affecting SMAD3 nuclear translocation, C-peptide prevented SMAD3 from binding to its sites in the Col4a1a2 , Col4a3a4 and Col4a5 promoters in HG-stimulated mesangial cells. In conclusion, C-peptide could prevent SMAD3 from binding to its sites in the Col4a1a2 , Col4a3a4 and Col4a5 promoters, to inhibit COL4 generation. These results may provide a mechanism for the alleviation of fibrosis in DN by C-peptide. © 2018 Society for Endocrinology.

  12. Solid-Phase Synthesis of Difficult Purine-Rich PNAs through Selective Hmb Incorporation: Application to the Total Synthesis of Cell Penetrating Peptide-PNAs

    Directory of Open Access Journals (Sweden)

    Julien Tailhades

    2017-10-01

    Full Text Available Antisense oligonucleotide (ASO-based drug development is gaining significant momentum following the recent FDA approval of Eteplirsen (an ASO based on phosphorodiamidate morpholino and Spinraza (2′-O-methoxyethyl-phosphorothioate in late 2016. Their attractiveness is mainly due to the backbone modifications which have improved the in vivo characteristics of oligonucleotide drugs. Another class of ASO, based on peptide nucleic acid (PNA chemistry, is also gaining popularity as a platform for development of gene-specific therapy for various disorders. However, the chemical synthesis of long PNAs, which are more target-specific, remains an ongoing challenge. Most of the reported methodology for the solid-phase synthesis of PNA suffer from poor coupling efficiency which limits production to short PNA sequences of less than 15 residues. Here, we have studied the effect of backbone modifications with Hmb (2-hydroxy-4-methoxybenzyl and Dmb (2,4-dimethoxybenzyl to ameliorate difficult couplings and reduce “on-resin” aggregation. We firstly synthesized a library of PNA dimers incorporating either Hmb or Dmb and identified that Hmb is superior to Dmb in terms of its ease of removal. Subsequently, we used Hmb backbone modification to synthesize a 22-mer purine-rich PNA, targeting dystrophin RNA splicing, which could not be synthesized by standard coupling methodology. Hmb backbone modification allowed this difficult PNA to be synthesized as well as to be continued to include a cell-penetrating peptide on the same solid support. This approach provides a novel and straightforward strategy for facile solid-phase synthesis of difficult purine-rich PNA sequences.

  13. Solid-phase synthesis of difficult purine-rich PNAs through selective Hmb incorporation: Application to the total synthesis of cell penetrating peptide-PNAs

    Science.gov (United States)

    Tailhades, Julien; Takizawa, Hotake; Gait, Michael J.; Wellings, Don A.; Wade, John D.; Aoki, Yoshitsugu; Shabanpoor, Fazel

    2017-10-01

    Antisense oligonucleotide (ASO)-based drug development is gaining significant momentum following the recent FDA approval of Eteplirsen (an ASO based on phosphorodiamidate morpholino) and Spinraza (2’-O-methoxyethyl-phosphorothioate) in late 2016. Their attractiveness is mainly due to the backbone modifications which have improved the in vivo characteristics of oligonucleotide drugs. Another class of ASO, based on peptide nucleic acid (PNA) chemistry, is also gaining popularity as a platform for development of gene-specific therapy for various disorders. However, the chemical synthesis of long PNAs, which are more target-specific, remains an ongoing challenge. Most of the reported methodology for the solid-phase synthesis of PNA suffer from poor coupling efficiency which limits production to short PNA sequences of less than 15 residues. Here we have studied the effect of backbone modifications with Hmb (2-hydroxy-4-methoxybenzyl) and Dmb (2,4-dimethoxybenzyl) to ameliorate difficult couplings and reduce “on-resin” aggregation. We firstly synthesized a library of PNA dimers incorporating either Hmb or Dmb and identified that Hmb is superior to Dmb in terms of its ease of removal. Subsequently, we used Hmb backbone modification to synthesize a 22-mer purine-rich PNA, targeting dystrophin RNA splicing, which could not be synthesized by standard coupling methodology. Hmb backbone modification allowed this difficult PNA to be synthesized as well as to be continued to include a cell-penetrating peptide on the same solid support. This approach provides a novel and straightforward strategy for facile solid-phase synthesis of difficult purine-rich PNA sequences.

  14. Method for innovative synthesis-design of chemical process flowsheets

    DEFF Research Database (Denmark)

    Kumar Tula, Anjan; Gani, Rafiqul

    Chemical process synthesis-design involve the identification of the processing route to reach a desired product from a specified set of raw materials, design of the operations involved in the processing route, the calculations of utility requirements, the calculations of waste and emission...... to the surrounding and many more. Different methods (knowledge-based [1], mathematical programming [2], hybrid, etc.) have been proposed and are also currently employed to solve these synthesis-design problems. D’ Anterroches [3] proposed a group contribution based approach to solve the synthesis-design problem...... of chemical processes, where, chemical process flowsheets could be synthesized in the same way as atoms or groups of atoms are synthesized to form molecules in computer aided molecular design (CAMD) techniques [4]. That, from a library of building blocks (functional process-groups) and a set of rules to join...

  15. FACILITATED CHEMICAL SYNTHESIS UNDER ALTERNATE REACTION CONDITIONS

    Science.gov (United States)

    The chemical research in the late 1990's witnessed a paradigm shift towards "environmentally-friendly chemistry" more popularly known as "green chemistry" due to the increasing environmental concerns and legislative requirements to curb the release of chemical waste into the atmo...

  16. Synthesis of fluorescent analogues of relaxin family peptides and their preliminary in vitro and in vivo characterization

    Directory of Open Access Journals (Sweden)

    Linda eChan

    2013-12-01

    Full Text Available Relaxin, a heterodimeric polypeptide hormone, is a key regulator of collagen metabolism and multiple vascular control pathways in humans and rodents. Its actions are mediated via its cognate G-protein-coupled receptor, RXFP1 although it also ‘pharmacologically’ activates RXFP2, the receptor for the related, insulin-like peptide 3 (INSL3, which has specific actions on reproduction and bone metabolism. Therefore, experimental tools to facilitate insights into the distinct biological actions of relaxin and INSL3 are required, particularly for studies of tissues containing both RXFP1 and RXFP2. Here, we chemically functionalized human (H2 relaxin, the RXFP1-selective relaxin analogue H2:A(4-24(F23A, and INSL3 to accommodate a fluorophore without marked reduction in binding or activation propensity. Chemical synthesis of the two chains for each peptide was followed by sequential regioselective formation of their three disulfide bonds. Click chemistry conjugation of Cy5.5 at the B-chain N-terminus, with conservation of the disulfide bonds, yielded the analogues displaying appropriate selective binding affinity and ability to activate RXFP1 and/or RXFP2 in vitro. The in vivo biological activity of Cy5.5-H2 relaxin and Cy5.5-H2:A(4-24(F23A was confirmed in mice, as acute icv infusion of these peptides (but not Cy5.5-INSL3 stimulated water drinking, an established behavioral response elicited by central RXFP1 activation. The central distribution of Cy5.5-conjugated peptides was examined in mice killed 30 min after infusion, revealing fluorescence within brain tissue near-adjacent to the cerebral ventricle walls relative to deeper brain areas. These data will aid the interpretation of behavioral studies. Production of fluorophore-conjugated relaxin family peptides will facilitate future pharmacological studies to probe the function of H2 relaxin/RXFP1 and INSL3/RXFP2 signaling in vivo while tracking their distribution following central or peripheral

  17. One-pot synthesis of water soluble iron nanoparticles using rationally-designed peptides and ligand release.

    Science.gov (United States)

    Papst, Stefanie; Cheong, Soshan; Banholzer, Moritz J; Brimble, Margaret A; Williams, David E; Tilley, Richard D

    2013-05-18

    Herein we report the rational design of new phosphopeptides for control of nucleation, growth and aggregation of water-soluble, superparamagnetic iron-iron oxide core-shell nanoparticles. The use of the designed peptides enables a one-pot synthesis that avoids utilizing unstable or toxic iron precursors, organic solvents, and the need for exchange of capping agent after synthesis of the NPs.

  18. Iodinated derivatives of vasoactive intestinal peptide (VIP), PHI and PHM: purification, chemical characterization and biological activity

    International Nuclear Information System (INIS)

    McMaster, D.; Suzuki, Y.; Rorstad, O.; Lederis, K.

    1987-01-01

    The iodination of vasoactive intestinal peptide (VIP) was studied, using a variety of enzymatic and chemical iodination methods. Reversed phase high performance liquid chromatography (HPLC) was used to purify the reaction products. The lactoperoxidase-glucose oxidase method gave excellent results in terms of reproducibility, iodine incorporation, and yield of the non-oxidized products [Tyr(I)10]VIP and [Tyr(I)22]VIP, and was used to prepare both 125 I and 127 I labelled derivatives. In both cases, direct application to HPLC and a single column system were used. Although the oxidized peptides [Tyr(I)10,Met(O)17]VIP and [Tyr(I)22,Met(O)17]VIP could be generated to varying degrees directly by iodination of VIP, these were most conveniently prepared by iodination of [Met(O)17]VIP. Iodinated derivatives of the homologous peptides PHI and PHM were likewise prepared by rapid, one-step HPLC procedures. The site and degree of iodination were determined by HPLC peptide mapping of tryptic digests and amino acid analyses, and in the case of [Tyr(I)10]VIP also by sequencing. The vasorelaxant activities of the iodinated peptides in bovine cerebral artery preparations did not differ significantly from those of the corresponding noniodinated peptides, with the exception of [Tyr(I)10,Met(O)17]VIP and [Tyr(I)22,Met(O)17]VIP which, unlike [Met(O)17]VIP itself, had slightly lower potency than VIP

  19. Alzheimer's disease against peptides products of enzymatic cleavage APP protein: Biological, pathobiological and physico-chemical properties of fibrillating peptides.

    Science.gov (United States)

    Marszałek, Małgorzata

    2017-05-17

    Various peptides products of enzymatic cleavage of key for Alzheimer's disease Amyloid Precursor Protein (APP) are well known, but still are matter of scientific debate. The Aβ type products are especially challenging for experimental and medical research. This paper outlines several, still poorly known, biological and medical processes such as peptides biology, i.e., formation, biodistribution, translocation, transport and finally removal from brain compartments and body fluids like Intracellular Fluid (ICF), Cerebrospinal Fluid (CSF), Interstitial Fluid (ISF), blood serum or urine. In addition, the following studies concerning AD patients might prove challenging and simultaneously promising: peptides translocation through Blood-Brain - Barrier (BBB) and Blood-Cerebrospinal Fluid Barrier (BCSFB) and their removal from the brain according to a new concept of glymphatic system; - diagnostic difficulties that stem from physico-chemical properties and the nature of proteins or fibrillating peptides itself like low concentration, short half-live and from experimental-technical problems as well like high adsorption or low solubility of Aβ, tau or amylin. The study of diagnostic parameters is very important, as it may better reflect early changes before the disease develops; one such parameter is the Aβ42/Aβ40 ratio, or the ratio with the total tau concentration combination and other new biomarkers like Aβ1-38; other factors include oxidative stress and inflammation process proteins, complement factor H, alpha-2-macroglobulin, or clusterin. The study of various forms of pathological amyloid deposits that emerge in different but specific brain regions AD patients seems to be crucial as well. The composition of the first initial pathological, pre-fibrillating monomers of fibrillating peptides and their role in AD development and disease progression have been described as well. They are even more challenging for science and simultaneously might be more promising in

  20. Racemic & quasi-racemic protein crystallography enabled by chemical protein synthesis.

    Science.gov (United States)

    Kent, Stephen Bh

    2018-04-04

    A racemic protein mixture can be used to form centrosymmetric crystals for structure determination by X-ray diffraction. Both the unnatural d-protein and the corresponding natural l-protein are made by total chemical synthesis based on native chemical ligation-chemoselective condensation of unprotected synthetic peptide segments. Racemic protein crystallography is important for structure determination of the many natural protein molecules that are refractory to crystallization. Racemic mixtures facilitate the crystallization of recalcitrant proteins, and give diffraction-quality crystals. Quasi-racemic crystallization, using a single d-protein molecule, can facilitate the determination of the structures of a series of l-protein analog molecules. Copyright © 2018 Elsevier Ltd. All rights reserved.

  1. Ocean acidification affects marine chemical communication by changing structure and function of peptide signalling molecules.

    Science.gov (United States)

    Roggatz, Christina C; Lorch, Mark; Hardege, Jörg D; Benoit, David M

    2016-12-01

    Ocean acidification is a global challenge that faces marine organisms in the near future with a predicted rapid drop in pH of up to 0.4 units by the end of this century. Effects of the change in ocean carbon chemistry and pH on the development, growth and fitness of marine animals are well documented. Recent evidence also suggests that a range of chemically mediated behaviours and interactions in marine fish and invertebrates will be affected. Marine animals use chemical cues, for example, to detect predators, for settlement, homing and reproduction. But, while effects of high CO 2 conditions on these behaviours are described across many species, little is known about the underlying mechanisms, particularly in invertebrates. Here, we investigate the direct influence of future oceanic pH conditions on the structure and function of three peptide signalling molecules with an interdisciplinary combination of methods. NMR spectroscopy and quantum chemical calculations were used to assess the direct molecular influence of pH on the peptide cues, and we tested the functionality of the cues in different pH conditions using behavioural bioassays with shore crabs (Carcinus maenas) as a model system. We found that peptide signalling cues are susceptible to protonation in future pH conditions, which will alter their overall charge. We also show that structure and electrostatic properties important for receptor binding differ significantly between the peptide forms present today and the protonated signalling peptides likely to be dominating in future oceans. The bioassays suggest an impaired functionality of the signalling peptides at low pH. Physiological changes due to high CO 2 conditions were found to play a less significant role in influencing the investigated behaviour. From our results, we conclude that the change of charge, structure and consequently function of signalling molecules presents one possible mechanism to explain altered behaviour under future oceanic p

  2. Development of chemical process for synthesis of polyunsaturated esters

    OpenAIRE

    Vera LÃcia Viana do Nascimento

    2014-01-01

    This work aimed to develop refining processes, chemical alcoholysis followed by separation of fatty acids using the complexation with urea technique for the synthesis of poly-unsaturated esters from waste of fish oils. The special crude fish oil was purchased from Company Campestre - SÃo Paulo. Initially this oil has undergone a process of physical and chemical refining. From the refined oil, an alcoholysis process was carried out to obtain the mixture of free fatty acids. From the hydrolyzed...

  3. Graphene: chemical approaches to the synthesis and modification

    Energy Technology Data Exchange (ETDEWEB)

    Grayfer, E D; Makotchenko, V G; Nazarov, Albert S; Kim, S J; Fedorov, Vladimir E

    2011-08-31

    Published data on the new carbon nanomaterial, graphene, are described systematically from the chemist's standpoint. The attention is focused on the chemical methods of the synthesis of graphene-like materials from various precursors: natural and expanded graphite, graphite oxide, graphite intercalation compounds, etc. Approaches to the chemical modification of the graphene plane by various reagents and routes for the preparation of colloidal dispersions of graphene are considered. The bibliography includes 220 references.

  4. Origins of the Mechanochemical Coupling of Peptide Bond Formation to Protein Synthesis.

    Science.gov (United States)

    Fritch, Benjamin; Kosolapov, Andrey; Hudson, Phillip; Nissley, Daniel A; Woodcock, H Lee; Deutsch, Carol; O'Brien, Edward P

    2018-04-18

    Mechanical forces acting on the ribosome can alter the speed of protein synthesis, indicating that mechanochemistry can contribute to translation control of gene expression. The naturally occurring sources of these mechanical forces, the mechanism by which they are transmitted 10 nm to the ribosome's catalytic core, and how they influence peptide bond formation rates are largely unknown. Here, we identify a new source of mechanical force acting on the ribosome by using in situ experimental measurements of changes in nascent-chain extension in the exit tunnel in conjunction with all-atom and coarse-grained computer simulations. We demonstrate that when the number of residues composing a nascent chain increases, its unstructured segments outside the ribosome exit tunnel generate piconewtons of force that are fully transmitted to the ribosome's P-site. The route of force transmission is shown to be through the nascent polypetide's backbone, not through the wall of the ribosome's exit tunnel. Utilizing quantum mechanical calculations we find that a consequence of such a pulling force is to decrease the transition state free energy barrier to peptide bond formation, indicating that the elongation of a nascent chain can accelerate translation. Since nascent protein segments can start out as largely unfolded structural ensembles, these results suggest a pulling force is present during protein synthesis that can modulate translation speed. The mechanism of force transmission we have identified and its consequences for peptide bond formation should be relevant regardless of the source of the pulling force.

  5. On the synthesis of peptide imprinted polymers by a combined suspension-Epitope polymerization method

    International Nuclear Information System (INIS)

    Kotrotsiou, O.; Chaitidou, S.; Kiparissides, C.

    2009-01-01

    In the past, molecularly imprinted polymers (MIPs), prepared by free-radical bulk polymerization, have been used for the selective recognition of small biomolecules (i.e., amino acids and amino acid derivatives). Presently, there is a need for the synthesis of MIPs capable of recognizing larger biomolecules (i.e., peptides and proteins). Moreover, it is highly desirable the production of MIP microparticles with well-defined morphological characteristics (e.g., particle size distribution, porosity, etc.) via particulate polymerization techniques. In the present study, the synthesis of molecularly imprinted microparticles, produced via the suspension and inverse suspension polymerization methods, using the 'epitope approach', is reported. The hydrophobic (i.e., Boc-Trp-Trp-Trp) or hydrophilic (i.e., His-Phe) oligo-peptides were employed as template molecules. The potential of the combined suspension polymerization method with the 'epitope approach' for the production of MIP microparticles is demonstrated, as well as the specificity and selectivity characteristics of the MIP microparticles towards hydrophobic and hydrophilic oligo-peptides. The proposed method appears to be a very promising and efficient technique for separation of proteins.

  6. Prediction of Xaa-Pro peptide bond conformation from sequence and chemical shifts

    Energy Technology Data Exchange (ETDEWEB)

    Shen Yang; Bax, Ad, E-mail: bax@nih.go [National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Laboratory of Chemical Physics (United States)

    2010-03-15

    We present a program, named Promega, to predict the Xaa-Pro peptide bond conformation on the basis of backbone chemical shifts and the amino acid sequence. Using a chemical shift database of proteins of known structure together with the PDB-extracted amino acid preference of cis Xaa-Pro peptide bonds, a cis/trans probability score is calculated from the backbone and {sup 13}C{sup {beta}} chemical shifts of the proline and its neighboring residues. For an arbitrary number of input chemical shifts, which may include Pro-{sup 13}C{sup {gamma}}, Promega calculates the statistical probability that a Xaa-Pro peptide bond is cis. Besides its potential as a validation tool, Promega is particularly useful for studies of larger proteins where Pro-{sup 13}C{sup {gamma}} assignments can be challenging, and for on-going efforts to determine protein structures exclusively on the basis of backbone and {sup 13}C{sup {beta}} chemical shifts.

  7. An Efficient, Green Chemical Synthesis of the Malaria Drug ...

    African Journals Online (AJOL)

    Results : A green-chemical synthesis of piperaquine is described that proceeds in 92 – 93 % overall yield. ... Keywords: ACTs, Dihydroartemisinin Piperaquine, Dihydroartemisinin, Green Chemistry, Malaria, ..... Mathers CD, Ezzati M, Lopez AD. ... Medicines Programme [Homepage on the Internet]. Geneva ... An Alternative.

  8. Microwave Technology--Applications in Chemical Synthesis

    Science.gov (United States)

    Microwave heating, being specific and instantaneous, is unique and has found a place for expeditious chemical syntheses. Specifically, the solvent-free reactions are convenient to perform and have advantages over the conventional heating protocols as summarized in the previous se...

  9. Synthesis, characterization and inhibitory activities of (4-N3[3,5-3H]Phe10)PKI(6-22)amide and its precursors: photoaffinity labeling peptides for the active site of cyclic AMP-dependent protein kinase.

    Science.gov (United States)

    Katz, B M; Lundquist, L J; Walsh, D A; Glass, D B

    1989-06-01

    PKI(6-22)amide is a 17 residue peptide corresponding to the active portion of the heat-stable inhibitor of cAMP-dependent protein kinase. The peptide is a potent (Ki = 1.6 nM), competitive inhibitor of the enzyme. The photoreactive peptide analog (4-azidophenylalanine10)PKI(6-22)amide was synthesized in both its non-radiolabeled and tritiated forms by chemical modification of precursor peptides that were prepared by stepwise solid-phase synthesis. (4-Amino[3,5-3H]phenylalanine10)PKI(6-22)amide, the precursor for the radiolabeled arylazide peptide, was obtained by catalytic reduction of the corresponding peptide containing the 3,5-diiodo-4-aminophenylalanine residue at position 10. The purified PKI peptides were analyzed by HPLC, amino acid analysis, and u.v. spectra. In the dark, (4-azidophenylalanine10)PKI(6-22)amide inhibited the catalytic subunit of cAMP-dependent protein kinase with a Ki value of 2.8 nM. The photoreactivity of the arylazide peptide was demonstrated by time-dependent u.v. spectral changes on exposure to light. Photolysis of the catalytic subunit (4-azido[3,5-3H]phenylalanine10)PKI(6-22)amide complex resulted in specific covalent labeling of the enzyme. The data indicate that this peptide is a useful photoaffinity labeling reagent for the active site of the protein kinase.

  10. The assembly and properties of protobiological structures - The beginnings of cellular peptide synthesis

    Science.gov (United States)

    Fox, S. W.; Nakashima, T.

    1980-01-01

    New data indicate that lysine-rich proteinoids have the ability to catalyze the synthesis of peptide bonds from a variety of amino acids and ATP. This capacity is evident in aqueous solution, in suspension of phase-separated complexes of lysine-rich proteinoid with acidic proteinoids, and in suspension of phase-separated particles composed of lysine-rich proteinoids with polynucleotides. Since the proteinoid complexes can contain other catalytic activities, including ability to catalyze internucleotide bond formation, it is inferred that the first protocells on earth already had a number of biological types of activity.

  11. Peptide Synthesis Method and Solid Support for Use in the Method

    DEFF Research Database (Denmark)

    1994-01-01

    A method for the solid-phase synthesis of peptides or proteins in high yield and high purity uses a solid support consisting of a functionalized polystyrene-grafted polymer substrate, the grafted polystyrene chains being substantially non-cross-linked and having a chain molecular weight, not incl...... is immersed in a solution of optionally substituted styrene monomer in an alcohol such as methanol, the volume percentage of styrene in the solution preferably being about 30% v/v, and subjected to gamma irradiation....

  12. Surface chemical immobilization of bioactive peptides on synthetic polymers for cardiac tissue engineering.

    Science.gov (United States)

    Rosellini, Elisabetta; Cristallini, Caterina; Guerra, Giulio D; Barbani, Niccoletta

    2015-01-01

    The aim of this work was the development of new synthetic polymeric systems, functionalized by surface chemical modification with bioactive peptides, for myocardial tissue engineering. Polycaprolactone and a poly(ester-ether-ester) block copolymer synthesized in our lab, polycaprolactone-poly(ethylene oxide)-polycaprolactone (PCL-PEO-PCL), were used as the substrates to be modified. Two pentapeptides, H-Gly-Arg-Gly-Asp-Ser-OH (GRGDS) from fibronectin and H-Tyr-Ile-Gly-Ser-Arg-OH (YIGSR) from laminin, were used for the functionalization. Polymeric membranes were obtained by casting from solutions and then functionalized by means of alkaline hydrolysis and subsequent coupling of the bioactive molecules through 1-(3-dimethylaminopropyl)-3-ethylcarbodimide hydrochloride/N-hydroxysuccinimide chemistry. The hydrolysis conditions, in terms of hydrolysis time, temperature, and sodium hydroxide concentration, were optimized for the two materials. The occurrence of the coupling reaction was demonstrated by infrared spectroscopy, as the presence on the functionalized materials of the absorption peaks typical of the two peptides. The peptide surface density was determined by chromatographic analysis and the distribution was studied by infrared chemical imaging. The results showed a nearly homogeneous peptide distribution, with a density above the minimum value necessary to promote cell adhesion. Preliminary in vitro cell culture studies demonstrated that the introduction of the bioactive molecules had a positive effect on improving C2C12 myoblasts growth on the synthetic materials.

  13. Chemical construction and structural permutation of potent cytotoxin polytheonamide B: discovery of artificial peptides with distinct functions.

    Science.gov (United States)

    Itoh, Hiroaki; Inoue, Masayuki

    2013-07-16

    Polytheonamide B (1), isolated from the marine sponge Theonella swinhoei, is a posttranslationally modified ribosomal peptide (MW 5030 Da) that displays extraordinary cytotoxicity. Among its 48 amino acid residues, this peptide includes a variety D- and L-amino acids that do not occur in proteins, and the chiralities of these amino acids alternate in sequence. These structural features induce the formation of a stable β6.3-helix, giving rise to a tubular structure of over 4 nm in length. In the biological setting, this fold is believed to transport cations across the lipid bilayer through a pore, thereby acting as an ion channel. In this Account, we discuss the construction and structural permutations of this potent cytotoxin. First we describe the 161-step chemical construction of this unusual peptide 1. By developing a synthetic route to 1, we established the chemical basis for subsequent SAR studies to pinpoint the proteinogenic and nonproteinogenic building blocks within the molecule that confer its toxicity and channel function. Using fully synthetic 1, we generated seven analogues with point mutations, and studies of their activity revealed the importance of the N-terminal moiety. Next, we simplified the structure of 1 by substituting six amino acid residues of 1 to design a more synthetically accessible analogue 9. This dansylated polytheonamide mimic 9 was synthesized in 127 total steps, and we evaluated its function to show that it can emulate the toxic and ion channel activities of 1 despite its multiple structural modifications. Finally, we applied a highly automated synthetic route to 48-mer 9 to generate 13 substructures of 27-39-mers. The 37-mer 12 exhibited nanomolar level toxicity through a potentially distinct mode of action from 1 and 9. The SAR studies of polytheonamide B and the 21 artificial analogues have deepened our understanding of the precise structural requirements for the biological functions of 1. They have also led to the discovery of

  14. Peptide Based Targeted Therapeutic Radiopharmaceuticals: A Focus on the Synthesis of Radiolabelled Nanobodies

    International Nuclear Information System (INIS)

    Impens, N.; Campsteyn, A.; Aerts, A.; Baatout, S.; Devoogdt, N.; Caveliers, V.; Xavier, C.; Lahoutte, T.

    2009-01-01

    In 1993, the Vrije Universiteit Brussel (Brussels, Belgium) discovered in the blood of camelidae antibodies consisting of only a heavy chain. Due to the lack of the light chain only the variable part of the heavy chain is important for antigen binding. This variable part of these heavy-chain-only antibodies is a good candidate as a targeted therapeutic radiopharmaceutical and was called a nanobody, having a molecular weight of about 15 kDa. Its dimensions are included in between the small peptides like derived from e.g. somatostatin, and the classical monoclonal antibodies. This makes that some characteristics like the physical behaviour, the chemical stability, the penetration in tumour and in healthy tissues, and the blood clearance lie in between the characteristics of the small peptides and the monoclonal antibodies, therefore taking advantage of both extremes. Nanobodies have been humanised to decrease the immunogenic response. The building blocks of molecules such as the octreotide, nanobodies and monoclonal antibodies are amino acids linked via peptide bonds. The modification reactions are therefore all based on the same 'peptide chemistry'. The functional groups on the present amino acids will determine the possible reactions. In order to link a radionuclide to the nanobodies, we opted to use bifunctional ligands containing DOTA, because this is a suitable chelating agent for the diagnostic radionuclide Ga-68, and for therapeutic radionuclides such as Lu-177 and Y-90, covering short and long range β-particle emitters suitable for attacking a wide range of tumour sizes. The ratio of bifunctional ligand to nanobody can be varied by carefully selecting the functional groups of the peptide involved in the reaction with the bifunctional ligand, avoiding the complementarity determining region (CDR), i.e. the part of the molecule binding to the antigen. This is a first way to predetermine the amount of radionuclides that can be linked to the peptide, or the

  15. Chiral thiazoline and thiazole building blocks for the synthesis of peptide-derived natural products.

    Science.gov (United States)

    Just-Baringo, Xavier; Albericio, Fernando; Alvarez, Mercedes

    2014-01-01

    Thiazoline and thiazole heterocycles are privileged motifs found in numerous peptide-derived natural products of biological interest. During the last decades, the synthesis of optically pure building blocks has been addressed by numerous groups, which have developed a plethora of strategies to that end. Efficient and reliable methodologies that are compatible with the intricate and capricious architectures of natural products are a must to further develop their science. Structure confirmation, structure-activity relationship studies and industrial production are fields of paramount importance that require these robust methodologies in order to successfully bring natural products into the clinic. Today's chemist toolbox is assorted with many powerful methods for chiral thiazoline and thiazole synthesis. Ranging from biomimetic approaches to stereoselective alkylations, one is likely to find a suitable method for their needs.

  16. Synthesis of peptide thioacids at neutral pH using bis(2-sulfanylethyl)amido peptide precursors.

    Science.gov (United States)

    Pira, Silvain L; Boll, Emmanuelle; Melnyk, Oleg

    2013-10-18

    Reaction of bis(2-sulfanylethyl)amido (SEA) peptides with triisopropylsilylthiol in water at neutral pH yields peptide thiocarboxylates. An alkylthioester derived from β-alanine was used to trap the released bis(2-sulfanylethyl)amine and displace the equilibrium toward the peptide thiocarboxylate.

  17. Alternative fuels and chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-12-01

    A DOE/PETC funded study was conducted to examine the use of a liquid phase mixed alcohol synthesis (LPMAS) plant to produce gasoline blending ethers. The LPMAS plant was integrated into three utilization scenarios: a coal fed IGCC power plant, a petroleum refinery using coke as a gasification feedstock, and a standalone natural gas fed partial oxidation plant. The objective of the study was to establish targets for the development of catalysts for the LPMAS reaction. In the IGCC scenario, syngas conversions need only be moderate because unconverted syngas is utilized by the combined cycle system. A once through LPMAS plant achieving syngas conversions in the range of 38--49% was found to be suitable. At a gas hourly space velocity of 5,000 sL/Kg-hr and a methanol:isobutanol selectivity ratio of 1.03, the target catalyst productivity ranges from 370 to 460 g iBuOH/Kg-hr. In the petroleum refinery scenario, high conversions ({approximately}95%) are required to avoid overloading the refinery fuel system with low Btu content unconverted syngas. To achieve these high conversions with the low H{sub 2}/CO ratio syngas, a recycle system was required (because of the limit imposed by methanol equilibrium), steam was injected into the LPMAS reactor, and CO{sub 2} was removed from the recycle loop. At the most economical recycle ratio, the target catalyst productivity is 265 g iBuOH/Kg-hr. In the standalone LPMAS scenario, essentially complete conversions are required to achieve a fuel balanced plant. At the most economical recycle ratio, the target catalyst productivity is 285 g iBuOH/Kg-hr. The economics of this scenario are highly dependent on the cost of the natural gas feedstock and the location of the plant. For all three case scenarios, the economics of a LPMAS plant is marginal at current ether market prices. Large improvements over demonstrated catalyst productivity and alcohol selectivity are required.

  18. Hexagonal ferrite powder synthesis using chemical coprecipitation

    International Nuclear Information System (INIS)

    Hsiang, H.-I; Yao, R.-Q.

    2007-01-01

    The formation mechanism of 3BaO.2CoO.12Fe 2 O 3 (Co 2 Z), 2BaO.2CoO.6Fe 2 O 3 (Co 2 Y) and BaO.6Fe 2 O 3 (BaM) powders were prepared using chemical coprecipitation methods in this study using X-ray diffraction (XRD), thermo-gravimetry (TG), differential thermal analysis (DTA) and Fourier transform infrared spectroscopy (FTIR). It was found that the BaM phase was formed directly through the reaction of the preceding ε-Fe 2 O 3 and amorphous BaCO 3 for BaM precursor. For the Co 2 Y precursor, the intermediate phase, BaM, was obtained through the reaction of the earlier formed BaFe 2 O 4 and α-Fe 2 O 3 . The Co 2 Y phase was obtained through a BaM and BaFe 2 O 4 reaction. However, for the Co 2 Z precursors, the BaM phase was obtained directly from the BaCO 3 and amorphous iron hydroxide reaction, with no α-Fe 2 O 3 and BaFe 2 O 4 formed as intermediates. Co 2 Z phase was obtained through the reaction of the two previous formed BaM and Co 2 Y phases

  19. Chemical synthesis and structure elucidation of bovine κ-casein (1-44)

    International Nuclear Information System (INIS)

    Bansal, Paramjit S.; Grieve, Paul A.; Marschke, Ronald J.; Daly, Norelle L.; McGhie, Emily; Craik, David J.; Alewood, Paul F.

    2006-01-01

    The caseins (α s1 , α s2 , β, and κ) are phosphoproteins present in bovine milk that have been studied for over a century and whose structures remain obscure. Here we describe the chemical synthesis and structure elucidation of the N-terminal segment (1-44) of bovine κ-casein, the protein which maintains the micellar structure of the caseins. κ-Casein (1-44) was synthesised by highly optimised Boc solid-phase peptide chemistry and characterised by mass spectrometry. Structure elucidation was carried out by circular dichroism and nuclear magnetic resonance spectroscopy. CD analysis demonstrated that the segment was ill defined in aqueous medium but in 30% trifluoroethanol it exhibited considerable helical structure. Further, NMR analysis showed the presence of a helical segment containing 26 residues which extends from Pro 8 to Arg 34 . This is First report which demonstrates extensive secondary structure within the casein class of proteins

  20. Chemical Synthesis of the 20 kDa Heme Protein Nitrophorin 4 by α-Ketoacid-Hydroxylamine (KAHA) Ligation.

    Science.gov (United States)

    He, Chunmao; Kulkarni, Sameer S; Thuaud, Frédéric; Bode, Jeffrey W

    2015-10-26

    The chemical synthesis of the 184-residue ferric heme-binding protein nitrophorin 4 was accomplished by sequential couplings of five unprotected peptide segments using α-ketoacid-hydroxylamine (KAHA) ligation reactions. The fully assembled protein was folded to its native structure and coordinated to the ferric heme b cofactor. The synthetic holoprotein, despite four homoserine residues at the ligation sites, showed identical properties to the wild-type protein in nitric oxide binding and nitrite dismutase reactivity. This work establishes the KAHA ligation as a valuable and viable approach for the chemical synthesis of proteins up to 20 kDa and demonstrates that it is well-suited for the preparation of hydrophobic protein targets. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Control of peptide nanotube diameter by chemical modifications of an aromatic residue involved in a single close contact

    Science.gov (United States)

    Tarabout, Christophe; Roux, Stéphane; Gobeaux, Frédéric; Fay, Nicolas; Pouget, Emilie; Meriadec, Cristelle; Ligeti, Melinda; Thomas, Daniel; IJsselstijn, Maarten; Besselievre, François; Buisson, David-Alexandre; Verbavatz, Jean-Marc; Petitjean, Michel; Valéry, Céline; Perrin, Lionel; Rousseau, Bernard; Artzner, Franck; Paternostre, Maité; Cintrat, Jean-Christophe

    2011-01-01

    Supramolecular self-assembly is an attractive pathway for bottom-up synthesis of novel nanomaterials. In particular, this approach allows the spontaneous formation of structures of well-defined shapes and monodisperse characteristic sizes. Because nanotechnology mainly relies on size-dependent physical phenomena, the control of monodispersity is required, but the possibility of tuning the size is also essential. For self-assembling systems, shape, size, and monodispersity are mainly settled by the chemical structure of the building block. Attempts to change the size notably by chemical modification usually end up with the loss of self-assembly. Here, we generated a library of 17 peptides forming nanotubes of monodisperse diameter ranging from 10 to 36 nm. A structural model taking into account close contacts explains how a modification of a few Å of a single aromatic residue induces a fourfold increase in nanotube diameter. The application of such a strategy is demonstrated by the formation of silica nanotubes of various diameters. PMID:21518895

  2. Aligator: A computational tool for optimizing total chemical synthesis of large proteins.

    Science.gov (United States)

    Jacobsen, Michael T; Erickson, Patrick W; Kay, Michael S

    2017-09-15

    The scope of chemical protein synthesis (CPS) continues to expand, driven primarily by advances in chemical ligation tools (e.g., reversible solubilizing groups and novel ligation chemistries). However, the design of an optimal synthesis route can be an arduous and fickle task due to the large number of theoretically possible, and in many cases problematic, synthetic strategies. In this perspective, we highlight recent CPS tool advances and then introduce a new and easy-to-use program, Aligator (Automated Ligator), for analyzing and designing the most efficient strategies for constructing large targets using CPS. As a model set, we selected the E. coli ribosomal proteins and associated factors for computational analysis. Aligator systematically scores and ranks all feasible synthetic strategies for a particular CPS target. The Aligator script methodically evaluates potential peptide segments for a target using a scoring function that includes solubility, ligation site quality, segment lengths, and number of ligations to provide a ranked list of potential synthetic strategies. We demonstrate the utility of Aligator by analyzing three recent CPS projects from our lab: TNFα (157 aa), GroES (97 aa), and DapA (312 aa). As the limits of CPS are extended, we expect that computational tools will play an increasingly important role in the efficient execution of ambitious CPS projects such as production of a mirror-image ribosome. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Temperature lowering in cryogenic chemical-synthesis techniques and system

    International Nuclear Information System (INIS)

    Martinez, H.E.; Nelson, T.O.; Vikdal, L.N.

    1993-01-01

    When evaluating a chemical synthesis process for a reaction that occurs on the cryogenically cooled walls, it is sometimes necessary to reduce the wall temperatures to enhance the chemical process. To evaluate the chemical process at lower than atmospheric boiling of liquid nitrogen, we built a system and used it to reduce the temperature of the liquid nitrogen. The technique of lowering the liquid nitrogen temperature by reducing the pressure of the boil-off is established knowledge. This paper presents the engineering aspects of the system, design features, equipment requirements, methods of control, and results of the chemical synthesis. The heat input to the system was ∼400 watts, placing a relatively large demand on the pumping system. Our system is a scale-up of the small laboratory experiment, and it provides the information needed to design an effective system. The major problem encountered was the large quantity of liquid escaping the system during the processing, placing a large gas load on the vacuum system

  4. Conserved Binding Regions Provide the Clue for Peptide-Based Vaccine Development: A Chemical Perspective

    Directory of Open Access Journals (Sweden)

    Hernando Curtidor

    2017-12-01

    Full Text Available Synthetic peptides have become invaluable biomedical research and medicinal chemistry tools for studying functional roles, i.e., binding or proteolytic activity, naturally-occurring regions’ immunogenicity in proteins and developing therapeutic agents and vaccines. Synthetic peptides can mimic protein sites; their structure and function can be easily modulated by specific amino acid replacement. They have major advantages, i.e., they are cheap, easily-produced and chemically stable, lack infectious and secondary adverse reactions and can induce immune responses via T- and B-cell epitopes. Our group has previously shown that using synthetic peptides and adopting a functional approach has led to identifying Plasmodium falciparum conserved regions binding to host cells. Conserved high activity binding peptides’ (cHABPs physicochemical, structural and immunological characteristics have been taken into account for properly modifying and converting them into highly immunogenic, protection-inducing peptides (mHABPs in the experimental Aotus monkey model. This article describes stereo–electron and topochemical characteristics regarding major histocompatibility complex (MHC-mHABP-T-cell receptor (TCR complex formation. Some mHABPs in this complex inducing long-lasting, protective immunity have been named immune protection-inducing protein structures (IMPIPS, forming the subunit components in chemically synthesized vaccines. This manuscript summarizes this particular field and adds our recent findings concerning intramolecular interactions (H-bonds or π-interactions enabling proper IMPIPS structure as well as the peripheral flanking residues (PFR to stabilize the MHCII-IMPIPS-TCR interaction, aimed at inducing long-lasting, protective immunological memory.

  5. Prebiotic Peptide (Amide) Bond Synthesis Accelerated by Glycerol and Bicarbonate Under Neutral to Alkaline Dry-Down Conditions

    Science.gov (United States)

    Forsythe, J. G.; Weber, A. L.

    2017-07-01

    We report a new process for robust peptide bond synthesis in the pH 6–10 range that involves dry-down heating of amino acids in the presence of glycerol and bicarbonate (substrates: L-alanine, L-2-aminobutyric acid, β-alanine, isoserine).

  6. Chemical synthesis, 3D structure, and ASIC binding site of the toxin mambalgin-2.

    Science.gov (United States)

    Schroeder, Christina I; Rash, Lachlan D; Vila-Farrés, Xavier; Rosengren, K Johan; Mobli, Mehdi; King, Glenn F; Alewood, Paul F; Craik, David J; Durek, Thomas

    2014-01-20

    Mambalgins are a novel class of snake venom components that exert potent analgesic effects mediated through the inhibition of acid-sensing ion channels (ASICs). The 57-residue polypeptide mambalgin-2 (Ma-2) was synthesized by using a combination of solid-phase peptide synthesis and native chemical ligation. The structure of the synthetic toxin, determined using homonuclear NMR, revealed an unusual three-finger toxin fold reminiscent of functionally unrelated snake toxins. Electrophysiological analysis of Ma-2 on wild-type and mutant ASIC1a receptors allowed us to identify α-helix 5, which borders on the functionally critical acidic pocket of the channel, as a major part of the Ma-2 binding site. This region is also crucial for the interaction of ASIC1a with the spider toxin PcTx1, thus suggesting that the binding sites for these toxins substantially overlap. This work lays the foundation for structure-activity relationship (SAR) studies and further development of this promising analgesic peptide. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Summarization on the synthesis and radionuclide-labeling of peptide nucleic acid for an oligonucleotide analogue

    International Nuclear Information System (INIS)

    Song, Hongtao; Zhang, Huaming; Gao, Hui

    2009-04-01

    Peptide nucleic acid (PNA), which is one kind of antisense nucleic acid compounds and an oligonucleotide analogue that binds strongly to DNA and RNA in a sequence specific manner, has its unique advantages in the field of molecular diagnostics and treatment of diseases. Now, people gradually attach more importance to PNA. To optimize the application of PNA in genetic re- search and therapy, a great number of backbone modifications on the newly- type structures of PNA were synthesized to improve its physicochemical proper- ties, such as hybridization speciality, solubility in biofluid, or cell permeability. The modified PNA labeled with radionuclides, which can obtain the aim at specific target and minimal non-target trauma, has important role in research and application of tumorous genitherapy. Here a review on the basic synthesis idea and several primary synthetic methods of PNA analogs was given, and also correlative studies and expectation on the compounds belonging to PNA series labeled with radionuclides were included. (authors)

  8. Synthesis and Radiolabeling of Modified Peptides Attached to Heterocyclic Rings and Their Possible Medical Applications

    International Nuclear Information System (INIS)

    Shams El-Din, H.A.A.

    2012-01-01

    Keeping in mind the pharmacological potential of heterocyclic rings as well as the advantage of biodegradability and biocompatibility of amino acids/peptides, in this thesis we were prompted for the following: 1. Synthesis of novel dipeptide derivatives coupled with different heterocyclic rings (pyridine, 1,2,4-triazol-pyridine, 1,3,4-oxadiazolpyridine and tetrazol-pyridine rings). 2. Characterization of the synthesized compounds on the basis of their spectral data (IR, Mass and 1 H-NMR spectra). 3. Study their antimicrobial activity as one of their expected biological activities. 4. Study the radioiodination of some synthesized dipeptide derivatives. 5. Study the biodistribution of the radiolabeled compounds in normal mice as preliminary studies for the possibility of using them as agents for imaging and treatment.

  9. Synthesis, Characterization and Biological Studies of 99mTc and 188Re Peptides

    Science.gov (United States)

    Sanders, Vanessa

    have the possible application to simplify the synthesis of the pharmaceutical. The versatility of the oxidation states of these metals leads to numerous possibilities in developing new radiopharmaceuticals. The coordination chemistry and reaction mechanisms must be efficiently characterized to ensure the reproducibility of the radiopharmaceutical. The current study focuses on technetium and rhenium complexes with peptides. These complexes have become increasing interesting for their use in diagnostic and therapeutic radiopharmaceuticals. The characterization of the complexation of Tc(V), and Rh(V) with the pentapeptide KYCAR (lysyl-tyrosyl-cystyl-alanyl-arginine) will be discussed. Complexes will be characterized by High Performance Liquid Chromatography (HPLC), UV-Visible Spectroscopy, Proton NMR, Circular Dichroism (CD), and Electrospray Ionization Mass Spectroscopy, to compare them to current radiopharmaceuticals. Information on the underlying reactions and coordination will be discussed.

  10. Oostatic peptides containing d-amino acids: synthesis, oostatic activity, degradation, accumulation in ovaries and NMR study

    Czech Academy of Sciences Publication Activity Database

    Hlaváček, Jan; Tykva, Richard; Holík, Josef; Bennettová, Blanka; Buděšínský, Miloš; Vlasáková, Věra; Černý, Bohuslav; Slaninová, Jiřina

    2012-01-01

    Roč. 42, č. 5 (2012), s. 1715-1725 ISSN 0939-4451 R&D Projects: GA ČR GA203/06/1272 Institutional research plan: CEZ:AV0Z40550506; CEZ:AV0Z50380511; CEZ:AV0Z50070508 Keywords : D-amino acids * oostatic peptide synthesis * H-3 labeling * oostatic activity in Neobellieria bullata * H-3 incorporation * Peptide degradation * NMR study Subject RIV: CC - Organic Chemistry Impact factor: 3.914, year: 2012

  11. Comparative syntheses of peptides and peptide thioesters derived from mouse and human prion proteins

    Czech Academy of Sciences Publication Activity Database

    Šebestík, Jaroslav; Zawada, Zbigniew; Šafařík, Martin; Hlaváček, Jan

    2012-01-01

    Roč. 43, č. 3 (2012), s. 1297-1309 ISSN 0939-4451 R&D Projects: GA ČR GA203/07/1517 Institutional research plan: CEZ:AV0Z40550506 Keywords : prion protein segments * classical synthesis * chemical ligation synthesis * peptide thioesters Subject RIV: CC - Organic Chemistry Impact factor: 3.914, year: 2012

  12. Design, synthesis, and actions of a novel chimeric natriuretic peptide: CD-NP.

    Science.gov (United States)

    Lisy, Ondrej; Huntley, Brenda K; McCormick, Daniel J; Kurlansky, Paul A; Burnett, John C

    2008-07-01

    Our aim was to design, synthesize and test in vivo and in vitro a new chimeric peptide that would combine the beneficial properties of 2 distinct natriuretic peptides with a biological profile that goes beyond native peptides. Studies have established the beneficial vascular and antiproliferative properties of C-type natriuretic peptide (CNP). While lacking renal actions, CNP is less hypotensive than the cardiac peptides atrial natriuretic peptide and B-type natriuretic peptide but unloads the heart due to venodilation. Dendroaspis natriuretic peptide is a potent natriuretic and diuretic peptide that is markedly hypotensive and functions via a separate guanylyl cyclase receptor compared with CNP. Here we engineered a novel chimeric peptide CD-NP that represents the fusion of the 22-amino acid peptide CNP together with the 15-amino acid linear C-terminus of Dendroaspis natriuretic peptide. We also determined in vitro in cardiac fibroblasts cyclic guanosine monophosphate-activating and antiproliferative properties of CD-NP. Our studies demonstrate in vivo that CD-NP is natriuretic and diuretic, glomerular filtration rate enhancing, cardiac unloading, and renin inhibiting. CD-NP also demonstrates less hypotensive properties when compared with B-type natriuretic peptide. In addition, CD-NP in vitro activates cyclic guanosine monophosphate and inhibits cardiac fibroblast proliferation. The current findings advance an innovative design strategy in natriuretic peptide drug discovery and development to create therapeutic peptides with favorable properties that may be preferable to those associated with native natriuretic peptides.

  13. Nanobiostructure of fibrous-like alumina functionalized with an analog of the BP100 peptide: Synthesis, characterization and biological applications.

    Science.gov (United States)

    Torres, L M F C; Braga, N A; Gomes, I P; Almeida, M T; Santos, T L; de Mesquita, J P; da Silva, L M; Martins, H R; Kato, K C; Dos Santos, W T P; Resende, J M; Pereira, M C; Bemquerer, M P; Rodrigues, M A; Verly, R M

    2018-03-01

    The functionalization of alumina nanoparticles of specific morphology with antimicrobial peptides (AMP) can be a promising strategy for modeling medical devices and packaging materials for cosmetics, medicines or food, since the contamination by pathogens could be reduced. In this paper, we show the synthesis of a fibrous-like alumina nanobiostructure, as well as its functionalization with the peptide EAAA-BP100, an analog of the antimicrobial peptide BP100. The antibacterial activity of the obtained material against some bacterial strains is also investigated. The covalent binding of the peptide to the nanoparticles was promoted by a reaction between the carboxyl group of the glutamate side chain (E1) of the peptide and the amino groups of the alumina nanoparticles, previously modified by reaction with 3-aminopropyltrietoxysilane (APTES). The functionalized nanoparticles were characterized by zeta potential measurements, Fourier transform infrared spectroscopy, and other physicochemical techniques. Although the obtained alumina nanobiostructure shows a relatively low degree of substitution with EAAA-BP100, antibacterial activities against Escherichia coli and Salmonella typhimurium strains are appreciably higher than the activities of the free peptide. The obtained results can affect the design of new hybrid nanobiomaterials based on nanoparticles functionalized with AMP. Copyright © 2018. Published by Elsevier B.V.

  14. Microbial chemical factories: recent advances in pathway engineering for synthesis of value added chemicals.

    Science.gov (United States)

    Dhamankar, Himanshu; Prather, Kristala L J

    2011-08-01

    The dwindling nature of petroleum and other fossil reserves has provided impetus towards microbial synthesis of fuels and value added chemicals from biomass-derived sugars as a renewable resource. Microbes have naturally evolved enzymes and pathways that can convert biomass into hundreds of unique chemical structures, a property that can be effectively exploited for their engineering into Microbial Chemical Factories (MCFs). De novo pathway engineering facilitates expansion of the repertoire of microbially synthesized compounds beyond natural products. In this review, we visit some recent successes in such novel pathway engineering and optimization, with particular emphasis on the selection and engineering of pathway enzymes and balancing of their accessory cofactors. Copyright © 2011 Elsevier Ltd. All rights reserved.

  15. Synthesis of protected peptides from the human IgG1 hinge region on PEG support using disulfide bond synthons and alkaline or enzymatic detachment

    Czech Academy of Sciences Publication Activity Database

    Niederhafner, Petr; Šafařík, Martin; Šebestík, Jaroslav; Gut, Vladimír; Maloň, Petr; Hlaváček, Jan

    2006-01-01

    Roč. 47, č. 6 (2006), s. 1023-1025 ISSN 0040-4039 R&D Projects: GA ČR(CZ) GA203/03/1362 Institutional research plan: CEZ:AV0Z40550506 Keywords : peptide synthesis * IgG1 hinge peptide * PEG carrier Subject RIV: CC - Organic Chemistry Impact factor: 2.509, year: 2006

  16. Synthesis of a designed transmembrane protein by thioether ligation of solubilised segments : Nα-haloacetylated peptides survived resin cleavage using TFA with EDT as scavenger

    NARCIS (Netherlands)

    Englebretsen, D.R; Choma, C.T.; Robillard, G.T.

    1998-01-01

    Nα-haloacetylated peptides made by Fmoc solid phase synthesis survived cleavage when EDT was used as a cleavage component. Two segments of a desgned transmembrane protein, one bromoacetylated, the other containing a cysteine, and each bearing a "solubilising tail" peptide, were synthesised by Fmoc

  17. Synthesis, secretion, function, metabolism and application of natriuretic peptides in heart failure.

    Science.gov (United States)

    Fu, Shihui; Ping, Ping; Wang, Fengqi; Luo, Leiming

    2018-01-01

    As a family of hormones with pleiotropic effects, natriuretic peptide (NP) system includes atrial NP (ANP), B-type NP (BNP), C-type NP (CNP), dendroaspis NP and urodilatin, with NP receptor-A (guanylate cyclase-A), NP receptor-B (guanylate cyclase-B) and NP receptor-C (clearance receptor). These peptides are genetically distinct, but structurally and functionally related for regulating circulatory homeostasis in vertebrates. In humans, ANP and BNP are encoded by NP precursor A (NPPA) and NPPB genes on chromosome 1, whereas CNP is encoded by NPPC on chromosome 2. NPs are synthesized and secreted through certain mechanisms by cardiomyocytes, fibroblasts, endotheliocytes, immune cells (neutrophils, T-cells and macrophages) and immature cells (embryonic stem cells, muscle satellite cells and cardiac precursor cells). They are mainly produced by cardiovascular, brain and renal tissues in response to wall stretch and other causes. NPs provide natriuresis, diuresis, vasodilation, antiproliferation, antihypertrophy, antifibrosis and other cardiometabolic protection. NPs represent body's own antihypertensive system, and provide compensatory protection to counterbalance vasoconstrictor-mitogenic-sodium retaining hormones, released by renin-angiotensin-aldosterone system (RAAS) and sympathetic nervous system (SNS). NPs play central roles in regulation of heart failure (HF), and are inactivated through not only NP receptor-C, but also neutral endopeptidase (NEP), dipeptidyl peptidase-4 and insulin degrading enzyme. Both BNP and N-terminal proBNP are useful biomarkers to not only make the diagnosis and assess the severity of HF, but also guide the therapy and predict the prognosis in patients with HF. Current NP-augmenting strategies include the synthesis of NPs or agonists to increase NP bioactivity and inhibition of NEP to reduce NP breakdown. Nesiritide has been established as an available therapy, and angiotensin receptor blocker NEP inhibitor (ARNI, LCZ696) has obtained

  18. Recent Developments in Chemical Synthesis with Biocatalysts in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Mahesh K. Potdar

    2015-09-01

    Full Text Available Over the past decade, a variety of ionic liquids have emerged as greener solvents for use in the chemical manufacturing industries. Their unique properties have attracted the interest of chemists worldwide to employ them as replacement for conventional solvents in a diverse range of chemical transformations including biotransformations. Biocatalysts are often regarded as green catalysts compared to conventional chemical catalysts in organic synthesis owing to their properties of low toxicity, biodegradability, excellent selectivity and good catalytic performance under mild reaction conditions. Similarly, a selected number of specific ionic liquids can be considered as greener solvents superior to organic solvents owing to their negligible vapor pressure, low flammability, low toxicity and ability to dissolve a wide range of organic and biological substances, including proteins. A combination of biocatalysts and ionic liquids thus appears to be a logical and promising opportunity for industrial use as an alternative to conventional organic chemistry processes employing organic solvents. This article provides an overview of recent developments in this field with special emphasis on the application of more sustainable enzyme-catalyzed reactions and separation processes employing ionic liquids, driven by advances in fundamental knowledge, process optimization and industrial deployment.

  19. Soft chemical synthesis of silicon nanosheets and their applications

    Energy Technology Data Exchange (ETDEWEB)

    Nakano, Hideyuki; Ikuno, Takashi [Toyota Central R& D Labs., Inc., 41-1 Yokomichi, Nagakute, Aichi 480-1192 (Japan)

    2016-12-15

    Two-dimensional silicon nanomaterials are expected to show different properties from those of bulk silicon materials by virtue of surface functionalization and quantum size effects. Since facile fabrication processes of large area silicon nanosheets (SiNSs) are required for practical applications, a development of soft chemical synthesis route without using conventional vacuum processes is a challenging issue. We have recently succeeded to prepare SiNSs with sub-nanometer thicknesses by exfoliating layered silicon compounds, and they are found to be composed of crystalline single-atom-thick silicon layers. In this review, we present the synthesis and modification methods of SiNSs. These SiNSs have atomically flat and smooth surfaces due to dense coverage of organic moieties, and they are easily self-assembled in a concentrated state to form a regularly stacked structure. We have also characterized the electron transport properties and the electronic structures of SiNSs. Finally, the potential applications of these SiNSs and organic modified SiNSs are also reviewed.

  20. Bioinspired chemical synthesis of monomeric and dimeric stephacidin A congeners

    Science.gov (United States)

    Mukai, Ken; de Sant'ana, Danilo Pereira; Hirooka, Yasuo; Mercado-Marin, Eduardo V.; Stephens, David E.; Kou, Kevin G. M.; Richter, Sven C.; Kelley, Naomi; Sarpong, Richmond

    2018-01-01

    Stephacidin A and its congeners are a collection of secondary metabolites that possess intriguing structural motifs. They stem from unusual biosynthetic sequences that lead to the incorporation of a prenyl or reverse-prenyl group into a bicyclo[2.2.2]diazaoctane framework, a chromene unit or the vestige thereof. To complement biosynthetic studies, which normally play a significant role in unveiling the biosynthetic pathways of natural products, here we demonstrate that chemical synthesis can provide important insights into biosynthesis. We identify a short total synthesis of congeners in the reverse-prenylated indole alkaloid family related to stephacidin A by taking advantage of a direct indole C6 halogenation of the related ketopremalbrancheamide. This novel strategic approach has now made possible the syntheses of several natural products, including malbrancheamides B and C, notoamides F, I and R, aspergamide B, and waikialoid A, which is a heterodimer of avrainvillamide and aspergamide B. Our approach to the preparation of these prenylated and reverse-prenylated indole alkaloids is bioinspired, and may also inform the as-yet undetermined biosynthesis of several congeners.

  1. Unusual chemical properties of N-terminal histidine residues of glucagon and vasoactive intestinal peptide

    International Nuclear Information System (INIS)

    Hefford, M.A.; Evans, R.M.; Oda, G.; Kaplan, H.

    1985-01-01

    An N-terminal histidine residue of a protein or peptide has two functional groups, viz., an alpha-amino group and an imidazole group. A new procedure, based on the competitive labeling approach described by Duggleby and Kaplan has been developed by which the chemical reactivity of each functional group in such a residue can be determined as a function of pH. Only very small amounts of material are required, which makes it possible to determine the chemical properties in dilute solution or in proteins and polypeptides that can be obtained in only minute quantities. With this approach, the reactivity of the alpha-amino group of histidylglycine toward 1-fluoro-2,4-dinitrobenzene gave an apparent pK /sub a/ value of 7.64 +/- 0.07 at 37 degrees C, in good agreement with a value of 7.69 +/- 0.02 obtained by acid-base titration. However, the reactivity of the imidazole function gave an apparent pK /sub a/ value of 7.16 +/- 0.07 as compared to the pK /sub a/ value of 5.85 +/- 0.01 obtained by acid-base titration. Similarly, in glucagon and vasoactive intestinal peptide (VIP), apparent pKa values of 7.60 +/- 0.04 and 7.88 +/- 0.18, respectively, were obtained for the alpha-amino of their N-terminal histidine, and pKa values of 7.43 +/- 0.09 and 7.59 +/- 0.18 were obtained for the imidazole function

  2. Design, Synthesis, and Biological Evaluation of Vanillin Hydroxamic Acid Derivatives as Novel Peptide Deformylase Inhibitors.

    Science.gov (United States)

    Gao, Jian; Qiu, Shengzhi; Liang, Li; Hao, Zhixiang; Zhou, Qianqian; Wang, Fanfan; Mou, Jie; Lin, Qisi

    2018-01-01

    Infectious disease is increasingly hampering human health, which challenge the discovery of new antibacterial target. Peptide deformylase (PDF), a metalloenzyme responsible for catalyzing the removal of the N-formyl group from nascent proteins, was considered as an important target in antibacterial drug discovery. Reported here are the design, synthesis and biological evaluation of vanillin hydroxamic acid derivatives. Analysis of the structure-activity relationships lead to the discovery of compound 8, which exhibits promising antibacterial activity against Escherichia coli, Staphylococcus aureus, Aspergillus oryzae, and Aspergillus foetidus with the MIC value of 0.32 µg/ml, 0.32 µg/ml, 0.16 µg/ml and 0.16 µg/ml, respectively. Furthermore, molecular docking study was applied to elucidate binding interaction between compound 8 and PDF, which indicate that compound 8 not only shares the same binding pocket with actinonin, but also has a similar binding pattern. In silico pharmacokinetic and toxicity prediction studies also suggested that compound 8 has a relatively high drug score of 0.80, and has no risk of toxicity. Compound 8 might represent a promising scaffold for the further development of novel antibacterial drugs. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  3. Synthesis and Pharmacology of Halogenated δ-Opioid-Selective [D-Ala2]Deltorphin II Peptide Analogues

    Science.gov (United States)

    Pescatore, Robyn; Marrone, Gina F.; Sedberry, Seth; Vinton, Daniel; Finkelstein, Netanel; Katlowitz, Yitzchak E.; Pasternak, Gavril W.; Wilson, Krista R.; Majumdar, Susruta

    2015-01-01

    Deltorphins are naturally occurring peptides produced by the skin of the giant monkey frog (Phyllomedusa bicolor). They are δ-opioid receptor-selective agonists. Herein, we report the design and synthesis of a peptide, Tyr-D-Ala-(pI)Phe-Glu-Ile-Ile-Gly-NH2 3 (GATE3-8), based on the [D-Ala2]deltorphin II template, which is δ-selective in in vitro radioligand binding assays over the μ- and κ-opioid receptors. It is a full agonist in [35S]GTPγS functional assays and analgesic when administered supraspinally to mice. Analgesia of 3 (GATE3-8) is blocked by the selective δ receptor antagonist naltrindole, indicating that the analgesic action of 3 is mediated by the δ-opioid receptor. We have established a radioligand in which 125I isincorporated into 3 (GATE3-8). The radioligand has a KD of 0.1 nM in Chinese hamster ovary (CHO) cells expressing the δ receptor. Additionally, a series of peptides based on 3 (GATE3-8) was synthesized by incorporating various halogens in the para position on the aromatic ring of Phe3. The peptides were characterized for binding affinity at the μ-, δ-, and κ-opioid receptors, which showed a linear correlation between binding affinity and the size of the halogen substituent. These peptides may be interesting tools for probing δ-opioid receptor pharmacology. PMID:25844930

  4. Synthesis and pharmacology of halogenated δ-opioid-selective [d-Ala(2)]deltorphin II peptide analogues.

    Science.gov (United States)

    Pescatore, Robyn; Marrone, Gina F; Sedberry, Seth; Vinton, Daniel; Finkelstein, Netanel; Katlowitz, Yitzchak E; Pasternak, Gavril W; Wilson, Krista R; Majumdar, Susruta

    2015-06-17

    Deltorphins are naturally occurring peptides produced by the skin of the giant monkey frog (Phyllomedusa bicolor). They are δ-opioid receptor-selective agonists. Herein, we report the design and synthesis of a peptide, Tyr-d-Ala-(pI)Phe-Glu-Ile-Ile-Gly-NH2 3 (GATE3-8), based on the [d-Ala(2)]deltorphin II template, which is δ-selective in in vitro radioligand binding assays over the μ- and κ-opioid receptors. It is a full agonist in [(35)S]GTPγS functional assays and analgesic when administered supraspinally to mice. Analgesia of 3 (GATE3-8) is blocked by the selective δ receptor antagonist naltrindole, indicating that the analgesic action of 3 is mediated by the δ-opioid receptor. We have established a radioligand in which (125)I is incorporated into 3 (GATE3-8). The radioligand has a KD of 0.1 nM in Chinese hamster ovary (CHO) cells expressing the δ receptor. Additionally, a series of peptides based on 3 (GATE3-8) was synthesized by incorporating various halogens in the para position on the aromatic ring of Phe(3). The peptides were characterized for binding affinity at the μ-, δ-, and κ-opioid receptors, which showed a linear correlation between binding affinity and the size of the halogen substituent. These peptides may be interesting tools for probing δ-opioid receptor pharmacology.

  5. Synthesis of a Hoechst 32258 Analogue Amino Acid Building Block for Direct Incorporation of a Fluorescent High-Affinity DNA Binding Motif into Peptides

    DEFF Research Database (Denmark)

    Harrit, Niels; Behrens, Carsten; Nielsen, P. E.

    2001-01-01

    The synthesis of a new versatile "Hoechst 33258-like" Boc-protected amino acid building block for peptide synthesis is described. It is demonstrated that this new ligand is an effective mimic of Hoechst 33258 in terms of DNA affinity and sequence specificity. Furthermore, this minor groove binder...

  6. New approach for direct chemical synthesis of hexagonal Co nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Abel, Frank M., E-mail: fabel@udel.edu [Physics and Astronomy, University of Delaware (United States); Tzitzios, Vasilis [Institute of Nanoscience and Nanotechnology, NCSR, Demokritos (Greece); Hadjipanayis, George C. [Physics and Astronomy, University of Delaware (United States)

    2016-02-15

    In this paper, we explore the possibility of producing hexagonal Cobalt nanoparticles, with high saturation magnetization by direct chemical synthesis. The nanoparticles were synthesized by reduction of anhydrous cobalt (II) chloride by NaBH{sub 4} in tetraglyme at temperatures in the range of 200–270 °C under a nitrogen–hydrogen atmosphere. The reactions were done at high temperatures to allow for the formation of as-made hexagonal cobalt. The size of the particles was controlled by the addition of different surfactants. The best magnetic properties so far were obtained on spherical hexagonal Co nanoparticles with an average size of 45 nm, a saturation magnetization of 143 emu/g and coercivity of 500 Oe. the saturation magnetization and coercivity were further improved by annealing the Co nanoparticles leading to saturation magnetization of 160 emu/g and coercivity of 540 Oe. - Highlights: • We synthesized hexagonal cobalt nanoparticles by a new wet chemical method. • We considered the effects of different surfactants on particles magnetic properties. • The as-made Co nanoparticles had magnetic properties of 143 emu/g and 500 Oe. • After annealing magnetic properties of 160 emu/g and 540 Oe were obtained.

  7. High-throughput peptide mass fingerprinting and protein macroarray analysis using chemical printing strategies

    International Nuclear Information System (INIS)

    Sloane, A.J.; Duff, J.L.; Hopwood, F.G.; Wilson, N.L.; Smith, P.E.; Hill, C.J.; Packer, N.H.; Williams, K.L.; Gooley, A.A.; Cole, R.A.; Cooley, P.W.; Wallace, D.B.

    2001-01-01

    We describe a 'chemical printer' that uses piezoelectric pulsing for rapid and accurate microdispensing of picolitre volumes of fluid for proteomic analysis of 'protein macroarrays'. Unlike positive transfer and pin transfer systems, our printer dispenses fluid in a non-contact process that ensures that the fluid source cannot be contaminated by substrate during a printing event. We demonstrate automated delivery of enzyme and matrix solutions for on-membrane protein digestion and subsequent peptide mass fingerprinting (pmf) analysis directly from the membrane surface using matrix-assisted laser-desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry (MS). This approach bypasses the more commonly used multi-step procedures, thereby permitting a more rapid procedure for protein identification. We also highlight the advantage of printing different chemistries onto an individual protein spot for multiple microscale analyses. This ability is particularly useful when detailed characterisation of rare and valuable sample is required. Using a combination of PNGase F and trypsin we have mapped sites of N-glycosylation using on-membrane digestion strategies. We also demonstrate the ability to print multiple serum samples in a micro-ELISA format and rapidly screen a protein macroarray of human blood plasma for pathogen-derived antigens. We anticipate that the 'chemical printer' will be a major component of proteomic platforms for high-throughput protein identification and characterisation with widespread applications in biomedical and diagnostic discovery

  8. The host antimicrobial peptide Bac71-35 binds to bacterial ribosomal proteins and inhibits protein synthesis.

    Science.gov (United States)

    Mardirossian, Mario; Grzela, Renata; Giglione, Carmela; Meinnel, Thierry; Gennaro, Renato; Mergaert, Peter; Scocchi, Marco

    2014-12-18

    Antimicrobial peptides (AMPs) are molecules from innate immunity with high potential as novel anti-infective agents. Most of them inactivate bacteria through pore formation or membrane barrier disruption, but others cross the membrane without damages and act inside the cells, affecting vital processes. However, little is known about their intracellular bacterial targets. Here we report that Bac71-35, a proline-rich AMP belonging to the cathelicidin family, can reach high concentrations (up to 340 μM) inside the E. coli cytoplasm. The peptide specifically and completely inhibits in vitro translation in the micromolar concentration range. Experiments of incorporation of radioactive precursors in macromolecules with E. coli cells confirmed that Bac71-35 affects specifically protein synthesis. Ribosome coprecipitation and crosslinking assays showed that the peptide interacts with ribosomes, binding to a limited subset of ribosomal proteins. Overall, these results indicate that the killing mechanism of Bac71-35 is based on a specific block of protein synthesis. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Synthesis and Characterization of Chemically Etched Nanostructured Silicon

    KAUST Repository

    Mughal, Asad Jahangir

    2012-05-01

    Silicon is an essential element in today’s modern world. Nanostructured Si is a more recently studied variant, which has currently garnered much attention. When its spatial dimensions are confined below a certain limit, its optical properties change dramatically. It transforms from an indirect bandgap material that does not absorb or emit light efficiently into one which can emit visible light at room temperatures. Although much work has been conducted in understanding the properties of nanostructured Si, in particular porous Si surfaces, a clear understanding of the origin of photoluminescence has not yet been produced. Typical synthesis approaches used to produce nanostructured Si, in particular porous Si and nanocrystalline Si have involved complex preparations used at high temperatures, pressures, or currents. The purpose of this thesis is to develop an easier synthesis approach to produce nanostructured Si as well as arrive at a clearer understanding of the origin of photoluminescence in these systems. We used a simple chemical etching technique followed by sonication to produce nanostructured Si suspensions. The etching process involved producing pores on the surface of a Si substrate in a solution containing hydrofluoric acid and an oxidant. Nanocrystalline Si as well as nanoscale amorphous porous Si suspensions were successfully synthesized using this process. We probed into the phase, composition, and origin of photoluminescence in these materials, through the use of several characterization techniques. TEM and SEM were used to determine morphology and phase. FT-IR and XPS were employed to study chemical compositions, and steady state and time resolved optical spectroscopy techniques were applied to resolve their photoluminescent properties. Our work has revealed that the type of oxidant utilized during etching had a significant impact on the final product. When using nitric acid as the oxidant, we formed nanocrystalline Si suspensions composed of

  10. Biomimetic and Aggregation-Driven Crystallization Route for Room-Temperature Material Synthesis: Growth of β-Ga2O3 Nanoparticles Using Peptide Assemblies as Nanoreactors

    Science.gov (United States)

    Lee, Sang-Yup; Gao, Xueyun; Matsui, Hiroshi

    2008-01-01

    The room temperature synthesis of β-Ga2O3 nanocrystal was examined by coupling two biomimetic crystallization techniques, the enzymatic peptide nano-assembly templating and the aggregation-driven crystallization. The catalytic template of peptide assembly nucleated and mineralized primary β-Ga2O3 crystals, and then fused them to grow single-crystalline and monodisperse nanoparticles in the cavity of the peptide assembly at room temperature. In this work, the peptide assembly was exploited as a nano-reactor with an enzymatic functionality catalyzing the hydrolysis of gallium precursors. In addition, the characteristic ring-structure of peptide assembly is expected to provide an efficient dehydration pathway and the crystallization control over the surface tension, which are advantageous for the β-Ga2O3 crystal growth. This multifunctional peptide assembly could be applied for syntheses of a variety of nanomaterials that are kinetically difficult to grow at room temperature. PMID:17302413

  11. Size-controlled synthesis of transition metal nanoparticles through chemical and photo-chemical routes

    Science.gov (United States)

    Tangeysh, Behzad

    The central objective of this work is developing convenient general procedures for controlling the formation and stabilization of nanoscale transition metal particles. Contemporary interest in developing alternative synthetic approaches for producing nanoparticles arises in large part from expanding applications of the nanomaterials in areas such as catalysis, electronics and medicine. This research focuses on advancing the existing nanoparticle synthetic routes by using a new class of polymer colloid materials as a chemical approach, and the laser irradiation of metal salt solution as a photo-chemical method to attain size and shape selectivity. Controlled synthesis of small metal nanoparticles with sizes ranging from 1 to 5nm is still a continuing challenge in nanomaterial synthesis. This research utilizes a new class of polymer colloid materials as nano-reactors and protective agents for controlling the formation of small transition metal nanoparticles. The polymer colloid particles were formed from cross-linking of dinegatively charged metal precursors with partially protonated poly dimethylaminoethylmethacrylate (PDMAEMA). Incorporation of [PtCl6]2- species into the colloidal particles prior to the chemical reduction was effectively employed as a new strategy for synthesis of unusually small platinum nanoparticles with narrow size distributions (1.12 +/-0.25nm). To explore the generality of this approach, in a series of proof-of-concept studies, this method was successfully employed for the synthesis of small palladium (1.4 +/-0.2nm) and copper nanoparticles (1.5 +/-0.6nm). The polymer colloid materials developed in this research are pH responsive, and are designed to self-assemble and/or disassemble by varying the levels of protonation of the polymer chains. This unique feature was used to tune the size of palladium nanoparticles in a small range from 1nm to 5nm. The procedure presented in this work is a new convenient room temperature route for synthesis of

  12. Microwave-assisted solid-phase peptide synthesis of the 60-110 domain of human pleiotrophin on 2-chlorotrityl resin.

    Science.gov (United States)

    Friligou, Irene; Papadimitriou, Evangelia; Gatos, Dimitrios; Matsoukas, John; Tselios, Theodore

    2011-05-01

    A fast and efficient microwave-assisted solid phase peptide synthesis (MW-SPPS) of a 51mer peptide, the main heparin-binding site (60-110) of human pleiotrophin (hPTN), using 2-chlorotrityl chloride resin (CLTR-Cl) following the 9-fluorenylmethyloxycarbonyl/tert-butyl (Fmoc/tBu) methodology and with the standard N,N'-diisopropylcarbodiimide/1-hydroxybenzotriazole (DIC/HOBt) coupling reagents, is described. An MW-SPPS protocol was for the first time successfully applied to the acid labile CLTR-Cl for the faster synthesis of long peptides (51mer peptide) and with an enhanced purity in comparison to conventional SPPS protocols. The synthesis of such long peptides is not trivial and it is generally achieved by recombinant techniques. The desired linear peptide was obtained in only 30 h of total processing time and in 51% crude yield, in which 60% was the purified product obtained with 99.4% purity. The synthesized peptide was purified by reversed phase high performance liquid chromatography (RP-HPLC) and identified by electrospray ionization mass spectrometry (ESI-MS). Then, the regioselective formation of the two disulfide bridges of hPTN 60-110 was successfully achieved by a two-step procedure, involving an oxidative folding step in dimethylsulfoxide (DMSO) to form the Cys(77)-Cys(109) bond, followed by iodine oxidation to form the Cys(67)-Cys(99) bond.

  13. Plant polyphenols: chemical properties, biological activities, and synthesis.

    Science.gov (United States)

    Quideau, Stéphane; Deffieux, Denis; Douat-Casassus, Céline; Pouységu, Laurent

    2011-01-17

    Eating five servings of fruits and vegetables per day! This is what is highly recommended and heavily advertised nowadays to the general public to stay fit and healthy! Drinking green tea on a regular basis, eating chocolate from time to time, as well as savoring a couple of glasses of red wine per day have been claimed to increase life expectancy even further! Why? The answer is in fact still under scientific scrutiny, but a particular class of compounds naturally occurring in fruits and vegetables is considered to be crucial for the expression of such human health benefits: the polyphenols! What are these plant products really? What are their physicochemical properties? How do they express their biological activity? Are they really valuable for disease prevention? Can they be used to develop new pharmaceutical drugs? What recent progress has been made toward their preparation by organic synthesis? This Review gives answers from a chemical perspective, summarizes the state of the art, and highlights the most significant advances in the field of polyphenol research. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Mechanochemical synthesis of nanostructured chemical hydrides in hydrogen alloying mills

    International Nuclear Information System (INIS)

    Wronski, Z.; Varin, R.A.; Chiu, C.; Czujko, T.; Calka, A.

    2007-01-01

    Mechanical alloying of magnesium metal powders with hydrogen in specialized hydrogen ball mills can be used as a direct route for mechanochemical synthesis of emerging chemical hydrides and hydride mixtures for advanced solid-state hydrogen storage. In the 2Mg-Fe system, we have successfully synthesized the ternary complex hydride Mg 2 FeH 6 in a mixture with nanometric Fe particles. The mixture of complex magnesium-iron hydride and nano-iron released 3-4 wt.%H 2 in a thermally programmed desorption experiment at the range 285-295 o C. Milling of the Mg-2Al powder mixture revealed a strong competition between formation of the Al(Mg) solid solution and the β-MgH 2 hydride. The former decomposes upon longer milling as the Mg atoms react with hydrogen to form the hydride phase, and drive the Al out of the solid solution. The mixture of magnesium dihydride and nano-aluminum released 2.1 wt.%H 2 in the temperature range 329-340 o C in the differential scanning calorimetry experiment. The formation of MgH 2 was suppressed in the Mg-B system; instead, a hydrogenated amorphous phase (Mg,B)H x , was formed in a mixture with nanometric MgB 2 . Annealing of the hydrogen-stabilized amorphous mixture produced crystalline MgB 2

  15. Mechano-chemical synthesis of strontium britholites: Reaction mechanism

    International Nuclear Information System (INIS)

    Gmati, N.; Boughzala, K.; Bouzouita, K.; Abdellaoui, M.

    2011-01-01

    The britholites have gained a great interest thanks to their potential applications as matrices for the confinement of the byproducts in the nuclear industry such as minor actinides and long-lived fission products. However, the preparation of britholites requires high temperatures, above 1200 C. In this work, we strive to prepare these kinds of compounds by a mechano-chemical synthesis at room temperature from the starting materials SrF 2 , SrCO 3 , Sr 2 P 2 O 7 , La 2 O 3 and SiO 2 using a planetary ball mill. The obtained results showed that the prepared products were carbonated apatites and the corresponding powders contained some unreacted silica and lanthana. To obtain pure britholites, a heat-treatment at 1100 C was required. The mechanism involved in the different steps of the reaction is discussed in this paper. The obtained results suggest that the use of raw materials containing no carbonate is expected to directly lead to pure britholites by appropriate milling at room temperature. (authors)

  16. DEVELOPMENT OF ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter J. Tijrn

    2003-05-31

    This Final Report for Cooperative Agreement No. DE-FC22-95PC93052, the ''Development of Alternative Fuels and Chemicals from Synthesis Gas,'' was prepared by Air Products and Chemicals, Inc. (Air Products), and covers activities from 29 December 1994 through 31 July 2002. The overall objectives of this program were to investigate potential technologies for the conversion of synthesis gas (syngas), a mixture primarily of hydrogen (H{sub 2}) and carbon monoxide (CO), to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at the LaPorte, Texas Alternative Fuels Development Unit (AFDU). Laboratory work was performed by Air Products and a variety of subcontractors, and focused on the study of the kinetics of production of methanol and dimethyl ether (DME) from syngas, the production of DME using the Liquid Phase Dimethyl Ether (LPDME{trademark}) Process, the conversion of DME to fuels and chemicals, and the production of other higher value products from syngas. Four operating campaigns were performed at the AFDU during the performance period. Tests of the Liquid Phase Methanol (LPMEOH{trademark}) Process and the LPDME{trademark} Process were made to confirm results from the laboratory program and to allow for the study of the hydrodynamics of the slurry bubble column reactor (SBCR) at a significant engineering scale. Two campaigns demonstrated the conversion of syngas to hydrocarbon products via the slurry-phase Fischer-Tropsch (F-T) process. Other topics that were studied within this program include the economics of production of methyl tert-butyl ether (MTBE), the identification of trace components in coal-derived syngas and the means to economically remove these species, and the study of systems for separation of wax from catalyst in the F-T process. The work performed under this Cooperative Agreement has continued to promote the development of technologies that use clean syngas produced

  17. Sensitivity of ab Initio vs Empirical Methods in Computing Structural Effects on NMR Chemical Shifts for the Example of Peptides.

    Science.gov (United States)

    Sumowski, Chris Vanessa; Hanni, Matti; Schweizer, Sabine; Ochsenfeld, Christian

    2014-01-14

    The structural sensitivity of NMR chemical shifts as computed by quantum chemical methods is compared to a variety of empirical approaches for the example of a prototypical peptide, the 38-residue kaliotoxin KTX comprising 573 atoms. Despite the simplicity of empirical chemical shift prediction programs, the agreement with experimental results is rather good, underlining their usefulness. However, we show in our present work that they are highly insensitive to structural changes, which renders their use for validating predicted structures questionable. In contrast, quantum chemical methods show the expected high sensitivity to structural and electronic changes. This appears to be independent of the quantum chemical approach or the inclusion of solvent effects. For the latter, explicit solvent simulations with increasing number of snapshots were performed for two conformers of an eight amino acid sequence. In conclusion, the empirical approaches neither provide the expected magnitude nor the patterns of NMR chemical shifts determined by the clearly more costly ab initio methods upon structural changes. This restricts the use of empirical prediction programs in studies where peptide and protein structures are utilized for the NMR chemical shift evaluation such as in NMR refinement processes, structural model verifications, or calculations of NMR nuclear spin relaxation rates.

  18. Optimization of synthesis and quality control procedures for the preparations of 18F and 123I labelled peptides

    International Nuclear Information System (INIS)

    Archimandritis, S.C.; Potamianos, S.; Varvarigou, A.D.

    2002-01-01

    Radiolabelled biomolecules like proteins and peptides, are playing now days an important role in experimental and clinical Nuclear Medicine. Radioiodination techniques remain important, with improvements accounting for high purity, specific activity and better in vivo stability. Radioiodination using prosthetic groups is the method of choice in cases where the molecules are lacking of thyrosyl groups in their structure and are also sensitive to circulating dehalogenase enzymes. This investigation was based on the need to optimize labelling and quality control techniques for these molecules. The N-succinimidyliodobenzoate (SIB) was used in this study as the prosthetic group for the radioiodination. Optimization of SIB synthesis and modification of the protocol resulted in an improved mean yield of SIB. The combination of TLC and column chromatography using silica gel proved suitable in identifying SIB. Furthermore, the ability of SIB to couple to protein was also used to confirm the presence of SIB. In this case, SEC and ITLC-SG proved suitable to confirm protein binding of SIB. Column chromatography using silica gel containing Sep-Pak was appropriate for SIB purification. Concerning SIB conjugation to peptides, high radioiodination yields were only possible for peptides with amino-containing-side-chain amino acids. Furthermore, lysine containing peptides retained stability, at 4 deg. C, for at least 24 h and reverse phase HPLC proved the most suitable technique for assessing conjugation of SIB to peptide. The biological evaluation of the radiolabelled product was made in normal mice. SIB and SIB-peptide conjugates were tested comparatively and a number of tentative but interesting inferences were drawn. SIB and its peptide conjugates exhibited good in vivo stability as evidenced by low thyroid accumulation and were cleared via the kidneys. A time dependant decrease in the% dose per gram of tissue indicates possible adrenal metabolism of SIB and SIB-peptide

  19. Fully convergent chemical synthesis of ester insulin: determination of the high resolution X-ray structure by racemic protein crystallography.

    Science.gov (United States)

    Avital-Shmilovici, Michal; Mandal, Kalyaneswar; Gates, Zachary P; Phillips, Nelson B; Weiss, Michael A; Kent, Stephen B H

    2013-02-27

    Efficient total synthesis of insulin is important to enable the application of medicinal chemistry to the optimization of the properties of this important protein molecule. Recently we described "ester insulin"--a novel form of insulin in which the function of the 35 residue C-peptide of proinsulin is replaced by a single covalent bond--as a key intermediate for the efficient total synthesis of insulin. Here we describe a fully convergent synthetic route to the ester insulin molecule from three unprotected peptide segments of approximately equal size. The synthetic ester insulin polypeptide chain folded much more rapidly than proinsulin, and at physiological pH. Both the D-protein and L-protein enantiomers of monomeric DKP ester insulin (i.e., [Asp(B10), Lys(B28), Pro(B29)]ester insulin) were prepared by total chemical synthesis. The atomic structure of the synthetic ester insulin molecule was determined by racemic protein X-ray crystallography to a resolution of 1.6 Å. Diffraction quality crystals were readily obtained from the racemic mixture of {D-DKP ester insulin + L-DKP ester insulin}, whereas crystals were not obtained from the L-ester insulin alone even after extensive trials. Both the D-protein and L-protein enantiomers of monomeric DKP ester insulin were assayed for receptor binding and in diabetic rats, before and after conversion by saponification to the corresponding DKP insulin enantiomers. L-DKP ester insulin bound weakly to the insulin receptor, while synthetic L-DKP insulin derived from the L-DKP ester insulin intermediate was fully active in binding to the insulin receptor. The D- and L-DKP ester insulins and D-DKP insulin were inactive in lowering blood glucose in diabetic rats, while synthetic L-DKP insulin was fully active in this biological assay. The structural basis of the lack of biological activity of ester insulin is discussed.

  20. Chemical Synthesis of Proanthocyanidins in Vitro and Their Reactions in Aging Wines

    Directory of Open Access Journals (Sweden)

    Qiu-Hong Pan

    2008-12-01

    Full Text Available Proanthocyanidins are present in many fruits and plant products like grapes and wine, and contribute to their taste and health benefits. In the past decades of years, substantial progresses has been achieved in the identification of composition and structure of proanthocyanidins, but the debate concerning the existence of an enzymatic or nonenzymatic mechanism for proanthocyanidin condensation still goes on. Substantial attention has been paid to elucidating the potential mechanism of formation by means of biomimetic and chemical synthesis in vitro. The present paper aims at summarizing the research status on chemical synthesis of proanthocyanidins, including non-enzymatic synthesis of proanthocyanidin precursors, chemical synthesis of proanthocyanidins with direct condensation of flavanols and stereoselective synthesis of proanthocyanidins. Proanthocyanidin-involved reactions in aging wines are also reviewed such as direct and indirect reactions among proanthocyanidins, flavanols and anthocyanins. Topics for future research in this field are also put forward in this paper.

  1. Novel thrombopoietin mimetic peptides bind c-Mpl receptor: Synthesis, biological evaluation and molecular modeling.

    Science.gov (United States)

    Liu, Yaquan; Tian, Fang; Zhi, Dejuan; Wang, Haiqing; Zhao, Chunyan; Li, Hongyu

    2017-02-01

    Thrombopoietin (TPO) acts in promoting the proliferation of hematopoietic stem cells and by initiating specific maturation events in megakaryocytes. Now, TPO-mimetic peptides with amino acid sequences unrelated to TPO are of considerable pharmaceutical interest. In the present paper, four new TPO mimetic peptides that bind and activate c-Mpl receptor have been identified, synthesized and tested by Dual-Luciferase reporter gene assay for biological activities. The molecular modeling research was also approached to understand key molecular mechanisms and structural features responsible for peptide binding with c-Mpl receptor. The results presented that three of four mimetic peptides showed significant activities. In addition, the molecular modeling approaches proved hydrophobic interactions were the driven positive forces for binding behavior between peptides and c-Mpl receptor. TPO peptide residues in P7, P13 and P7' positions were identified by the analysis of hydrogen bonds and energy decompositions as the key ones for benefiting better biological activities. Our data suggested the synthesized peptides have considerable potential for the future development of stable and highly active TPO mimetic peptides. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Synthesis, analysis, and cytotoxic effects of novel SMAC-based peptides

    Czech Academy of Sciences Publication Activity Database

    Georgieva, M.; Dzimbova, T.; Sázelová, Petra; Detcheva, R.; Kašička, Václav; Momekov, G.; Pajpanova, T.

    2015-01-01

    Roč. 47, č. 8 (2015), s. 1687 ISSN 0939-4451. [International Congress on Amino Acids , Peptides and Proteins /14./. 03.08.2015-07.08.2015, Vienna] Institutional support: RVO:61388963 Keywords : apoptotic peptides * SMAC-mimetics * capillary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation

  3. Synthesis of α,γ-peptide hybrids by selective conversion of glutamic acid units.

    Science.gov (United States)

    Saavedra, Carlos J; Boto, Alicia; Hernández, Rosendo

    2012-07-06

    The site-selective modification of small peptides at a glutamate residue allows the ready preparation of α,γ-hybrids. In this way, a single peptide can be transformed into a variety of hybrid derivatives. The process takes place under very mild conditions, and good global yields are obtained.

  4. A Fly-Through Mission Strategy Targeting Peptide as a Signature of Chemical Evolution and Possible Life in Enceladus Plumes

    Science.gov (United States)

    Fujishima, Kosuke; Dziomba, Szymon; Takahagi, Wataru; Shibuya, Takazo; Takano, Yoshinori; Guerrouache, Mohamed; Carbonnier, Benjamin; Takai, Ken; Rothschild, Lynn J.; Yano, Hajime

    2016-01-01

    In situ detection of organic molecules in the extraterrestrial environment provides a key step towards better understanding the variety and the distribution of building blocks of life and it may ultimately lead to finding extraterrestrial life within the Solar System. Here we present combined results of two separate experiments that enable us to realize such in situ life signature detection from the deep habitats of the "Ocean World": a hydrothermal reactor experiment simulating complex organic synthesis and a simulated fly-through capture experiment of organic-bearing microparticles using silica aerogels, followed by subsequent analysis. Both experiments employ peptide as a plausible organics existing in Encleadus plume particles produced in its subsurface ocean. Recent laboratory hydrothermal experiments and a theoretical model on silica saturation indicated an on going hydrothermal reactions in subsurface Enceladus ocean. Given the porous chondritic origin of the core, it is likely that organic compounds originated by radiation chemistry such as amino acid precursors could have been provided, leached, and altered through widespread water-rock interactions. By using the same laboratory experimental setup from the latest water-rock interaction study, we performed amino acid polymerization experiments for 144 days and monitored the organic complexity changing over time. So far over 3,000 peaks up to the size of greater than 600 MW were observed through the analysis of capillary electrophoresis time-of-flight mass spectrometry (CE-TOF-MS) with an indication of amino acid derivatives and short peptides. Generally abiotic polymerization of enantiomeric amino acids results in forming stereoisomeric peptides with identical molecular weight and formula as opposed to homochiral biopolymers. Assuming Enceladus plume particles may contain a mixture of stereoisomeric peptides, we were able to distinguish 16 of the 17 stereoisomeric tripeptides as a test sample using

  5. Evaluation of a high-throughput peptide reactivity format assay for assessment of the skin sensitization potential of chemicals

    Directory of Open Access Journals (Sweden)

    Chin Lin eWong

    2016-03-01

    Full Text Available The direct peptide reactivity assay (DPRA is a validated method for in vitro assessment of the skin sensitization potential of chemicals. In the present work, we describe a peptide reactivity assay using 96-well plate format and systematically identified the optimal assay conditions for accurate and reproducible classification of chemicals with known sensitizing capacity. The aim of the research is to ensure that the analytical component of the peptide reactivity assay is robust, accurate and reproducible in accordance with criteria that are used for the validation of bioanalytical methods. Analytical performance was evaluated using quality control samples (QCs; heptapeptides at low, medium and high concentrations and incubation of control chemicals (chemicals with known sensitization capacity, weak, moderate, strong, extreme and non-sensitizers with each of three synthetic heptapeptides, viz Cor1-C420 (Ac-NKKCDLF, cysteine- (Ac-RFAACAA and lysine- (Ac-RFAAKAA containing heptapeptides. The optimal incubation temperature for all three heptapeptides was 25°C. Apparent heptapeptide depletion was affected by vial material composition. Incubation of test chemicals with Cor1-C420, showed that peptide depletion was unchanged in polypropylene vials over 3-days storage in an autosampler but this was not the case for borosilicate glass vials. For cysteine-containing heptapeptide, the concentration was not stable by day 3 post-incubation in borosilicate glass vials. Although the lysine-containing heptapeptide concentration was unchanged in both polypropylene and borosilicate glass vials, the apparent extent of lysine-containing heptapeptide depletion by ethyl acrylate, differed between polypropylene (24.7% and glass (47.3% vials. Additionally, the peptide-chemical complexes for Cor1-C420-cinnamaldehyde and cysteine-containing heptapeptide-2,4-dinitrochlorobenzene were partially reversible during 3-days of autosampler storage. These observations further

  6. Direct chemical synthesis of MnO2 nanowhiskers on MXene surfaces for supercapacitor applications

    KAUST Repository

    Baby, Rakhi Raghavan; Ahmed, Bilal; Anjum, Dalaver H.; Alshareef, Husam N.

    2016-01-01

    Transition metal carbides (MXenes) are an emerging class of two dimensional (2D) materials with promising electrochemical energy storage performance. Herein, for the first time, by direct chemical synthesis, nanocrystalline ε-MnO2 whiskers were

  7. Peptide synthesis by enzymatic catalysis: new application to the total radiosynthesis of the tritiated leucine-enkephalin hormone, using Y carboxypeptidase

    International Nuclear Information System (INIS)

    Hellio, F.

    1986-01-01

    A new method of enzymatic labelling of peptide hormones is described. The enzyme used, a protease, Y carboxypeptidase is able, in some conditions, to catalyze the formation of peptide bounds. This property has been used for the synthesis of a pentapeptide, the tritiated leucine-enkephalin, with the incorporation of every radioactive amino acid. The specific radioactivity of the labelled molecule is 139 Ci/mmole and its biological properties (receptor binding and immunoreactivity) are identical with native leucine-enkephalin properties [fr

  8. Alzheimer’s disease against peptides products of enzymatic cleavage APP protein: Biological, pathobiological and physico-chemical properties of fibrillating peptides

    Directory of Open Access Journals (Sweden)

    Małgorzata Marszałek

    2017-05-01

    Full Text Available Various peptides products of enzymatic cleavage of key for Alzheimer’s disease Amyloid Precursor Protein (APP are well known, but still are matter of scientific debate. The Aβ type products are especially challenging for experimental and medical research. This paper outlines several, still poorly known, biological and medical processes such as peptides biology, i.e., formation, biodistribution, translocation, transport and finally removal from brain compartments and body fluids like Intracellular Fluid (ICF, Cerebrospinal Fluid (CSF, Interstitial Fluid (ISF, blood serum or urine. In addition, the following studies concerning AD patients might prove challenging and simultaneously promising: peptides translocation through Blood-Brain – Barrier (BBB and Blood–Cerebrospinal Fluid Barrier (BCSFB and their removal from the brain according to a new concept of glymphatic system; – diagnostic difficulties that stem from physico-chemical properties and the nature of proteins or fibrillating peptides itself like low concentration, short half-live and from experimental-technical problems as well like high adsorption or low solubility of Aβ, tau or amylin. The study of diagnostic parameters is very important, as it may better reflect early changes before the disease develops; one such parameter is the Aβ42/Aβ40 ratio, or the ratio with the total tau concentration combination and other new biomarkers like Aβ1-38; other factors include oxidative stress and inflammation process proteins, complement factor H, alpha-2-macroglobulin, or clusterin. The study of various forms of pathological amyloid deposits that emerge in different but specific brain regions AD patients seems to be crucial as well. The composition of the first initial pathological, pre-fibrillating monomers of fibrillating peptides and their role in AD development and disease progression have been described as well. They are even more challenging for science and simultaneously might be

  9. On-bead chemical synthesis and display of phosphopeptides for affinity pull-down proteomics

    DEFF Research Database (Denmark)

    Malene, Brandt; Madsen, Jens C.; Bunkenborg, Jakob

    2006-01-01

    We describe a new method for phosphopeptide proteomics based on the solid-phase synthesis of phosphopeptides on beads suitable for affinity pull-down experiments. Peptide sequences containing the Bad Ser112 and Ser136 phosphorylation motifs were used as bait in affinity pull-down experiments...... (aldehyde) at the C terminus for potential activity-based proteomics. The synthetic support-bound Bad phosphopeptides were able to pull down 14-3-3zeta. Furthermore, Bad phosphopeptides bound endogenous 14-3-3 proteins, and all seven members of the 14-3-3 family were identified by mass spectrometry....... In control experiments, none of the unphosphorylated Bad peptides bound transfected 14-3-3zeta or endogenous 14-3-3. We conclude that the combined synthesis and display of phosphopeptides on-bead is a fast and efficient method for affinity pull-down proteomics....

  10. Rational design and synthesis of an orally bioavailable peptide guided by NMR amide temperature coefficients

    Science.gov (United States)

    Wang, Conan K.; Northfield, Susan E.; Colless, Barbara; Chaousis, Stephanie; Hamernig, Ingrid; Lohman, Rink-Jan; Nielsen, Daniel S.; Schroeder, Christina I.; Liras, Spiros; Price, David A.; Fairlie, David P.; Craik, David J.

    2014-01-01

    Enhancing the oral bioavailability of peptide drug leads is a major challenge in drug design. As such, methods to address this challenge are highly sought after by the pharmaceutical industry. Here, we propose a strategy to identify appropriate amides for N-methylation using temperature coefficients measured by NMR to identify exposed amides in cyclic peptides. N-methylation effectively caps these amides, modifying the overall solvation properties of the peptides and making them more membrane permeable. The approach for identifying sites for N-methylation is a rapid alternative to the elucidation of 3D structures of peptide drug leads, which has been a commonly used structure-guided approach in the past. Five leucine-rich peptide scaffolds are reported with selectively designed N-methylated derivatives. In vitro membrane permeability was assessed by parallel artificial membrane permeability assay and Caco-2 assay. The most promising N-methylated peptide was then tested in vivo. Here we report a novel peptide (15), which displayed an oral bioavailability of 33% in a rat model, thus validating the design approach. We show that this approach can also be used to explain the notable increase in oral bioavailability of a somatostatin analog. PMID:25416591

  11. Synthesis and characterization of designed BMHP1-derived self-assembling peptides for tissue engineering applications.

    Science.gov (United States)

    Silva, Diego; Natalello, Antonino; Sanii, Babak; Vasita, Rajesh; Saracino, Gloria; Zuckermann, Ronald N; Doglia, Silvia Maria; Gelain, Fabrizio

    2013-01-21

    The importance of self-assembling peptides (SAPs) in regenerative medicine is becoming increasingly recognized. The propensity of SAPs to form nanostructured fibers is governed by multiple forces including hydrogen bonds, hydrophobic interactions and π-π aromatic interactions among side chains of the amino acids. Single residue modifications in SAP sequences can significantly affect these forces. BMHP1-derived SAPs is a class of biotinylated oligopeptides, which self-assemble in β-structured fibers to form a self-healing hydrogel. In the current study, selected modifications in previously described BMHP1-derived SAPs were designed in order to investigate the influence of modified residues on self-assembly kinetics and scaffold formation properties. The Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analysis demonstrated the secondary structure (β-sheet) formation in all modified SAP sequences, whereas atomic force microscopy (AFM) analysis further confirmed the presence of nanofibers. Furthermore, the fiber shape and dimension analysis by AFM showed flattened and twisted fiber morphology ranging from ∼8 nm to ∼70 nm. The mechanical properties of the pre-assembled and post assembled solution were investigated by rheometry. The shear-thinning behavior and rapid re-healing properties of the pre-assembled solutions make them a preferable choice for injectable scaffolds. The wide range of stiffnesses (G')--from ∼1000 to ∼27,000 Pa--exhibited by the post-assembled scaffolds demonstrated their potential for a variety of tissue engineering applications. The extra cellular matrix (ECM) mimicking (physically and chemically) properties of SAP scaffolds enhanced cell adhesion and proliferation. The capability of the scaffold to facilitate murine neural stem cell (mNSC) proliferation was evaluated in vitro: the increased mNSCs adhesion and proliferation demonstrated the potential of newly synthesized SAPs for regenerative medicine

  12. An Efficient, Green Chemical Synthesis of the Malaria Drug ...

    African Journals Online (AJOL)

    Purpose: To provide a robust, efficient synthesis of the malaria drug piperaquine for potential use in resource-poor settings. Methods: We used in-process analytical technologies (IPAT; HPLC) and a program of experiments to develop a synthesis of piperaquine that avoids the presence of a toxic impurity in the API and is ...

  13. Synthesis of two tritium-labeled derivatives of a vasopressin antagonist peptide

    International Nuclear Information System (INIS)

    Landvatter, S.W.; Heys, J.R.

    1986-01-01

    SK and F 101926, a potent vasopressin antagonist, has been tritium labeled in the tyrosine residue via exchange followed by solid phase coupling to a hexapeptide. The peptide thus obtained was subsequently coupled with a PMP residue, cleaved from the resin with HF, oxidized by ferricyanide and purified by HPLC giving the desired cyclic peptide. Alternatively, a labeled PMP residue can be prepared via reduction starting from phenol. Conversion of the labeled cyclohexanone to PMP followed by solid phase coupling to a heptapeptide can then afford PMP labeled peptide. 3 refs

  14. Induction of hepatic protein synthesis by a peptide in blood plasma of patients with sepsis and trauma.

    Science.gov (United States)

    Loda, M; Clowes, G H; Dinarello, C A; George, B C; Lane, B; Richardson, W

    1984-08-01

    Accelerated release of amino acids from muscle and their uptake for protein synthesis by liver and other visceral tissues are characteristic of trauma or sepsis. Experimentally, this response is induced by interleukin-1 (IL-1) generated by activated macrophages in vitro. However, IL-1 has not been demonstrated in human blood. A small 4000-dalton peptide recently isolated from plasma of patients with sepsis and trauma induces muscle proteolysis and is called "proteolysis-inducing factor" (PIF). To test whether this agent has the ability also to induce hepatic protein synthesis, a series of animal experiments and clinical observations were undertaken. The structural and secretory (acute-phase reactants) in vitro protein synthesis in livers of normal rats injected intraperitoneally with IL-1 or PIF was significantly greater than that of normal rats or those injected with Ringer's lactate (p less than 0.01). In patients with sepsis and trauma the central plasma clearance rate of amino acids, a measure of visceral (principally hepatic) amino acid uptake, was elevated and correlated with the rates of protein synthesis in incubated liver slices obtained by biopsy at operation from the same patients (p less than 0.05). Both in vivo measured central plasma clearance rate of amino acids and in vitro measured hepatic protein synthesis correlated with plasma levels of PIF in the same patients (p less than 0.01 and p less than 0.05, respectively). We conclude that since PIF, and not IL-1, is present in human plasma and both are produced by activated macrophages, PIF seems to be the stable circulating cleavage product of IL-1, which induces not only muscle proteolysis but also hepatic protein synthesis, principally in the form of acute-phase reactants during infection and other states in which inflammation is present.

  15. A statistical view of protein chemical synthesis using NCL and extended methodologies.

    Science.gov (United States)

    Agouridas, Vangelis; El Mahdi, Ouafâa; Cargoët, Marine; Melnyk, Oleg

    2017-09-15

    Native chemical ligation and extended methodologies are the most popular chemoselective reactions for protein chemical synthesis. Their combination with desulfurization techniques can give access to small or challenging proteins that are exploited in a large variety of research areas. In this report, we have conducted a statistical review of their use for protein chemical synthesis in order to provide a flavor of the recent trends and identify the most popular chemical tools used by protein chemists. To this end, a protein chemical synthesis (PCS) database (http://pcs-db.fr) was created by collecting a set of relevant data from more than 450 publications covering the period 1994-2017. A preliminary account of what this database tells us is presented in this report. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Synthesis and chemical recycling of high polymers using C1 compounds; C1 kagobutsu ni yoru kobunshi no chemical recycle

    Energy Technology Data Exchange (ETDEWEB)

    Masuda, T. [National Institute of Materials and Chemical Research, Tsukuba (Japan)

    1997-09-01

    The paper outlined a study of the synthesis of high polymers using C1 compounds which are continuously usable chemical materials and the related compounds such as the derivatives, and also the chemical recycle. In the case of waste plastics mixed in urban refuse, effective is the chemical recycle where C1 compounds obtained by gasifying the mixed waste are used as high polymer material. For the synthesis and recycle of high polymers using C1 compounds, there are three routes: Route A (recycle via high polymer materials), Route B (recycle via C1 compounds and high polymer materials), and Route C including global-scale carbon recycle (recycle via carbon dioxide from biodegradable plastics using microorganism). Among high polymers, those that can be synthesized from C1 compounds, for example, polymethylene, polyacetal and polyketone can be chemically recycled by Route B. 30 refs., 2 figs., 1 tab.

  17. An Intrinsically Disordered Peptide from Ebola Virus VP35 Controls Viral RNA Synthesis by Modulating Nucleoprotein-RNA Interactions

    Directory of Open Access Journals (Sweden)

    Daisy W. Leung

    2015-04-01

    Full Text Available During viral RNA synthesis, Ebola virus (EBOV nucleoprotein (NP alternates between an RNA-template-bound form and a template-free form to provide the viral polymerase access to the RNA template. In addition, newly synthesized NP must be prevented from indiscriminately binding to noncognate RNAs. Here, we investigate the molecular bases for these critical processes. We identify an intrinsically disordered peptide derived from EBOV VP35 (NPBP, residues 20–48 that binds NP with high affinity and specificity, inhibits NP oligomerization, and releases RNA from NP-RNA complexes in vitro. The structure of the NPBP/ΔNPNTD complex, solved to 3.7 Å resolution, reveals how NPBP peptide occludes a large surface area that is important for NP-NP and NP-RNA interactions and for viral RNA synthesis. Together, our results identify a highly conserved viral interface that is important for EBOV replication and can be targeted for therapeutic development.

  18. An Intrinsically Disordered Peptide from Ebola Virus VP35 Controls Viral RNA Synthesis by Modulating Nucleoprotein-RNA Interactions.

    Science.gov (United States)

    Leung, Daisy W; Borek, Dominika; Luthra, Priya; Binning, Jennifer M; Anantpadma, Manu; Liu, Gai; Harvey, Ian B; Su, Zhaoming; Endlich-Frazier, Ariel; Pan, Juanli; Shabman, Reed S; Chiu, Wah; Davey, Robert A; Otwinowski, Zbyszek; Basler, Christopher F; Amarasinghe, Gaya K

    2015-04-21

    During viral RNA synthesis, Ebola virus (EBOV) nucleoprotein (NP) alternates between an RNA-template-bound form and a template-free form to provide the viral polymerase access to the RNA template. In addition, newly synthesized NP must be prevented from indiscriminately binding to noncognate RNAs. Here, we investigate the molecular bases for these critical processes. We identify an intrinsically disordered peptide derived from EBOV VP35 (NPBP, residues 20-48) that binds NP with high affinity and specificity, inhibits NP oligomerization, and releases RNA from NP-RNA complexes in vitro. The structure of the NPBP/ΔNPNTD complex, solved to 3.7 Å resolution, reveals how NPBP peptide occludes a large surface area that is important for NP-NP and NP-RNA interactions and for viral RNA synthesis. Together, our results identify a highly conserved viral interface that is important for EBOV replication and can be targeted for therapeutic development. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

  19. Synthesis of protected 2-pyrrolylalanine for peptide chemistry and examination of its influence on prolyl amide isomer equilibrium.

    Science.gov (United States)

    Dörr, Aurélie A; Lubell, William D

    2012-08-03

    Protected enantiopure 2-pyrrolylalanine was synthesized for application in peptide science as an electron-rich arylalanine (histidine) analog with π-donor capability. (2S)-N-(Boc)-N'-(Phenylsulfonyl)-, (2S)-N,N'-bis-(phenylsulfonyl)-, and (2S)-N,N'-bis-(Boc)-3-(2-pyrrolyl)alanines (10, 3, and 14, respectively) were made in 13-17% overall yields and six to seven steps from oxazolidine β-methyl ester 4. Homoallylic ketone 5 was prepared by a copper-catalyzed cascade addition of vinylmagnesium bromide to ester 4 and converted to pyrrolyl amino alcohol 7 by olefin oxidation and Paal-Knorr condensation. Protecting group shuffle and oxidation of the primary alcohol enabled the synthesis of pyrrolylalanines. The bis-Boc analog 14 proved useful in peptide chemistry and was employed to make N-acetyl-pyrrolylalaninyl-proline N''-methylamide 25. A study of the influence of the pyrrole moiety on the prolyl amide isomer equilibrium of 25 using (1)H NMR spectroscopy in chloroform, DMSO, and water demonstrated that the pyrrolylalanine peptide exhibited behavior and conformations different from those of other arylalanine analogs.

  20. Mechanism of papain-catalyzed synthesis of oligo-tyrosine peptides.

    Science.gov (United States)

    Mitsuhashi, Jun; Nakayama, Tsutomu; Narai-Kanayama, Asako

    2015-01-01

    Di-, tri-, and tetra-tyrosine peptides with angiotensin I-converting enzyme inhibitory activity were synthesized by papain-catalyzed polymerization of L-tyrosine ethyl ester in aqueous media at 30 °C. Varying the reaction pH from 6.0 to 7.5 and the initial concentration of the ester substrate from 25 to 100 mM, the highest yield of oligo-tyrosine peptides (79% on a substrate basis) was produced at pH 6.5 and 75 mM, respectively. In the reaction initiated with 100 mM of the substrate, approx. 50% yield of insoluble, highly polymerized peptides accumulated. At less than 15 mM, the reaction proceeded poorly; however, from 30 mM to 120 mM a dose-dependent increase in the consumption rate of the substrate was observed with a sigmoidal curve. Meanwhile, each of the tri- and tetra-tyrosine peptides, even at approx. 5mM, was consumed effectively by papain but was not elongated to insoluble polymers. For deacylation of the acyl-papain intermediate through which a new peptide bond is made, L-tyrosine ethyl ester, even at 5mM, showed higher nucleophilic activity than di- and tri-tyrosine. These results indicate that the mechanism through which papain polymerizes L-tyrosine ethyl ester is as follows: the first interaction between papain and the ester substrate is a rate-limiting step; oligo-tyrosine peptides produced early in the reaction period are preferentially used as acyl donors, while the initial ester substrate strongly contributes as a nucleophile to the elongation of the peptide product; and the balance between hydrolytic fragmentation and further elongation of oligo-tyrosine peptides is dependent on the surrounding concentration of the ester substrate. Copyright © 2015 Elsevier Inc. All rights reserved.

  1. Improving surface functional properties of tofu whey-derived peptides by chemical modification with fatty acids.

    Science.gov (United States)

    Matemu, Athanasia Oswald; Katayama, Shigeru; Kayahara, Hisataka; Murasawa, Hisashi; Nakamura, Soichiro

    2012-04-01

    Effect of acylation with saturated fatty acids on surface functional properties of tofu whey-derived peptides was investigated. Tofu whey (TW) and soy proteins (7S, 11S, and acid-precipitated soy protein [APP]) were hydrolyzed by Protease M 'Amano' G, and resulting peptide mixtures were acylated with esterified fatty acids of different chain length (6C to 18C) to form a covalent linkage between the carboxyl group of fatty acid and the free amino groups of peptide. Acylation significantly (P properties of 7S, 11S, and APP peptides independent of fatty acid chain length. Acylation decreased water binding capacity although oil binding capacity of acylated tofu whey ultra filtered fraction (UFTW acids had shown significant higher surface hydrophobicity as in contrast with acylated UFTW acids can further affect functional properties of soy proteins. © 2012 Institute of Food Technologists®

  2. Synthesis of New Vinyl Monomers for Chemical Agent Sensing Applications

    National Research Council Canada - National Science Library

    Hogen-Esch, Thieo

    2001-01-01

    The synthesis of styrene momomer p-vinylbenzoylacetophenone (monomer i) has been carried by the acetylation of 2- chloroethylbenzene and base elimination of the resulting 4-acetyl-2-chloroethylbenzene to give 4-acetylstyrene...

  3. Sustainable Applications of Nano-Catalysts and Alternative Methods in the Greener Synthesis and Transformations of Chemical

    Science.gov (United States)

    The presentation summarizes our sustainable chemical synthesis activity involving benign alternatives, such as the use of supported reagents, and greener reaction medium in aqueous or solvent-free conditions.1 The synthesis of heterocyclic compounds, coupling reactions, and a var...

  4. Chemically functionalized gold nanoparticles: Synthesis, characterization, and applications

    Science.gov (United States)

    Daniel, Weston Lewis

    This thesis focuses on the development and application of gold nanoparticle based detection systems and biomimetic structures. Each class of modified nanoparticle has properties that are defined by its chemical moieties that interface with solution and the gold nanoparticle core. In Chapter 2, a comparison of the biomolecular composition and binding properties of various preparations of antibody oligonucleotide gold nanoparticle conjugates is presented. These constructs differed significantly in terms of their structure and binding properties. Chapter 3 reports the use of electroless gold deposition as a light scattering signal enhancer in a multiplexed, microarray-based scanometric immunoassay using the gold nanoparticle probes evaluated in Chapter 2. The use of gold development results in greater signal enhancement than the typical silver development, and multiple rounds of metal development were found to increase the resulting signal compared to one development. Chapter 4 describes an amplified scanometric detection method for human telomerase activity. Gold nanoparticles functionalized with specific oligonucleotide sequences can efficiently capture telomerase enzymes and subsequently be elongated. Both the elongated and unmodified oligonucleotide sequences are simultaneously measured. At low telomerase concentrations, elongated strands cannot be detected, but the unmodified sequences, which come from the same probe particles, can be detected because their concentration is higher, providing a novel form of amplification. Chapter 5 reports the development of a novel colorimetric nitrite and nitrate ion assay based upon gold nanoparticle probes functionalized with Griess reaction reagents. This assay takes advantage of the distance-dependent plasmonic properties of the gold nanoparticles and the ability of nitrite ion to facilitate the cross coupling of novel nanoparticle probes. The assay works on the concept of a kinetic end point and can be triggered at the EPA

  5. NMR spectroscopic studies of a TAT-derived model peptide in imidazolium-based ILs: influence on chemical shifts and the cis/trans equilibrium state.

    Science.gov (United States)

    Wiedemann, Christoph; Ohlenschläger, Oliver; Mrestani-Klaus, Carmen; Bordusa, Frank

    2017-09-13

    NMR spectroscopy was used to study systematically the impact of imidazolium-based ionic liquid (IL) solutions on a TAT-derived model peptide containing Xaa-Pro peptide bonds. The selected IL anions cover a wide range of the Hofmeister series of ions. Based on highly resolved one- and two-dimensional NMR spectra individual 1 H and 13 C peptide chemical shift differences were analysed and a classification of IL anions according to the Hofmeister series was derived. The observed chemical shift changes indicate significant interactions between the peptide and the ILs. In addition, we examined the impact of different ILs towards the cis/trans equilibrium state of the Xaa-Pro peptide bonds. In this context, the IL cations appear to be of exceptional importance for inducing an alteration of the native cis/trans equilibrium state of Xaa-Pro bonds in favour of the trans-isomers.

  6. Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

    International Nuclear Information System (INIS)

    Ridder, Barbara; Foertsch, Tobias C.; Welle, Alexander; Mattes, Daniela S.; Bojnicic-Kninski, Clemens M. von; Loeffler, Felix F.; Nesterov-Mueller, Alexander; Meier, Michael A.R.; Breitling, Frank

    2016-01-01

    Highlights: • New matrix material for peptide array synthesis from a ‘solid solvent’. • Resolution was increased with possible spot densities of up to 20.000 spots per cm"2. • The coupling depth and the effectiveness of washing steps analyzed by ToF-SIMS. • Adaptations and custom changes of the matrix material are possible. - Abstract: Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a “solid” solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm"2, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

  7. Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

    Energy Technology Data Exchange (ETDEWEB)

    Ridder, Barbara [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Foertsch, Tobias C. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Welle, Alexander [Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Mattes, Daniela S. [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Bojnicic-Kninski, Clemens M. von; Loeffler, Felix F.; Nesterov-Mueller, Alexander [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Meier, Michael A.R., E-mail: m.a.r.meier@kit.edu [Institute of Organic Chemistry (IOC), Karlsruhe Institute of Technology (KIT), Fritz-Haber-Weg 6, 76131 Karlsruhe (Germany); Breitling, Frank, E-mail: frank.breitling@kit.edu [Institute of Microstructure Technology (IMT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

    2016-12-15

    Highlights: • New matrix material for peptide array synthesis from a ‘solid solvent’. • Resolution was increased with possible spot densities of up to 20.000 spots per cm{sup 2}. • The coupling depth and the effectiveness of washing steps analyzed by ToF-SIMS. • Adaptations and custom changes of the matrix material are possible. - Abstract: Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a “solid” solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm{sup 2}, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

  8. Structure, synthesis, and molecular cloning of dermaseptins B, a family of skin peptide antibiotics.

    Science.gov (United States)

    Charpentier, S; Amiche, M; Mester, J; Vouille, V; Le Caer, J P; Nicolas, P; Delfour, A

    1998-06-12

    Analysis of antimicrobial activities that are present in the skin secretions of the South American frog Phyllomedusa bicolor revealed six polycationic (lysine-rich) and amphipathic alpha-helical peptides, 24-33 residues long, termed dermaseptins B1 to B6, respectively. Prepro-dermaseptins B all contain an almost identical signal peptide, which is followed by a conserved acidic propiece, a processing signal Lys-Arg, and a dermaseptin progenitor sequence. The 22-residue signal peptide plus the first 3 residues of the acidic propiece are encoded by conserved nucleotides encompassed by the first coding exon of the dermaseptin genes. The 25-residue amino-terminal region of prepro-dermaseptins B shares 50% identity with the corresponding region of precursors for D-amino acid containing opioid peptides or for antimicrobial peptides originating from the skin of distantly related frog species. The remarkable similarity found between prepro-proteins that encode end products with strikingly different sequences, conformations, biological activities and modes of action suggests that the corresponding genes have evolved through dissemination of a conserved "secretory cassette" exon.

  9. Peptide chemistry toolbox - Transforming natural peptides into peptide therapeutics.

    Science.gov (United States)

    Erak, Miloš; Bellmann-Sickert, Kathrin; Els-Heindl, Sylvia; Beck-Sickinger, Annette G

    2018-06-01

    The development of solid phase peptide synthesis has released tremendous opportunities for using synthetic peptides in medicinal applications. In the last decades, peptide therapeutics became an emerging market in pharmaceutical industry. The need for synthetic strategies in order to improve peptidic properties, such as longer half-life, higher bioavailability, increased potency and efficiency is accordingly rising. In this mini-review, we present a toolbox of modifications in peptide chemistry for overcoming the main drawbacks during the transition from natural peptides to peptide therapeutics. Modifications at the level of the peptide backbone, amino acid side chains and higher orders of structures are described. Furthermore, we are discussing the future of peptide therapeutics development and their impact on the pharmaceutical market. Copyright © 2018 Elsevier Ltd. All rights reserved.

  10. CHEMICAL SYNTHESIS USING 'GREENER' ALTERNATIVE REACTION CONDITIONS AND MEDIA

    Science.gov (United States)

    The chemical research during the last decade has witnessed a paradigm shift towards "environmentally-friendly chemistry" more popularly known as "green chemistry" due to the increasing environmental concerns and legislative requirements to curb the release of chemical waste into ...

  11. Molecular tools for the construction of peptide-based materials.

    Science.gov (United States)

    Ramakers, B E I; van Hest, J C M; Löwik, D W P M

    2014-04-21

    Proteins and peptides are fundamental components of living systems where they play crucial roles at both functional and structural level. The versatile biological properties of these molecules make them interesting building blocks for the construction of bio-active and biocompatible materials. A variety of molecular tools can be used to fashion the peptides necessary for the assembly of these materials. In this tutorial review we shall describe five of the main techniques, namely solid phase peptide synthesis, native chemical ligation, Staudinger ligation, NCA polymerisation, and genetic engineering, that have been used to great effect for the construction of a host of peptide-based materials.

  12. AP-1/KIF13A Blocking Peptides Impair Melanosome Maturation and Melanin Synthesis

    Directory of Open Access Journals (Sweden)

    Cécile Campagne

    2018-02-01

    Full Text Available Melanocytes are specialized cells that generate unique organelles called melanosomes in which melanin is synthesized and stored. Melanosome biogenesis and melanocyte pigmentation require the transport and delivery of melanin synthesizing enzymes, such as tyrosinase and related proteins (e.g., TYRP1, from endosomes to maturing melanosomes. Among the proteins controlling endosome-melanosome transport, AP-1 together with KIF13A coordinates the endosomal sorting and trafficking of TYRP1 to melanosomes. We identify here β1-adaptin AP-1 subunit-derived peptides of 5 amino acids that block the interaction of KIF13A with AP-1 in cells. Incubating these peptides with human MNT-1 cells or 3D-reconstructed pigmented epidermis decreases pigmentation by impacting the maturation of melanosomes in fully pigmented organelles. This study highlights that peptides targeting the intracellular trafficking of melanocytes are candidate molecules to tune pigmentation in health and disease.

  13. Synthesis, secretion, function, metabolism and application of natriuretic peptides in heart failure

    OpenAIRE

    Fu, Shihui; Ping, Ping; Wang, Fengqi; Luo, Leiming

    2018-01-01

    As a family of hormones with pleiotropic effects, natriuretic peptide (NP) system includes atrial NP (ANP), B-type NP (BNP), C-type NP (CNP), dendroaspis NP and urodilatin, with NP receptor-A (guanylate cyclase-A), NP receptor-B (guanylate cyclase-B) and NP receptor-C (clearance receptor). These peptides are genetically distinct, but structurally and functionally related for regulating circulatory homeostasis in vertebrates. In humans, ANP and BNP are encoded by NP precursor A (NPPA) and NPPB...

  14. Evolutionary combinatorial chemistry, a novel tool for SAR studies on peptide transport across the blood-brain barrier. Part 2. Design, synthesis and evaluation of a first generation of peptides.

    Science.gov (United States)

    Teixidó, Meritxell; Belda, Ignasi; Zurita, Esther; Llorà, Xavier; Fabre, Myriam; Vilaró, Senén; Albericio, Fernando; Giralt, Ernest

    2005-12-01

    The use of high-throughput methods in drug discovery allows the generation and testing of a large number of compounds, but at the price of providing redundant information. Evolutionary combinatorial chemistry combines the selection and synthesis of biologically active compounds with artificial intelligence optimization methods, such as genetic algorithms (GA). Drug candidates for the treatment of central nervous system (CNS) disorders must overcome the blood-brain barrier (BBB). This paper reports a new genetic algorithm that searches for the optimal physicochemical properties for peptide transport across the blood-brain barrier. A first generation of peptides has been generated and synthesized. Due to the high content of N-methyl amino acids present in most of these peptides, their syntheses were especially challenging due to over-incorporations, deletions and DKP formations. Distinct fragmentation patterns during peptide cleavage have been identified. The first generation of peptides has been studied by evaluation techniques such as immobilized artificial membrane chromatography (IAMC), a cell-based assay, log Poctanol/water calculations, etc. Finally, a second generation has been proposed. (c) 2005 European Peptide Society and John Wiley & Sons, Ltd.

  15. Facile synthesis of aliphatic isothiocyanates and thioureas on solid phase using peptide coupling reagents

    DEFF Research Database (Denmark)

    Boas, Ulrik; Andersen, Heidi Gertz; Christensen, Jørn B.

    2004-01-01

    Peptide coupling reagents can be used as versatile reagents for the formation of aliphatic isothiocyanates and thioureas on solid phase from the corresponding solid-phase anchored aliphatic primary amines. The formation of the thioureas is fast and highly chemoselective, and proceeds via formatio...

  16. Synthesis and characterisation of substrate-based peptides as inhibitors of histone demethylase KDM4C

    DEFF Research Database (Denmark)

    Nielsen, Simon D; Leurs, Ulrike; Bergner, Magnus

    2016-01-01

    different series of peptides were designed and synthesized. One series contained N-acylated H3K9 and two series introduced triazoles in this position via click chemistry to enable facile variation of headgroups. As the click reaction is compatible with free amino acids this was performed on an azido...

  17. Dimeric Building Blocks for Solid-Phase Synthesis of α-Peptide-β-Peptoid Chimeras

    DEFF Research Database (Denmark)

    Seigan, Gitte Bonke; Vedel, Line; Matthias, Witt,

    2008-01-01

    Recently, a novel type of antimicrobial and proteolytically stable peptidomimetic oligomers having an α-peptide-β-peptoid chimeric backbone was reported. The present paper describes efficient protocols for the preparation of a wide range of dimeric building blocks, displaying different types of s...

  18. Synthesis and Biological Evaluation of a Chitobiose-Based Peptide N-Glycanase Inhibitor Library

    NARCIS (Netherlands)

    Witte, Martin D.; Horst, Danielle; Wiertz, Emmanuel J.H.J.; Marel, Gijsbert A. van der; Overkleeft, Herman S.

    2009-01-01

    Peptide N-glycanase (PNGase), the enzyme responsible for the deglycosylation of N-linked glycoproteins, has an active site related to that of cysteine proteases. Chitiobiose was equipped with electrophilic traps often used in cysteine protease inhibitors, and the resulting compounds were evaluated

  19. Design and synthesis of macrocyclic peptidyl hydroxamates as peptide deformylase inhibitors.

    Science.gov (United States)

    Shen, Gang; Zhu, Jinge; Simpson, Anthony M; Pei, Dehua

    2008-05-15

    Macrocyclic peptidyl hydroxamates were designed, synthesized, and evaluated as peptide deformylase (PDF) inhibitors. The most potent compound exhibited tight, slow-binding inhibition of Escherichia coli PDF (K(I)(*)=4.4 nM) and had potent antibacterial activity against Gram-positive bacterium Bacillus subtilis (MIC=2-4 microg/mL).

  20. Solid-Phase Synthesis of Modified Peptides as Putative Inhibitors of Histone Modifying Enzymes

    DEFF Research Database (Denmark)

    Cohrt, Anders Emil O'Hanlon

    to be compatible with all 20 naturally occurring amino acids, and were furthermore feasible on several commonly used polymeric supports. By using dilute SnCl4 for N -Boc deprotection, and NaOH for the release of material from the solid support, N -modified peptides were cleanly obtained in excellent yields...

  1. Expanding the pleuromutilin class of antibiotics by de novo chemical synthesis

    Science.gov (United States)

    Lotesta, Stephen D.; Liu, Junjia; Yates, Emma V.; Krieger, Inna; Sacchettini, James C.; Freundlich, Joel S.; Sorensen, Erik J.

    2011-01-01

    New pleuromutilin-like compounds were synthesized in approximately 11 steps from 3-allylcyclopent-2-enone by a strategy featuring sequential carbonyl addition reactions. Several analogs possessing the C14 tiamulin ester side chain displayed activity in a Mycobacterium tuberculosis mc27000 assay. The results described herein provide a basis for further efforts to expand the structural and stereochemical diversity of the pleuromutilin class of bacterial protein synthesis inhibitors through advances in chemical synthesis. PMID:21874155

  2. Synthesis and Characterization of Block Copolymers with Unique Chemical Functionalities and Entropically-Hindering Moieties

    Science.gov (United States)

    2017-08-14

    methanol as a function of chemistry , morphology and hydration levels. Accomplishments: This section is included in the "upload" section. Training...Copolymer Blend Membranes.” In Press, Polymer Engineering and Science, DOI: 10.1002 /pen.24508, 2017. 5. M. Pérez-Pérez and D. Suleiman. “Synthesis and...Synthesis and Characterization of Sulfonated Amine Block Copolymers for Energy Efficient Applications". Chemical Engineering Symposium, University of

  3. Synthesis, quantum chemical computations and x-ray ...

    African Journals Online (AJOL)

    Benyza N

    2017-05-01

    May 1, 2017 ... manganese (+II) co-ordination with pyridine-2,6-dicarboxamide oxime. We report here the synthesis, the single crystal X-ray structure of the complex and the Optimization of the structure using ... Absorption coefficient (mm. -1. ).

  4. Molecular design, synthesis and evaluation of chemical biology tools

    NARCIS (Netherlands)

    Hoogenboom, Jorin

    2017-01-01

    Chapter 1 provides a perspective of synthetic organic chemistry as a discipline involved in the design, synthesis and evaluation of complex molecules. The reader is introduced with a brief history of synthetic organic chemistry, all the while dealing with different aspects of

  5. Type I Collagen Synthesis Marker Procollagen I N-Terminal Peptide (PINP) in Prostate Cancer Patients Undergoing Intermittent Androgen Suppression

    Energy Technology Data Exchange (ETDEWEB)

    Hamilton, Gerhard, E-mail: gerhard.hamilton@toc.lbg.ac.at; Olszewski-Hamilton, Ulrike [Ludwig Boltzmann Cluster of Translational of Oncology, Nussdorfer Strasse 64, Vienna A-1090 (Austria); Theyer, Gerhard [Hospital Kittsee, Kittsee A-2421, Burgenland (Austria)

    2011-09-15

    Intermittent androgen suppression (IAS) therapy for prostate cancer patients attempts to maintain the hormone dependence of the tumor cells by cycles alternating between androgen suppression (AS) and treatment cessation till a certain prostate-specific antigen (PSA) threshold is reached. Side effects are expected to be reduced, compared to standard continuous androgen suppression (CAS) therapy. The present study examined the effect of IAS on bone metabolism by determinations of serum procollagen I N-terminal peptide (PINP), a biochemical marker of collagen synthesis. A total of 105 treatment cycles of 58 patients with prostate cancer stages ≥pT2 was studied assessing testosterone, PSA and PINP levels at monthly intervals. During phases of AS lasting for up to nine months PSA levels were reversibly reduced, indicating apoptotic regression of the prostatic tumors. Within the first cycle PINP increased at the end of the AS period and peaked in the treatment cessation phase. During the following two cycles a similar pattern was observed for PINP, except a break in collagen synthesis as indicated by low PINP levels in the first months off treatment. Therefore, measurements of the serum PINP concentration indicated increased bone matrix synthesis in response to >6 months of AS, which uninterruptedly continued into the first treatment cessation phase, with a break into each of the following two pauses. In summary, synthesis of bone matrix collagen increases while degradation decreases during off-treatment phases in patients undergoing IAS. Although a direct relationship between bone matrix turnover and risk of fractures is difficult to establish, IAS for treatment of biochemical progression of prostate tumors is expected to reduce osteoporosis in elderly men often at high risk for bone fractures representing a highly suitable patient population for this kind of therapy.

  6. Phase-assisted synthesis and DNA unpacking evaluation of biologically inspired metallo nanocomplexes using peptide as unique building block.

    Science.gov (United States)

    Raman, N; Sudharsan, S

    2011-12-01

    The goal of nanomaterials' surface modification using a biomaterial is to preserve the materials' bulk properties while modifying only their surface to possess desired recognition and specificity. Here, we have developed a phase-assisted, modified Brust-Schiffrin methodological synthesis of metallo nanocomplexes anchored by a peptide, N,N'-(1,3-propylene)-bis-hippuricamide. The spectral, thermal and morphological characterizations assure the formation of nanocomplexes. Therapeutic behavior of all the nanocomplexes has been well sighted by evaluating their DNA unpacking skills. In addition, we demonstrate their biological inspiration by targeting few bacterial and fungal strains. The in vitro antimicrobial investigation reports that all the nanocomplexes disrupt microbial cell walls/membranes efficiently and inhibit the growth of microbes. These sorts of nanocomplexes synthesized in large quantities and at low cost, deliver versatile biomedical applications, and can be used to treat various diseases which may often cause high mortality. Copyright © 2011 Elsevier Inc. All rights reserved.

  7. Direct synthesis of nanocrystalline oxide powders by wet-chemical techniques

    Directory of Open Access Journals (Sweden)

    Vladimir V. Srdić

    2010-09-01

    Full Text Available In a recent period there is a great need for increasing the knowledge of tailoring the innovative procedures for the synthesis of electroceramic nanopowders and materials with improved quality for specific application. In order to produce electroceramics with desirable microstructure and properties, synthesis of stoichiometric, ultra-fine and agglomerate free powders with narrow size distributions is one of the most important steps. Within this scope, in the present paper we summarize our recent results on direct synthesis of some important perovskites and ferrites nanopowders by wet-chemical techniques.

  8. Synthesis of Reusable Silica Nanosphere-Supported Pt(IV Complex for Formation of Disulfide Bonds in Peptides

    Directory of Open Access Journals (Sweden)

    Xiaonan Hou

    2017-02-01

    Full Text Available Some peptide-based drugs, including oxytocin, vasopressin, ziconotide, pramlintide, nesiritide, and octreotide, contain one intramolecular disulfide bond. A novel and reusable monodispersed silica nanosphere-supported Pt(IV complex (SiO2@TPEA@Pt(IV; TPEA: N-[3-(trimethoxysilylpropyl]ethylenediamine was synthesized via a four-step procedure and was used for the formation of intramolecular disulfide bonds in peptides. Transmission electron microscopy (TEM and chemical mapping results for the Pt(II intermediates and for SiO2@TPEA@Pt(IV show that the silica nanospheres possess a monodisperse spherical structure and contain uniformly-distributed Si, O, C, N, Cl, and Pt. The valence state of Pt on the silica nanospheres was characterized by X-ray photoelectron spectroscopy (XPS. The Pt(IV loaded on SiO2@TPEA@Pt(IV was 0.15 mmol/g, as determined by UV-VIS spectrometry. The formation of intramolecular disulfides in six dithiol-containing peptides of variable lengths by the use of SiO2@TPEA@Pt(IV was investigated, and the relative oxidation yields were determined by high-performance liquid chromatography (HPLC. In addition, peptide 1 (Ac-CPFC-NH2 was utilized to study the reusability of SiO2@TPEA@Pt(IV. No significant decrease in the relative oxidation yield was observed after ten reaction cycles. Moreover, the structure of SiO2@TPEA@Pt(IV after being used for ten cycles was determined to be similar to its initial one, demonstrating the cycling stability of the complex.

  9. Synthesis of stable isotopically labeled peptides with filter-assisted enzymatic labeling for the diagnosis of hepatitis B virus infection utilizing mass spectrometry-based proteomics strategy

    International Nuclear Information System (INIS)

    Tsai, Hsing-Fen; Hsiao, He-Hsuan

    2017-01-01

    A facile method for the preparation of stable isotopically labeled peptides was developed by means of filter-assisted tryptic "1"6O/"1"8O water labeling, which could be directly applied to the determination of hepatitis B virus infection from human serum with tandem mass spectrometry. Tryptic peptides of hepatitis B surface antigen or hepatitis B e antigen from different subtypes of hepatitis B virus were synthesized with traditional solid-phase peptide synthesis as potential biomarkers. Trypsin catalyzed oxygen-18 exchange at their amidated c-terminus of arginine or lysine residue. The protease catalyzed oxygen-18 to oxygen-16 back exchange reaction was eliminated due to the complete removal of trypsin by the centrifugal filter containing a thin membrane associated with molecular weight cut-off of 10 KDa. The synthetic isotopic peptides were spiked into trichloroacetic acid/acetone precipitated human serum as internal standards and were selectively detected with multiplexed parallel reaction monitoring on a hybrid quadrupole-orbitrap mass spectrometer. The limit of detection for all synthetic peptides were in the range of 0.09 fmol–1.13 fmol. The results indicated that the peptide YLWEWASVR derived from hepatitis B surface antigen was quantified approximately 200 fmol per μl serum and may serve as a diagnostic biomarker for the detection of hepatitis B virus infected disease. - Highlights: • Facile synthesis of an inexpensive and highly reproducible stable isotopically labeled peptides. • Complete incorporation of two "1"8O atoms into synthesized peptides with filter-assisted enzymatic labeling. • Targeted analysis with parallel reaction monitoring assay for the disease diagnosis.

  10. Synthesis of stable isotopically labeled peptides with filter-assisted enzymatic labeling for the diagnosis of hepatitis B virus infection utilizing mass spectrometry-based proteomics strategy

    Energy Technology Data Exchange (ETDEWEB)

    Tsai, Hsing-Fen; Hsiao, He-Hsuan, E-mail: hhhsiao@dragon.nchu.edu.tw

    2017-03-01

    A facile method for the preparation of stable isotopically labeled peptides was developed by means of filter-assisted tryptic {sup 16}O/{sup 18}O water labeling, which could be directly applied to the determination of hepatitis B virus infection from human serum with tandem mass spectrometry. Tryptic peptides of hepatitis B surface antigen or hepatitis B e antigen from different subtypes of hepatitis B virus were synthesized with traditional solid-phase peptide synthesis as potential biomarkers. Trypsin catalyzed oxygen-18 exchange at their amidated c-terminus of arginine or lysine residue. The protease catalyzed oxygen-18 to oxygen-16 back exchange reaction was eliminated due to the complete removal of trypsin by the centrifugal filter containing a thin membrane associated with molecular weight cut-off of 10 KDa. The synthetic isotopic peptides were spiked into trichloroacetic acid/acetone precipitated human serum as internal standards and were selectively detected with multiplexed parallel reaction monitoring on a hybrid quadrupole-orbitrap mass spectrometer. The limit of detection for all synthetic peptides were in the range of 0.09 fmol–1.13 fmol. The results indicated that the peptide YLWEWASVR derived from hepatitis B surface antigen was quantified approximately 200 fmol per μl serum and may serve as a diagnostic biomarker for the detection of hepatitis B virus infected disease. - Highlights: • Facile synthesis of an inexpensive and highly reproducible stable isotopically labeled peptides. • Complete incorporation of two {sup 18}O atoms into synthesized peptides with filter-assisted enzymatic labeling. • Targeted analysis with parallel reaction monitoring assay for the disease diagnosis.

  11. Identification, characterization, and synthesis of peptide epitopes and a recombinant six-epitope protein for Trichomonas vaginalis serodiagnosis

    Directory of Open Access Journals (Sweden)

    Alderete JF

    2013-08-01

    Full Text Available J F Alderete, Calvin J NeaceSchool of Molecular Biosciences, College of Veterinary Medicine, Washington State University, Pullman, WA, USAAbstract: There is a need for a rapid, accurate serodiagnostic test useful for both women and men infected by Trichomonas vaginalis, which causes the number one sexually transmitted infection (STI. Women and men exposed to T. vaginalis make serum antibody to fructose-1,6-bisphosphate aldolase (ALD, α-enolase (ENO, and glyceraldehyde-3-phosphate dehydrogenase (GAP. We identified, by epitope mapping, the common and distinct epitopes of each protein detected by the sera of women patients with trichomonosis and by the sera of men highly seropositive to the immunogenic protein α-actinin (positive control sera. We analyzed the amino acid sequences to determine the extent of identity of the epitopes of each protein with other proteins in the databanks. This approach identified epitopes unique to T. vaginalis, indicating these peptide-epitopes as possible targets for a serodiagnostic test. Individual or combinations of 15-mer peptide epitopes with low to no identity with other proteins were reactive with positive control sera from both women and men but were unreactive with negative control sera. These analyses permitted the synthesis of a recombinant His6 fusion protein of 111 amino acids with an Mr of ~13.4 kDa, which consisted of 15-mer peptides of two distinct epitopes each for ALD, ENO, and GAP. This recombinant protein was purified by affinity chromatography. This composite protein was detected by enzyme-linked immunosorbent assay (ELISA, dot blots, and immunoblots, using positive control sera from women and men. These data indicate that it is possible to identify epitopes and that either singly, in combination, or as a composite protein represent targets for a point-of-care serodiagnostic test for T. vaginalis.Keywords: diagnostics, point-of-care, targets, trichomonosis

  12. High-flexibility combinatorial peptide synthesis with laser-based transfer of monomers in solid matrix material.

    Science.gov (United States)

    Loeffler, Felix F; Foertsch, Tobias C; Popov, Roman; Mattes, Daniela S; Schlageter, Martin; Sedlmayr, Martyna; Ridder, Barbara; Dang, Florian-Xuan; von Bojničić-Kninski, Clemens; Weber, Laura K; Fischer, Andrea; Greifenstein, Juliane; Bykovskaya, Valentina; Buliev, Ivan; Bischoff, F Ralf; Hahn, Lothar; Meier, Michael A R; Bräse, Stefan; Powell, Annie K; Balaban, Teodor Silviu; Breitling, Frank; Nesterov-Mueller, Alexander

    2016-06-14

    Laser writing is used to structure surfaces in many different ways in materials and life sciences. However, combinatorial patterning applications are still limited. Here we present a method for cost-efficient combinatorial synthesis of very-high-density peptide arrays with natural and synthetic monomers. A laser automatically transfers nanometre-thin solid material spots from different donor slides to an acceptor. Each donor bears a thin polymer film, embedding one type of monomer. Coupling occurs in a separate heating step, where the matrix becomes viscous and building blocks diffuse and couple to the acceptor surface. Furthermore, we can consecutively deposit two material layers of activation reagents and amino acids. Subsequent heat-induced mixing facilitates an in situ activation and coupling of the monomers. This allows us to incorporate building blocks with click chemistry compatibility or a large variety of commercially available non-activated, for example, posttranslationally modified building blocks into the array's peptides with >17,000 spots per cm(2).

  13. Immunoregulatory activities of human immunodeficiency virus (HIV) proteins: Effect of HIV recombinant and synthetic peptides on immunoglobulin synthesis and proliferative responses by normal lymphocytes

    International Nuclear Information System (INIS)

    Nair, M.P.N.; Pottathil, R.; Heimer, E.P.; Schwartz, S.A.

    1988-01-01

    Recombinant and synthetic peptides corresponding to envelope proteins of the human immunodeficiency virus (HIV) were examined for their effects on the activities of lymphocytes from normal donors in vitro. Although lymphocytes cultured with env-gag peptides produced significant amounts of IgG, addition of env-gag peptides to a pokeweed mitogen-induced B-cell activation system resulted in suppression of immunoglobulin synthesis by normal lymphocytes. Recombinant antigens, env-gag and env-80 dihydrofolate reductase (DHFR), produced a substantial proliferative response by peripheral blood mononuclear cells (PBMC) as determined by [ 3 H]thymidine incorporation. PBMC precultured with HIV synthetic peptide env 578-608 also manifested significant proliferative responses as compared to control cultures. CD3 + lymphocytes precultured with recombinant HIV antigens, env-gag and env-80 DHFR, and synthetic HIV peptide, env 487-511, showed moderate but significant proliferative responses. Both recombinant antigens and synthetic peptides also produced a dose-dependent stimulatory effect on proliferation by CD3 - lymphocytes. These studies demonstrate that recombinant and synthetic peptides of the HIV genome express immunoregulatory T- and B-cell epitopes. Identification of unique HIV epitopes with immunogenic and immunoregulatory activities is necessary for the development of an effective vaccine against HIV infection

  14. “Miswak” Based Green Synthesis of Silver Nanoparticles: Evaluation and Comparison of Their Microbicidal Activities with the Chemical Synthesis

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2016-11-01

    Full Text Available Microbicidal potential of silver nanoparticles (Ag-NPs can be drastically improved by improving their solubility or wettability in the aqueous medium. In the present study, we report the synthesis of both green and chemical synthesis of Ag-NPs, and evaluate the effect of the dispersion qualities of as-prepared Ag-NPs from both methods on their antimicrobial activities. The green synthesis of Ag-NPs is carried out by using an aqueous solution of readily available Salvadora persica L. root extract (RE as a bioreductant. The formation of highly crystalline Ag-NPs was established by various analytical and microscopic techniques. The rich phenolic contents of S. persica L. RE (Miswak not only promoted the reduction and formation of NPs but they also facilitated the stabilization of the Ag-NPs, which was established by Fourier transform infrared spectroscopy (FT-IR analysis. Furthermore, the influence of the volume of the RE on the size and the dispersion qualities of the NPs was also evaluated. It was revealed that with increasing the volume of RE the size of the NPs was deteriorated, whereas at lower concentrations of RE smaller size and less aggregated NPs were obtained. During this study, the antimicrobial activities of both chemically and green synthesized Ag-NPs, along with the aqueous RE of S. persica L., were evaluated against various microorganisms. It was observed that the green synthesized Ag-NPs exhibit comparable or slightly higher antibacterial activities than the chemically obtained Ag-NPs.

  15. Multiarm-polyethylene glycol-polyglutamic acid peptide dendrimer: Design, synthesis, and dissolving thrombus.

    Science.gov (United States)

    Zhang, Shao-Fei; Lü, Shaoyu; Gao, Chunmei; Yang, Jiandong; Yan, Xiang; Li, Tao; Wen, Na; Huang, Mengjie; Liu, Mingzhu

    2018-06-01

    Thrombotic events affect many individuals in a number of ways, all of which can cause significant morbidity and mortality. Nattokinase (NK), as a novel thrombolytic drug, has been used for thrombolytic therapy. It not only possesses plasminogen activator activity, but also directly digests fibrin through limited proteolysis. However, it may undergo inactivation and denaturation in the harsh external environment. In this study, a multiarm-polyethylene glycol-polyglutamic acid peptide dendrimer was fabricated and used as a carrier for NK protection and delivery. Different arm numbers of polyethylene glycol-polyglutamic acid peptide dendrimers (x-PEG(G 3 ) x , x = 2, 4, 6, 8) were designed, prepared, and characterized by 1 H NMR and FTIR. Then, x-PEG(G 3 ) x were loaded with NK to form nanocomposites. Their size and morphology were determined by dynamic light scattering and transmission electron microscopy. Enzyme activity was evaluated via UV-Vis absorbance spectra, fluorescence spectra, circular dichroism spectra, and zeta potential measurements. The study reveals that the obtained x-PEG(G 3 ) x /NK nanocomposites possess high enzyme activity. In addition, the nanocomposites show increased viability of rat macrophage cells, and excellent thrombolysis ability in vitro and in vivo. This work establishes a multiarm-polyethylene glycol-polyglutamic acid peptide dendrimer with potential application in NK carrier and thrombolytic therapy. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 1687-1696, 2018. © 2018 Wiley Periodicals, Inc.

  16. Design and synthesis of multiple antigenic peptides and their application for dengue diagnosis.

    Science.gov (United States)

    Rai, Reeta; Dubey, Sameer; Santosh, K V; Biswas, Ashutosh; Mehrotra, Vinit; Rao, D N

    2017-09-01

    Major difficulty in development of dengue diagnostics is availability of suitable antigens. To overcome this, we made an attempt to develop a peptide based diagnosis which offers significant advantage over other methods. With the help of in silico methods, two epitopes were selected from envelope protein and three from NS1 protein of dengue virus. These were synthesized in combination as three multiple antigenic peptides (MAPs). We have tested 157 dengue positive sera confirmed for NS1 antigen. MAP1 showed 96.81% sera positive for IgM and 68.15% positive for IgG. MAP2 detected 94.90% IgM and 59.23% IgG positive sera. MAP3 also detected 96.17% IgM and 59.87% IgG positive sera. To the best of our knowledge this is the first study describing the use of synthetic multiple antigenic peptides for the diagnosis of dengue infection. This study describes MAPs as a promising tool for the use in serodiagnosis of dengue. Copyright © 2017 International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

  17. Characterization of a novel androgen receptor (AR) coregulator RIPK1 and related chemicals that suppress AR-mediated prostate cancer growth via peptide and chemical screening.

    Science.gov (United States)

    Hsu, Cheng-Lung; Liu, Jai-Shin; Lin, Ting-Wei; Chang, Ying-Hsu; Kuo, Yung-Chia; Lin, An-Chi; Ting, Huei-Ju; Pang, See-Tong; Lee, Li-Yu; Ma, Wen-Lung; Lin, Chun-Cheng; Wu, Wen-Guey

    2017-09-19

    Using bicalutamide-androgen receptor (AR) DNA binding domain-ligand binding domain as bait, we observed enrichment of FxxFY motif-containing peptides. Protein database searches revealed the presence of receptor-interacting protein kinase 1 (RIPK1) harboring one FxxFY motif. RIPK1 interacted directly with AR and suppressed AR transactivation in a dose-dependent manner. Domain mapping experiments showed that the FxxFY motif in RIPK1 is critical for interactions with AR and the death domain of RIPK1 plays a crucial role in its inhibitory effect on transactivation. In terms of tissue expression, RIPK1 levels were markedly higher in benign prostate hyperplasia and non-cancerous tissue regions relative to the tumor area. With the aid of computer modeling for screening of chemicals targeting activation function 2 (AF-2) of AR, we identified oxadiazole derivatives as good candidates and subsequently generated a small library of these compounds. A number of candidates could effectively suppress AR transactivation and AR-related functions in vitro and in vivo with tolerable toxicity via inhibiting AR-peptide, AR-coregulator and AR N-C interactions. Combination of these chemicals with antiandrogen had an additive suppressive effect on AR transcriptional activity. Our collective findings may pave the way in creating new strategies for the development and design of anti-AR drugs.

  18. Synthesis of chiral polyaniline films via chemical vapor phase polymerization

    DEFF Research Database (Denmark)

    Chen, J.; Winther-Jensen, B.; Pornputtkul, Y.

    2006-01-01

    Electrically and optically active polyaniline films doped with (1)-(-)-10- camphorsulfonic acid were successfully deposited on nonconductive substrates via chemical vapor phase polymerization. The above polyaniline/ R- camphorsulfonate films were characterized by electrochemical and physical...

  19. Chemical equilibrium of glycerol carbonate synthesis from glycerol

    International Nuclear Information System (INIS)

    Li Jiabo; Wang Tao

    2011-01-01

    Research highlights: → Transesterification of glycerol with cyclic carbonates or alkyl carbonates is thermodynamically favourable for the preparation of glycerol carbonate from glycerol. → The reaction of glycerol and carbon dioxide is thermodynamically limited. → High temperature and low pressure is favourable to the reaction of glycerol and urea. → Increasing temperature can increase the chemical equilibrium constant for the reaction of glycerol and dimethyl carbonate. → For the reaction of glycerol and ethylene carbonate, increasing temperature can decrease the chemical equilibrium constant. - Abstract: In this paper, the chemical equilibrium for the glycerol carbonate preparation from glycerol was investigated. The chemical equilibrium constants were calculated for the reactions to produce glycerol carbonate from glycerol. The theoretical calculation was compared with the experimental results for the transesterification of glycerol with dimethyl carbonate. Transesterification of glycerol with cyclic carbonates or alkyl carbonates is thermodynamically favourable for producing glycerol carbonate from glycerol according to the equilibrium constant. Increasing temperature can increase the chemical equilibrium constant for the reaction of glycerol with dimethyl carbonate. For the reaction of glycerol with ethylene carbonate, increasing temperature can decrease the chemical equilibrium constant. The reaction of glycerol with carbon dioxide is thermodynamically limited. High temperature and low pressure are favourable to the reaction of glycerol and urea.

  20. Expression, stabilization and purification of membrane proteins via diverse protein synthesis systems and detergents involving cell-free associated with self-assembly peptide surfactants.

    Science.gov (United States)

    Zheng, Xuan; Dong, Shuangshuang; Zheng, Jie; Li, Duanhua; Li, Feng; Luo, Zhongli

    2014-01-01

    G-protein coupled receptors (GPCRs) are involved in regulating most of physiological actions and metabolism in the bodies, which have become most frequently addressed therapeutic targets for various disorders and diseases. Purified GPCR-based drug discoveries have become routine that approaches to structural study, novel biophysical and biochemical function analyses. However, several bottlenecks that GPCR-directed drugs need to conquer the problems including overexpression, solubilization, and purification as well as stabilization. The breakthroughs are to obtain efficient protein yield and stabilize their functional conformation which are both urgently requiring of effective protein synthesis system methods and optimal surfactants. Cell-free protein synthesis system is superior to the high yields and post-translation modifications, and early signs of self-assembly peptide detergents also emerged to superiority in purification of membrane proteins. We herein focus several predominant protein synthesis systems and surfactants involving the novel peptide detergents, and uncover the advantages of cell-free protein synthesis system with self-assembling peptide detergents in purification of functional GPCRs. This review is useful to further study in membrane proteins as well as the new drug exploration. Copyright © 2014 Elsevier Inc. All rights reserved.

  1. Phosphorus-containing cyclodextrins. Characteristics of the synthesis and chemical behaviour

    International Nuclear Information System (INIS)

    Grachev, M K

    2013-01-01

    Published data on the preparation of phosphorus-containing cyclodextrins are summarized. It is demonstrated that some significant features of their synthesis and chemical behaviour are caused by specific supramolecular interactions involving the inner chiral cavity of cyclodextrins capable of incorporating various guests, which often leads to alteration of customary routes of chemical transformations. The possibilities of practical applications of phosphorus-containing cyclodextrins are briefly analyzed. The bibliography includes 89 references

  2. Applications of Process Synthesis: Moving from Conventional Chemical Processes towards Biorefinery Processes

    DEFF Research Database (Denmark)

    Yuan, Zhihong; Chen, Bingzhen; Gani, Rafiqul

    2013-01-01

    Concerns about diminishing petroleum reserves, enhanced worldwide demand for fuels and fluctuations in the global oil market, together with climate change and national security have promoted many initiatives for exploring alternative, non-petroleum based processes. Among these initiatives......, biorefinery processes for converting biomass-derived carbohydrates into transportation fuels and chemicals are now gaining more and more attention from both academia and industry. Process synthesis, which has played a vital role for the development, design and operation of (petro) chemical processes, can...

  3. Activation of aluminum as an effective reducing agent by pitting corrosion for wet-chemical synthesis.

    Science.gov (United States)

    Li, Wei; Cochell, Thomas; Manthiram, Arumugam

    2013-01-01

    Metallic aluminum (Al) is of interest as a reducing agent because of its low standard reduction potential. However, its surface is invariably covered with a dense aluminum oxide film, which prevents its effective use as a reducing agent in wet-chemical synthesis. Pitting corrosion, known as an undesired reaction destroying Al and is enhanced by anions such as F⁻, Cl⁻, and Br⁻ in aqueous solutions, is applied here for the first time to activate Al as a reducing agent for wet-chemical synthesis of a diverse array of metals and alloys. Specifically, we demonstrate the synthesis of highly dispersed palladium nanoparticles on carbon black with stabilizers and the intermetallic Cu₂Sb/C, which are promising candidates, respectively, for fuel cell catalysts and lithium-ion battery anodes. Atomic hydrogen, an intermediate during the pitting corrosion of Al in protonic solvents (e.g., water and ethylene glycol), is validated as the actual reducing agent.

  4. Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

    CSIR Research Space (South Africa)

    Motlatle, Abesach M

    2016-10-01

    Full Text Available of Nanoparticle Research, vol. 18: DOI: 10.1007/s11051-016-3614-8 Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles Motlatle AM Kesevan Pillai S Scriba MR Ray SS ABSTRACT: Cu...

  5. A wet-chemical approach to perovskite and fluorite-type nanoceramics: synthesis and processing

    NARCIS (Netherlands)

    Veldhuis, Sjoerd

    2015-01-01

    In thesis the low-temperature, wet-chemical approach to various functional inorganic oxide materials is described. The main focus of this research is to control the material’s synthesis from liquid precursor to metal oxide powder or thin film; while understanding its formation mechanism. In

  6. Facile Synthesis of Magnetic Mesoporous Hollow Carbon Microspheres for Rapid Capture of Low-Concentration Peptides

    OpenAIRE

    Cheng, Gong; Zhou, Ming-Da; Zheng, Si-Yang

    2014-01-01

    Mesoporous and hollow carbon microspheres embedded with magnetic nanoparticles (denoted as MHM) were prepared via a facile self-sacrificial method for rapid capture of low-abundant peptides from complex biological samples. The morphology, structure, surface property, and magnetism were well-characterized. The hollow magnetic carbon microspheres have a saturation magnetization value of 130.2 emu g?1 at room temperature and a Brunauer?Emmett?Teller specific surface area of 48.8 m2 g?1 with an a...

  7. Synthesis of graphene platelets by chemical and electrochemical route

    Energy Technology Data Exchange (ETDEWEB)

    Ramachandran, Rajendran; Felix, Sathiyanathan [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Joshi, Girish M. [Materials Physics Division, School of Advanced Sciences, VIT University, Vellore 632014, Tamil Nadu (India); Raghupathy, Bala P.C., E-mail: balapraveen2000@yahoo.com [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Research and Advanced Engineering Division (Materials), Renault Nissan Technology and Business Center India (P) Ltd., Chennai, Tamil Nadu (India); Jeong, Soon Kwan, E-mail: jeongsk@kier.re.kr [Climate Change Technology Research Division, Korea Institute of Energy Research, Yuseong-gu, Daejeon 305-343 (Korea, Republic of); Grace, Andrews Nirmala, E-mail: anirmalagrace@vit.ac.in [Centre for Nanotechnology Research, VIT University, Vellore 632014, Tamil Nadu (India); Climate Change Technology Research Division, Korea Institute of Energy Research, Yuseong-gu, Daejeon 305-343 (Korea, Republic of)

    2013-10-15

    Graphical abstract: A schematic showing the overall reduction process of graphite to reduced graphene platelets by chemical and electrochemical route. - Highlights: • Graphene was prepared by diverse routes viz. chemical and electrochemical methods. • NaBH{sub 4} was effective for removing oxygen functional groups from graphene oxide. • Sodium borohydride reduced graphene oxide (SRGO) showed high specific capacitance. • Electrochemical rendered a cheap route for production of graphene in powder form. - Abstract: Graphene platelets were synthesized from graphene oxide by chemical and electrochemical route. Under the chemical method, sodium borohydride and hydrazine chloride were used as reductants to produce graphene. In this paper, a novel and cost effective electrochemical method, which can simplify the process of reduction on a larger scale, is demonstrated. The electrochemical method proposed in this paper produces graphene in powder form with good yield. The atomic force microscopic images confirmed that the graphene samples prepared by all the routes have multilayers of graphene. The electrochemical process provided a new route to make relatively larger area graphene sheets, which will have interest for further patterning applications. Attempt was made to quantify the quantum of reduction using cyclic voltammetry and choronopotentiometry techniques on reduced graphene samples. As a measure in reading the specific capacitance values, a maximum specific capacitance value of 265.3 F/g was obtained in sodium borohydride reduced graphene oxide.

  8. Application of mechano-chemical synthesis for protective coating

    Indian Academy of Sciences (India)

    This can either be prevented by using grinding medium and container of same material of the milled material or by adding a coating of the milled material on them. The paper describes the observations made during a mechano-chemical reaction, being used for coating the balls and vials in a planetary ball mill.

  9. Synthesis of graphene platelets by chemical and electrochemical route

    International Nuclear Information System (INIS)

    Ramachandran, Rajendran; Felix, Sathiyanathan; Joshi, Girish M.; Raghupathy, Bala P.C.; Jeong, Soon Kwan; Grace, Andrews Nirmala

    2013-01-01

    Graphical abstract: A schematic showing the overall reduction process of graphite to reduced graphene platelets by chemical and electrochemical route. - Highlights: • Graphene was prepared by diverse routes viz. chemical and electrochemical methods. • NaBH 4 was effective for removing oxygen functional groups from graphene oxide. • Sodium borohydride reduced graphene oxide (SRGO) showed high specific capacitance. • Electrochemical rendered a cheap route for production of graphene in powder form. - Abstract: Graphene platelets were synthesized from graphene oxide by chemical and electrochemical route. Under the chemical method, sodium borohydride and hydrazine chloride were used as reductants to produce graphene. In this paper, a novel and cost effective electrochemical method, which can simplify the process of reduction on a larger scale, is demonstrated. The electrochemical method proposed in this paper produces graphene in powder form with good yield. The atomic force microscopic images confirmed that the graphene samples prepared by all the routes have multilayers of graphene. The electrochemical process provided a new route to make relatively larger area graphene sheets, which will have interest for further patterning applications. Attempt was made to quantify the quantum of reduction using cyclic voltammetry and choronopotentiometry techniques on reduced graphene samples. As a measure in reading the specific capacitance values, a maximum specific capacitance value of 265.3 F/g was obtained in sodium borohydride reduced graphene oxide

  10. A chemical platform approach on cardanol oil: from the synthesis of building blocks to polymer synthesis

    Directory of Open Access Journals (Sweden)

    Jaillet Fanny

    2016-09-01

    Full Text Available This review proposes a platform approach for the synthesis of various building blocks from cardanol oil in one or two-steps synthesis. Cardanol is a natural phenol issued from Cashew nutshell liquid (CNSL. CNSL is a non-edible renewable resource, co-produced from cashew industry in large commercial volumes. Cardanol is non-toxic and particularly suitable as an aromatic renewable resource for polymers and materials. Various routes were used for the synthesis of di- and poly-functional building blocks used thereafter in polymer syntheses. Phenolation was used to dimerize/oligomerize cardanol to propose increase functionality of cardanol. Thio-ene was used to synthesize new reactive amines. Epoxidation and (methacrylation were also used to insert oxirane or (methacrylate groups in order to synthesize polymers and materials.

  11. Design, synthesis and in vitro evaluation of heterobivalent peptidic radioligands targeting both GRP- and VPAC1-Receptors concomitantly overexpressed on various malignancies - Is the concept feasible?

    Science.gov (United States)

    Lindner, Simon; Fiedler, Luise; Wängler, Björn; Bartenstein, Peter; Schirrmacher, Ralf; Wängler, Carmen

    2018-05-29

    Radiolabeled heterobivalent peptidic ligands (HBPLs), being able to address different receptors, are highly interesting tumor imaging agents as they can offer multiple advantages over monovalent peptide receptor ligands. However, few examples of radiolabeled HBPLs have been described so far. One promising approach is the combination of gastrin-releasing peptide receptor (GRPR)- and vasoactive intestinal peptide receptor subtype 1 (VPAC 1 R)-targeting peptides into one single radioligand since gastrinomas, prostate and breast cancer have been shown to concomitantly or complementarily overexpress both receptors. Here we report the design and synthesis of different HBPLs, comprising a GRPR-binding (BBN 7-14 ) and a VPAC 1 R-targeting (PACAP-27) peptide. The heterodimers were varied with regard to the distance between the peptide binders and the steric rigidity of the systems. We radiolabeled the HBPLs 19-23 as well as their monomeric reference standards 26 and 27 with 68 Ga, achieving radiochemical yields and purities of 95-99% and non-optimized molar activities of 25-61 GBq/μmol. We tested the stability of the radioligands and further evaluated them in vitro regarding their uptake in different prostate carcinoma cell lines (PC-3, DU-145 and VCaP cells). We found that the heterobivalent substances [ 68 Ga]19 - [ 68 Ga]23 showed comparable uptakes into the tumor cells to those of the respective monomers [ 68 Ga]26 and [ 68 Ga]27, indicating that both peptides are still able to address their target receptors. Furthermore, the obtained results indicate that in case of overall low receptor densities, heterobivalent peptides surpass peptide monomers in tumor cell uptake. Most importantly, it could be shown by blocking studies that both peptide parts of the HBPL [ 68 Ga]19 contributed to tumor cell uptake in VCaP cells, expressing both receptor types. Thus, we describe here the first examples of HBPLs being able to address the GRPR as well as the VPAC 1 R and have the

  12. Analysing chemical equilibrium conditions when studying butyl acetate synthesis

    OpenAIRE

    Álvaro Orjuela Londoño; Fernando Leiva Lenis; Luis Alejandro Boyacá Mendivelso; Gerardo Rodríguez Niño; Luis María Carballo Suárez

    2010-01-01

    This work studied the liquid phase of acetic acid and butyl alcohol esterification reaction (P atm = 560 mmHg),using an ion exchange resin (Lewatit K-2431) as catalyst. A set of assays were carried out for determining the effect of catalyst load, temperature and molar ratio (acid/alcohol) on chemical equilibrium constant. Components’ selective sorption on the resin matrix was noticed; its effect on equilibrium conditions was verified, by using different acid/alcohol starting ratios. A non-ide...

  13. Nanostructured conjugated polymers in chemical sensors: synthesis, properties and applications.

    Science.gov (United States)

    Correa, D S; Medeiros, E S; Oliveira, J E; Paterno, L G; Mattoso, Luiz C

    2014-09-01

    Conjugated polymers are organic materials endowed with a π-electron conjugation along the polymer backbone that present appealing electrical and optical properties for technological applications. By using conjugated polymeric materials in the nanoscale, such properties can be further enhanced. In addition, the use of nanostructured materials makes possible miniaturize devices at the micro/nano scale. The applications of conjugated nanostructured polymers include sensors, actuators, flexible displays, discrete electronic devices, and smart fabric, to name a few. In particular, the use of conjugated polymers in chemical and biological sensors is made feasible owning to their sensitivity to the physicochemical conditions of its surrounding environment, such as chemical composition, pH, dielectric constant, humidity or even temperature. Subtle changes in these conditions bring about variations on the electrical (resistivity and capacitance), optical (absorptivity, luminescence, etc.), and mechanical properties of the conjugated polymer, which can be precisely measured by different experimental methods and ultimately associated with a specific analyte and its concentration. The present review article highlights the main features of conjugated polymers that make them suitable for chemical sensors. An especial emphasis is given to nanostructured sensors systems, which present high sensitivity and selectivity, and find application in beverage and food quality control, pharmaceutical industries, medical diagnosis, environmental monitoring, and homeland security, and other applications as discussed throughout this review.

  14. Mapping the dark space of chemical reactions with extended nanomole synthesis and MALDI-TOF MS.

    Science.gov (United States)

    Lin, Shishi; Dikler, Sergei; Blincoe, William D; Ferguson, Ronald D; Sheridan, Robert P; Peng, Zhengwei; Conway, Donald V; Zawatzky, Kerstin; Wang, Heather; Cernak, Tim; Davies, Ian W; DiRocco, Daniel A; Sheng, Huaming; Welch, Christopher J; Dreher, Spencer D

    2018-05-24

    Understanding the practical limitations of chemical reactions is critically important for efficiently planning the synthesis of compounds in pharmaceutical, agrochemical and specialty chemical research and development. However, literature reports of the scope of new reactions are often cursory and biased toward successful results, severely limiting the ability to predict reaction outcomes for untested substrates. We herein illustrate strategies for carrying out large scale surveys of chemical reactivity using a material-sparing nanomole-scale automated synthesis platform with greatly expanded synthetic scope combined with ultra-high throughput (uHT) matrix assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS). Copyright © 2018, American Association for the Advancement of Science.

  15. Design, synthesis, and validation of a β-turn mimetic library targeting protein-protein and peptide-receptor interactions.

    Science.gov (United States)

    Whitby, Landon R; Ando, Yoshio; Setola, Vincent; Vogt, Peter K; Roth, Bryan L; Boger, Dale L

    2011-07-06

    The design and synthesis of a β-turn mimetic library as a key component of a small-molecule library targeting the major recognition motifs involved in protein-protein interactions is described. Analysis of a geometric characterization of 10,245 β-turns in the protein data bank (PDB) suggested that trans-pyrrolidine-3,4-dicarboxamide could serve as an effective and synthetically accessible library template. This was confirmed by initially screening select compounds against a series of peptide-activated GPCRs that recognize a β-turn structure in their endogenous ligands. This validation study was highlighted by identification of both nonbasic and basic small molecules with high affinities (K(i) = 390 and 23 nM, respectively) for the κ-opioid receptor (KOR). Consistent with the screening capabilities of collaborators and following the design validation, the complete library was assembled as 210 mixtures of 20 compounds, providing a total of 4200 compounds designed to mimic all possible permutations of 3 of the 4 residues in a naturally occurring β-turn. Unique to the design and because of the C(2) symmetry of the template, a typical 20 × 20 × 20-mix (8000 compounds prepared as 400 mixtures of 20 compounds) needed to represent 20 variations in the side chains of three amino acid residues reduces to a 210 × 20-mix, thereby simplifying the library synthesis and subsequent screening. The library was prepared using a solution-phase synthetic protocol with liquid-liquid or liquid-solid extractions for purification and conducted on a scale that insures its long-term availability for screening campaigns. Screening the library against the human opioid receptors (KOR, MOR, and DOR) identified not only the activity of library members expected to mimic the opioid receptor peptide ligands but also additional side-chain combinations that provided enhanced receptor binding selectivities (>100-fold) and affinities (as low as K(i) = 80 nM for KOR). A key insight to emerge from

  16. Increased synthesis of heparin affin regulatory peptide in the perforant path lesioned mouse hippocampal formation

    DEFF Research Database (Denmark)

    Poulsen, F R; Lagord, C; Courty, J

    2000-01-01

    Heparin affin regulatory peptide (HARP), also known as pleiotrophin or heparin-binding growth-associated molecule, is a developmentally regulated extracellular matrix protein that induces cell proliferation and promotes neurite outgrowth in vitro as well as pre- and postsynaptic developmental...... differentiation in vivo. Here we have investigated the expression of HARP mRNA and protein in the perforant path lesioned C57B1/6 mouse hippocampal formation from 1 to 35 days after surgery. This type of lesion induces a dense anterograde and terminal axonal degeneration, activation of glial cells, and reactive...... axonal sprouting within the perforant path zones of the fascia dentata and hippocampus as well as axotomy-induced retrograde neuronal degeneration in the entorhinal cortex. Analysis of sham- and unoperated control mice showed that HARP mRNA is expressed in neurons and white and gray matter glial cells...

  17. The Chemical Basis for the Origin of the Genetic Code and the Process of Protein Synthesis

    Science.gov (United States)

    Lacey, James C., Jr.

    1990-01-01

    A model for the origin of protein synthesis. The essential features of the model are that 5'-AMP and perhaps other monoribonucleotides can serve as catalysts for the selective synthesis of L-based peptides. A unique set of characteristics of 5'-AMP is responsible for the selective catalysts and these characteristics are described in detail. The model involves the formation of diesters as intermediates and selectivity for use of the L-isomer occurs principally at the step of forming the diester. However, in the formation of acetyl phenylalanine-AMP monoester there is a selectivity for esterification by the D-isomer. Data showing this selectivity is presented. This selectivity for D-isomer disappears after the first step. The identity was confirmed of all four of possible diesters of acetyl-D- and -L phenylaline with 5'-AMP by nuclear magnetic resonance (NMR). The data using flourescence and NMR show the Trp ring can associate with the adenine ring more strongly when the D-isomer is in the 2' position than it can when in the 3' position. These same data also suggest a molecular mechanisim for the faster esterificaton of 5'-AMP by acetyl-D-phenylaline. Some new data is also presented on the possible structure of the 2' isomer of acetyl-D-tryptophan-AMP monoester. The HPLC elution times of all four possible acetyl diphenylalanine esters of 5'-AMP were studied, these peptidyl esters will be products in the studies of peptide formation on the ribose of 5'-AMP. Other studies were on the rate of synthesis and the identity of the product when producing 3'Ac-Phe-2'tBOC-Phe-AMP diester. HPLC purification and identification of this product were accomplished.

  18. Use of carbonates for biological and chemical synthesis

    Science.gov (United States)

    Rau, Gregory Hudson

    2014-09-09

    A system of using carbonates, especially water-insoluble or sparing soluble mineral carbonates, for maintaining or increasing dissolved inorganic carbon concentrations in aqueous media. In particular, the system generates concentrated dissolve inorganic carbon substrates for photosynthetic, chemosynthetic, or abiotic chemical production of carbonaceous or other compounds in solution. In some embodiments, the invention can also enhance the dissolution and retention of carbon dioxide in aqueous media, and can produce pH buffering capacity, metal ions, and heat, which can be beneficial to the preceding syntheses.

  19. Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

    International Nuclear Information System (INIS)

    Chongad, L S; Sharma, A; Banerjee, M; Jain, A

    2016-01-01

    Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H 2 S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD. (paper)

  20. Comparative study between bioapatite and synthetic hydroxyapatite obtained by chemical precipitation and mechanochemical synthesis

    International Nuclear Information System (INIS)

    Quispe M, J.; Moreno, M.; Montano, J.; Pillaca, M.; Guzman, A.; Cavero, A.; Arce, M.

    2009-01-01

    A comparative study between the inorganic component of a human bone tissue with respect of apatite synthesized by chemical precipitation, mechanochemical synthesis and a sample of commercial hidroxyapatite are shown. The samples were studied by X-ray diffraction, atomic absorption spectroscopy and Fourier transform infrared spectroscopy. The results show similar structural characteristics among all samples identifying that sample prepared by mechanochemical synthesis is a kind of hydroxyapatite which has substitutions of carbonate in its crystalline structure, similar to the inorganic component of bone tissue. (author).

  1. A Review of Carbon Nanomaterials’ Synthesis via the Chemical Vapor Deposition (CVD Method

    Directory of Open Access Journals (Sweden)

    Yehia M. Manawi

    2018-05-01

    Full Text Available Carbon nanomaterials have been extensively used in many applications owing to their unique thermal, electrical and mechanical properties. One of the prime challenges is the production of these nanomaterials on a large scale. This review paper summarizes the synthesis of various carbon nanomaterials via the chemical vapor deposition (CVD method. These carbon nanomaterials include fullerenes, carbon nanotubes (CNTs, carbon nanofibers (CNFs, graphene, carbide-derived carbon (CDC, carbon nano-onion (CNO and MXenes. Furthermore, current challenges in the synthesis and application of these nanomaterials are highlighted with suggested areas for future research.

  2. A Review of Carbon Nanomaterials’ Synthesis via the Chemical Vapor Deposition (CVD) Method

    Science.gov (United States)

    Manawi, Yehia M.; Samara, Ayman; Al-Ansari, Tareq; Atieh, Muataz A.

    2018-01-01

    Carbon nanomaterials have been extensively used in many applications owing to their unique thermal, electrical and mechanical properties. One of the prime challenges is the production of these nanomaterials on a large scale. This review paper summarizes the synthesis of various carbon nanomaterials via the chemical vapor deposition (CVD) method. These carbon nanomaterials include fullerenes, carbon nanotubes (CNTs), carbon nanofibers (CNFs), graphene, carbide-derived carbon (CDC), carbon nano-onion (CNO) and MXenes. Furthermore, current challenges in the synthesis and application of these nanomaterials are highlighted with suggested areas for future research. PMID:29772760

  3. Synthesis of biotinyl derivatives of peptide hormones and other biological materials

    International Nuclear Information System (INIS)

    Finn, F.M.; Hofmann, K.H.

    1985-01-01

    Methods for the preparation of biotinylated ligands for the avidin-biotin system are described. Also described are procedures for modifying and labelling avidin and for assessing the rate of dissociation of biotin derivatives from avidin. The most widely used procedure for introducing biotin into other molecules involves acylation with N-hydroxysuccinimido-biotinate. Experimental details are given for the synthesis of dethiobiotin, iminobiotin, and biotinylated ligands in which a 6-aminohexanoic acid spacer is interposed between the biotin or biotin derivative and the insulin molecule. The syntheses of biotinylated corticotropins are presented only in principle

  4. Chemical synthesis and stabilization of magnesium substituted brushite

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Donghyun [Department of Biomedical Engineering, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756 (Korea, Republic of); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Mechanical Engineering and Materials Sceince, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Chemical and Petroleum Engineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States)

    2010-08-30

    Hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) is the most ubiquitous calcium phosphate phase used in implant coatings and more recently in gene/drug delivery applications due to its chemical stability under normal physiological conditions (37 deg. C, pH {approx} 7.5, 1 atm.). However, different calcium phosphate phases, such as brushite (CaH(PO{sub 4}){center_dot}2(H{sub 2}O)) and tricalcium phosphate (Ca{sub 3}(PO{sub 4}){sub 2}) which are thermodynamically unstable under physiological conditions are also being explored for biomedical applications. One way of stabilizing these phases under physiological conditions is to introduce magnesium to substitute for calcium in the brushite lattice. The role of magnesium as a stabilizing agent for synthesizing brushite under physiological conditions at room temperature has been studied. Chemical analysis, Fourier transform infrared spectroscopy and X-ray diffraction have also been conducted to validate the formation of magnesium substituted brushite under physiological conditions.

  5. DESIGN, SYNTHESIS, AND APPLICATION OF THE TRIMETHOPRIM-BASED CHEMICAL TAG FOR LIVE CELL IMAGING

    Science.gov (United States)

    Jing, Chaoran; Cornish, Virginia W.

    2013-01-01

    Over the past decade chemical tags have been developed to complement the use of fluorescent proteins in live cell imaging. Chemical tags retain the specificity of protein labeling achieved with fluorescent proteins through genetic encoding, but provide smaller, more robust tags and modular use of organic fluorophores with high photon-output and tailored functionalities. The trimethoprim-based chemical tag (TMP-tag) was initially developed based on the high affinity interaction between E.coli dihydrofolatereductase and the antibiotic trimethoprim and subsequently rendered covalent and fluorogenic via proximity-induced protein labeling reactions. To date, the TMP-tag is one of the few chemical tags that enable intracellular protein labeling and high-resolution live cell imaging. Here we describe the general design, chemical synthesis, and application of TMP-tag for live cell imaging. Alternative protocols for synthesizing and using the covalent and the fluorogenic TMP-tags are also included. PMID:23839994

  6. Design, synthesis, and validation of an in vitro platform peptide-whole cell screening assay using MTT reagent

    Directory of Open Access Journals (Sweden)

    Sahar Ahmed

    2017-05-01

    Full Text Available An in vitro platform to perform peptide screening against different cancer cell lines was designed. The strategy for this screening relied on the design and detection of high-affinity cancer-targeting peptides based on the sequences of NGR and P160. Evaluation of the best binding peptides was performed via incubation of the peptide array-bounded cells with MTT reagent, which is reduced to purple formazan in living cells and further quantified using an Elispot and Kodak imager. For proof of concept, a peptide library (132 spots, and 66 different peptides was designed, synthesized, and screened against different cancer cell lines. The current strategy assists in the identification of positive and negative peptides as well as the relative binding between positive ones. Better binding peptide sequences of the NGR motif were demonstrated to show up to a 2.6-fold increase in CD13+ cell lines with insignificant binding to CD13− ones. Comparable results were observed for P160 peptide sequences, to which different peptides had increased binding, with an up to 3-fold increase relative to the native P160 peptide. Based on our results, new peptide sequences for cancer targeting were identified, and the developed strategy was applied to two different peptide libraries.

  7. Pyrrhocoricin, a proline-rich antimicrobial peptide derived from insect, inhibits the translation process in the cell-free Escherichia coli protein synthesis system.

    Science.gov (United States)

    Taniguchi, Masayuki; Ochiai, Akihito; Kondo, Hiroshi; Fukuda, Shun; Ishiyama, Yohei; Saitoh, Eiichi; Kato, Tetsuo; Tanaka, Takaaki

    2016-05-01

    Previous studies have shown that pyrrhocoricin, a proline-rich antimicrobial peptide (PrAMP), killed sensitive species in a dose-dependent manner by specifically binding to DnaK. Here, on the basis of the finding that DnaK-deficient Escherichia coli strains are susceptible to PrAMPs, we used pyrrhocoricin to investigate internal targets other than DnaK. Using conventional antibiotics (bleomycin, streptomycin, and fosfomycin) that have known modes of action, first, we validated the availability of an assay using a cell-free rapid translation system (RTS), which is an in vitro protein synthesis system based on E. coli lysate, for evaluating inhibition of protein synthesis. We found that, similarly to bleomycin and streptomycin, pyrrhocoricin inhibited GFP synthesis in RTS in a concentration-dependent manner. In addition, blockage of transcription and translation steps in RTS was individually estimated using RT-PCR after gene expression to determine mRNA products and using sodium dodecyl sulfate-polyacrylamide gel electrophoresis to determine the amounts of GFP expressed from purified mRNA, respectively. The results demonstrated that this inhibition of GFP synthesis by pyrrhocoricin did not occur at the transcription step but rather at the translation step, in a manner similar to that of GFP synthesis by streptomycin, an inhibitor of the translation step by causing misreading of tRNA. These results suggest that RTS is a powerful assay system for determining if antimicrobial peptides inhibit protein synthesis and its transcription and/or translation steps. This is the first study to have shown that pyrrhocoricin inhibited protein synthesis by specifically repressing the translation step. Copyright © 2015 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  8. Synthesis of mullite coatings by chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mulpuri, R.P.; Auger, M.; Sarin, V.K. [Boston Univ., MA (United States)

    1996-08-01

    Formation of mullite on ceramic substrates via chemical vapor deposition was investigated. Mullite is a solid solution of Al{sub 2}O{sub 3} and SiO{sub 2} with a composition of 3Al{sub 2}O{sub 3}{circ}2SiO{sub 2}. Thermodynamic calculations performed on the AlCl{sub 3}-SiCl{sub 4}-CO{sub 2}-H{sub 2} system were used to construct equilibrium CVD phase diagrams. With the aid of these diagrams and consideration of kinetic rate limiting factors, initial process parameters were determined. Through process optimization, crystalline CVD mullite coatings have been successfully grown on SiC and Si{sub 3}N{sub 4} substrates. Results from the thermodynamic analysis, process optimization, and effect of various process parameters on deposition rate and coating morphology are discussed.

  9. A simple wet chemical synthesis and characterization of hydroxyapatite nanorods

    International Nuclear Information System (INIS)

    Liu Yingkai; Hou Dedong; Wang Guanghou

    2004-01-01

    Calcium hydroxyapatite (Ca 5 (PO 4 ) 3 (OH):HAP) nanorods have been synthesized successfully via wet chemical technique at low temperature in the presence of suitable surfactant. The as-made nanorods have a diameter of 50-80 nm and a length of 0.5-1.2 μm. The microstructures and composition are characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectrometer (FT-IR). The formation mechanism of HAP nanorod is discussed in detail. It has been found that nanorods are pure, there is no HAP carbonated HAP. The growth mechanism of HAP nanorods could be explained by a soft template

  10. Room-temperature synthesis of core-shell structured magnetic covalent organic frameworks for efficient enrichment of peptides and simultaneous exclusion of proteins.

    Science.gov (United States)

    Lin, Guo; Gao, Chaohong; Zheng, Qiong; Lei, Zhixian; Geng, Huijuan; Lin, Zian; Yang, Huanghao; Cai, Zongwei

    2017-03-28

    Core-shell structured magnetic covalent organic frameworks (Fe 3 O 4 @COFs) were synthesized via a facile approach at room temperature. Combining the advantages of high porosity, magnetic responsiveness, chemical stability and selectivity, Fe 3 O 4 @COFs can serve as an ideal absorbent for the highly efficient enrichment of peptides and the simultaneous exclusion of proteins from complex biological samples.

  11. Bacterial Peptide Deformylase Inhibition of Tetrazole-Substituted Biaryl Acid Analogs: Synthesis, Biological Evaluations, and Molecular Docking Study.

    Science.gov (United States)

    Khan, Firoz A Kalam; Patil, Rajendra H; Patil, Manjiri; Arote, Rohidas; Shinde, Devanand B; Sangshetti, Jaiprakash N

    2016-12-01

    The synthesis and screening of tetrazole-substituted biaryl acid analogs 7a-l as bacterial peptide deformylase (PDF) enzyme inhibitors is reported. The compounds 7e (IC 50 value = 5.50 μM) and 7g (IC 50 value = 7.25 μM) showed good PDF inhibition activity. The compounds 7e (MIC range = 10.75-11.66 μg/mL) and 7g (MIC range = 8.91-12.83 μg/mL) also showed potent antibacterial activity when compared with the standard ciprofloxacin (MIC range = 25-50 μg/mL). Thus, the active derivatives were not only potent PDF enzyme inhibitors but also efficient antibacterial agents. In order to gain more insight into the binding mode of the compounds with the PDF enzyme, the most active compounds 7e and 7g, the moderately active compound 7k, and the least active compound 7h were docked against the PDF enzyme of Escherichia coli. The docking study of the most active compounds 7e and 7g against the PDF enzyme exhibited good binding properties. Hence, we believe our synthesized compounds 7a-l could serve as reservoir for bacterial PDF inhibitor development. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Oxalyl retro-peptide gelators. Synthesis, gelation properties and stereochemical effects.

    Science.gov (United States)

    Makarević, Janja; Jokić, Milan; Frkanec, Leo; Caplar, Vesna; Sijaković Vujičić, Nataša; Zinić, Mladen

    2010-10-04

    In this work we report on gelation properties, self-assembly motifs, chirality effects and morphological characteristics of gels formed by chiral retro-dipeptidic gelators in the form of terminal diacids (1a-5a) and their dimethyl ester (1b-5b) and dicarboxamide (1c-5c) derivatives. Terminal free acid retro-dipeptides (S,S)-bis(LeuLeu) 1a, (S,S)-bis(PhgPhg) 3a and (S,S)-bis(PhePhe) 5a showed moderate to excellent gelation of highly polar water/DMSO and water/DMF solvent mixtures. Retro-peptides incorporating different amino acids (S,S)-(LeuPhg) 2a and (S,S)-(PhgLeu) 4a showed no or very weak gelation. Different gelation effectiveness was found for racemic and single enantiomer gelators. The heterochiral (S,R)-1c diastereoisomer is capable of immobilizing up to 10 and 4 times larger volumes of dichloromethane/DMSO and toluene/DMSO solvent mixtures compared to homochiral (S,S)-1c. Based on the results of (1)H NMR, FTIR, CD investigations, molecular modeling and XRPD studies of diasteroisomeric diesters (S,S)-1b/(S,R)-1b and diacids (S,S)-1b/(S,R)-1a, a basic packing model in their gel aggregates is proposed. The intermolecular hydrogen bonding between extended gelator molecules utilizing both, the oxalamide and peptidic units and layered organization were identified as the most likely motifs appearing in the gel aggregates. Molecular modeling studies of (S,S)-1a/(S,R)-1a and (S,S)-1b/(S,R)-1b diasteroisomeric pairs revealed a decisive stereochemical influence yielding distinctly different low energy conformations: those of (S,R)-diastereoisomers with lipophilic i-Bu groups and polar carboxylic acid or ester groups located on the opposite sides of the oxalamide plane resembling bola amphiphilic structures and those of (S,S)-diasteroisomers possessing the same groups located at both sides of the oxalamide plane. Such conformational characteristics were found to strongly influence both, gelator effectiveness and morphological characteristics of gel aggregates.

  13. Oxalyl retro-peptide gelators. Synthesis, gelation properties and stereochemical effects

    Directory of Open Access Journals (Sweden)

    Janja Makarević

    2010-10-01

    Full Text Available In this work we report on gelation properties, self-assembly motifs, chirality effects and morphological characteristics of gels formed by chiral retro-dipeptidic gelators in the form of terminal diacids (1a–5a and their dimethyl ester (1b–5b and dicarboxamide (1c–5c derivatives. Terminal free acid retro-dipeptides (S,S-bis(LeuLeu 1a, (S,S-bis(PhgPhg 3a and (S,S-bis(PhePhe 5a showed moderate to excellent gelation of highly polar water/DMSO and water/DMF solvent mixtures. Retro-peptides incorporating different amino acids (S,S-(LeuPhg 2a and (S,S-(PhgLeu 4a showed no or very weak gelation. Different gelation effectiveness was found for racemic and single enantiomer gelators. The heterochiral (S,R-1c diastereoisomer is capable of immobilizing up to 10 and 4 times larger volumes of dichloromethane/DMSO and toluene/DMSO solvent mixtures compared to homochiral (S,S-1c. Based on the results of 1H NMR, FTIR, CD investigations, molecular modeling and XRPD studies of diasteroisomeric diesters (S,S-1b/(S,R-1b and diacids (S,S-1b/(S,R-1a, a basic packing model in their gel aggregates is proposed. The intermolecular hydrogen bonding between extended gelator molecules utilizing both, the oxalamide and peptidic units and layered organization were identified as the most likely motifs appearing in the gel aggregates. Molecular modeling studies of (S,S-1a/(S,R-1a and (S,S-1b/(S,R-1b diasteroisomeric pairs revealed a decisive stereochemical influence yielding distinctly different low energy conformations: those of (S,R-diastereoisomers with lipophilic i-Bu groups and polar carboxylic acid or ester groups located on the opposite sides of the oxalamide plane resembling bola amphiphilic structures and those of (S,S-diasteroisomers possessing the same groups located at both sides of the oxalamide plane. Such conformational characteristics were found to strongly influence both, gelator effectiveness and morphological characteristics of gel aggregates.

  14. Amino-acid- and peptide-directed synthesis of chiral plasmonic gold nanoparticles.

    Science.gov (United States)

    Lee, Hye-Eun; Ahn, Hyo-Yong; Mun, Jungho; Lee, Yoon Young; Kim, Minkyung; Cho, Nam Heon; Chang, Kiseok; Kim, Wook Sung; Rho, Junsuk; Nam, Ki Tae

    2018-04-01

    Understanding chirality, or handedness, in molecules is important because of the enantioselectivity that is observed in many biochemical reactions 1 , and because of the recent development of chiral metamaterials with exceptional light-manipulating capabilities, such as polarization control 2-4 , a negative refractive index 5 and chiral sensing 6 . Chiral nanostructures have been produced using nanofabrication techniques such as lithography 7 and molecular self-assembly 8-11 , but large-scale and simple fabrication methods for three-dimensional chiral structures remain a challenge. In this regard, chirality transfer represents a simpler and more efficient method for controlling chiral morphology 12-18 . Although a few studies 18,19 have described the transfer of molecular chirality into micrometre-sized helical ceramic crystals, this technique has yet to be implemented for metal nanoparticles with sizes of hundreds of nanometres. Here we develop a strategy for synthesizing chiral gold nanoparticles that involves using amino acids and peptides to control the optical activity, handedness and chiral plasmonic resonance of the nanoparticles. The key requirement for achieving such chiral structures is the formation of high-Miller-index surfaces ({hkl}, h ≠ k ≠ l ≠ 0) that are intrinsically chiral, owing to the presence of 'kink' sites 20-22 in the nanoparticles during growth. The presence of chiral components at the inorganic surface of the nanoparticles and in the amino acids and peptides results in enantioselective interactions at the interface between these elements; these interactions lead to asymmetric evolution of the nanoparticles and the formation of helicoid morphologies that consist of highly twisted chiral elements. The gold nanoparticles that we grow display strong chiral plasmonic optical activity (a dis-symmetry factor of 0.2), even when dispersed randomly in solution; this observation is supported by theoretical calculations and direct

  15. Radiochemical problems of radiation chemical synthesis in n, γ-field of nuclear reactor

    International Nuclear Information System (INIS)

    Mironov, V.P.; Frejdus, N.V.; Bugaenko, L.T.; Kalyazin, E.P.; Petryaev, E.P.

    1981-01-01

    A wide applicability of products of radiation chemical synthesis (RCS), using n, γ-irradiation, is limited by possible contamination of the latter with long-lived radioactive isotopes of chemical elements included in the composition of the reagent and compounds syntesized (chemically non-separable radionuclides - CNR). A technique of the determination of the limit accumulation CNR on the basis of radiation chemical parameters of the synthesis (radiation-chemical yield, the dose rate absorbed, singleness of purpose of RCS etc.) and radiochemical parameters of formation and accumulation of CNR (radiochemical yields of CNR in the products of radiolysis, neutron fluence, the reagent purity etc.) is suggested. The radiochemical evaluation of CNR accumulation (tritium and carbon-14), formed at the expense of activation with neutrons of chemical elements of water and organic substances, consisting of hydrogen, carbon and oxygen has shown that at relatively low yields of final products (> or approximately 3 molecules/100 eV) no accumulation of radionuclides in concentrations reaching the average admissible concentration takes place [ru

  16. Procafd: Computer Aided Tool for Synthesis-Design & Analysis of Chemical Process Flowsheets

    DEFF Research Database (Denmark)

    Kumar Tula, Anjan; Eden, Mario R.; Gani, Rafiqul

    2015-01-01

    and emission to the surrounding and many more. In terms of approaches to solve the synthesis-design problem three major lines of attack have emerged: (a) the knowledge based approach [1] which relies on engineering knowledge & problem insights, (b) the optimization approach [2] which relies on the use...... of mathematical programming techniques, (c) hybrid approach which combine two or more approaches. D’Anterroches [3] proposed a group contribution based hybrid approach to solve the synthesis-design problem where, chemical process flowsheets could be synthesized in the same way as atoms or groups of atoms...... parameters for the operations of the high ranked flowsheets are established through reverse engineering approaches based on driving forces available for each operation. In the final stage, rigorous simulation is performed to validate the synthesis-design. Note that since the flowsheet is synthesized...

  17. Synthesis of peptide templated copper nanoclusters for fluorometric determination of Fe(III) in human serum

    International Nuclear Information System (INIS)

    Tang, Ting; Ouyang, Jiang; Hu, Lanshuang; Guo, Linyan; Yang, Minghui; Chen, Xiang

    2016-01-01

    Copper nanoclusters (Cu-NCs) were prepared by reducing CuCl 2 with ascorbic acid in the presence of the short peptide template Cys-Cys-Cys-Asp-Leu. They were characterized by UV-vis absorption and fluorescence spectroscopy, transmission electron microscopy and X-ray photoelectron spectroscopy. The Cu-NCs have a size of ∼2 nm, can be well dispersed in water and are photostable. Their fluorescence (peaking at 425 nm under 365-nm excitation) is quenched by Fe(III) ions. Based on this finding, a sensitive and selective fluorescence assay for the detection of Fe(III) was developed. Under optimized conditions and a pH value of 2.0, the assay displays a linear response in the 0.05 to 30 μM Fe(III) concentration range, with a detection limit of 20 nM based on an S/N ratio of 3. The assay was successfully applied to the determination of Fe(III) in spiked human serum where is gave recoveries that ranged from 96.2 % to 98.3 %. (author)

  18. Synthesis and functional evaluation of a peptide derivative of 1-beta-D-arabinofuranosylcytosine.

    Science.gov (United States)

    Balajthy, Z; Aradi, J; Kiss, I T; Elödi, P

    1992-09-04

    We have synthesized a peptidyl prodrug derivative of 1-beta-D-arabinofuranosylcytosine (1) designed to be a selective substrate of plasmin. D-Val-Leu-Lys-ara-C (2) was obtained by coupling the protected peptide Cbz-D-Val-Leu-(N6-Cbz)Lys-OH and ara-C (1) by a water-soluble carbodiimide (EDCI), followed by the removal of the Cbz groups by using catalytic hydrogenolysis over Pd/C. The kinetic constant of hydrolysis of 2 in the presence of plasmin demonstrated effective release of 1. The amino group of 1, which is sensitive to the removal by cytidine deaminase, is protected in 2 by the formation of the amide bond resulting in a prolonged half-life of 2 in biological milieu. The antiproliferative efficiency of 2 against L1210 leukemic cells was significantly higher than that of 1. The activity of 2 was abolished in the presence of serine proteinase inhibitor, (4-amidinopheny)methanesulfonyl fluoride. These data indicate that 2 is a prodrug form of 1 in systems generating plasmin.

  19. Synthesis and optical properties of pyrrolidinyl peptide nucleic acid carrying a clicked Nile red label

    Directory of Open Access Journals (Sweden)

    Nattawut Yotapan

    2014-09-01

    Full Text Available DNA or its analogues with an environment-sensitive fluorescent label are potentially useful as a probe for studying the structure and dynamics of nucleic acids. In this work, pyrrolidinyl peptide nucleic acid (acpcPNA was labeled at its backbone with Nile red, a solvatochromic benzophenoxazine dye, by means of click chemistry. The optical properties of the Nile red-labeled acpcPNA were investigated by UV–vis and fluorescence spectroscopy in the absence and in the presence of DNA. In contrast to the usual quenching observed in Nile red-labeled DNA, the hybridization with DNA resulted in blue shifting and an enhanced fluorescence regardless of the neighboring bases. More pronounced blue shifts and fluorescence enhancements were observed when the DNA target carried a base insertion in close proximity to the Nile red label. The results indicate that the Nile red label is located in a more hydrophobic environment in acpcPNA–DNA duplexes than in the single-stranded acpcPNA. The different fluorescence properties of the acpcPNA hybrids of complementary DNA and DNA carrying a base insertion are suggestive of different interactions between the Nile red label and the duplexes.

  20. Synthesis of PEGylated polyglutamic acid peptide dendrimer and its application in dissolving thrombus.

    Science.gov (United States)

    Zhang, Shao-Fei; Gao, Chunmei; Lü, Shaoyu; He, Jiujun; Liu, Mingzhu; Wu, Can; Liu, Yijing; Zhang, Xinyu; Liu, Zhen

    2017-11-01

    Nattokinase (NK) has been used as a new generation thrombolytic drug, due to its high safety, low cost and low side effects. However, it is sensitive to external environment and may lose the enzyme activity easily. Peptide dendrimer possesses functional groups on its surface, adjustable sizes, biodegradability, biocompatibility, and low toxicity, which could be used as ideal carrier for drug protection and delivery. Demonstrated for the first time in this paper, a PEGylated dendrimer (G n -PEG-G n ) composed of polyglutamic acid is designed and synthesized as delivery platform of NK for thrombus treatment. A panel of PEGylated dendrimers with three different generations of 2, 3, 4 was prepared to investigate the effect of dendrimer architecture on the properties and therapeutic efficacy of the resultant NK-loaded delivery systems in terms of the morphology, dimension and enzyme activity. The results demonstrated that the NK-loaded G 3 -PEG-G 3 (G 3 -PEG-G 3 /NK ratio of 6/1), of all the formulations, displayed the optimal enzyme activity for dissolving thrombus in vitro, thus offering great potential for the treatment of thrombus. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Using 1H and 13C NMR chemical shifts to determine cyclic peptide conformations: a combined molecular dynamics and quantum mechanics approach.

    Science.gov (United States)

    Nguyen, Q Nhu N; Schwochert, Joshua; Tantillo, Dean J; Lokey, R Scott

    2018-05-10

    Solving conformations of cyclic peptides can provide insight into structure-activity and structure-property relationships, which can help in the design of compounds with improved bioactivity and/or ADME characteristics. The most common approaches for determining the structures of cyclic peptides are based on NMR-derived distance restraints obtained from NOESY or ROESY cross-peak intensities, and 3J-based dihedral restraints using the Karplus relationship. Unfortunately, these observables are often too weak, sparse, or degenerate to provide unequivocal, high-confidence solution structures, prompting us to investigate an alternative approach that relies only on 1H and 13C chemical shifts as experimental observables. This method, which we call conformational analysis from NMR and density-functional prediction of low-energy ensembles (CANDLE), uses molecular dynamics (MD) simulations to generate conformer families and density functional theory (DFT) calculations to predict their 1H and 13C chemical shifts. Iterative conformer searches and DFT energy calculations on a cyclic peptide-peptoid hybrid yielded Boltzmann ensembles whose predicted chemical shifts matched the experimental values better than any single conformer. For these compounds, CANDLE outperformed the classic NOE- and 3J-coupling-based approach by disambiguating similar β-turn types and also enabled the structural elucidation of the minor conformer. Through the use of chemical shifts, in conjunction with DFT and MD calculations, CANDLE can help illuminate conformational ensembles of cyclic peptides in solution.

  2. Synthesis and characterization of carbon nanofilms for chemical sensing

    Science.gov (United States)

    Kumar, Vivek

    Carbon nanofilms obtained by high temperature graphitization of diamond surface in inert atmospheres or vacuum are modified by treatment in plasma of different precursor gases. At temperatures above 1000 °C, a stable conductive film of thickness between 10 - 100 nm and specific resistivity 10-3-10-4 Ωm, depending upon the heating conditions and the growth atmosphere, is formed on diamond surface. A gray, thin film of high surface resistivity is obtained in high vacuum, while at low vacuum (below 10-4 mbar), a thick black film of low surface resistivity forms. It is observed that the exposure to plasma reduces the surface conductance of carbon nanofilms as result of a partial removal of carbon and the plasma-stimulated amorphization. The rate of the reduction of conductance and hence the etching ability of plasma depends on the type of precursor gas. Hydrogen reveals the strongest etching ability, followed by oxygen and argon, whereas SF6 is ineffective. The carbon nanofilms show significant sensitivity of their electrical conductance to temperature and exposure to the vapors of common organic compounds. The oxygen plasma treated films exhibit selective response to acetone and water vapors. The fast response and recovery of the conductance are the features of the carbon nanofilms. The plasma-treated carbon nanofilm on graphitized diamond surface is discussed as a promising sensing material for development of all-carbon chemical sensors, which may be suitable for biological and medical applications. An alternative approach of fabrication of temperature and chemical sensitive carbon nanofilms on insulating substrates is proposed. The films are obtained by direct deposition of sputtered carbon on highly polished quartz substrates followed by subsequent annealing at temperatures above 400 °C. It is observed that the as-deposited films are essentially amorphous, while the heating induces irreversible structural ordering and gradual conversion of amorphous carbon in

  3. A functional mimic of natural peroxidases : synthesis and catalytic activity of a non-heme iron peptide hydroperoxide complex

    NARCIS (Netherlands)

    Choma, CT; Schudde, EP; Kellogg, RM; Robillard, GT; Feringa, BL

    1998-01-01

    Site-selective attachment of unprotected peptides to a non-heme iron complex is achieved by displacing two halides on the catalyst by peptide caesium thiolates, This coupling approach should be compatible with any peptide sequence provided there is only a single reduced cysteine. The oxidation

  4. Chemical annotation of small and peptide-like molecules at the Protein Data Bank

    Science.gov (United States)

    Young, Jasmine Y.; Feng, Zukang; Dimitropoulos, Dimitris; Sala, Raul; Westbrook, John; Zhuravleva, Marina; Shao, Chenghua; Quesada, Martha; Peisach, Ezra; Berman, Helen M.

    2013-01-01

    Over the past decade, the number of polymers and their complexes with small molecules in the Protein Data Bank archive (PDB) has continued to increase significantly. To support scientific advancements and ensure the best quality and completeness of the data files over the next 10 years and beyond, the Worldwide PDB partnership that manages the PDB archive is developing a new deposition and annotation system. This system focuses on efficient data capture across all supported experimental methods. The new deposition and annotation system is composed of four major modules that together support all of the processing requirements for a PDB entry. In this article, we describe one such module called the Chemical Component Annotation Tool. This tool uses information from both the Chemical Component Dictionary and Biologically Interesting molecule Reference Dictionary to aid in annotation. Benchmark studies have shown that the Chemical Component Annotation Tool provides significant improvements in processing efficiency and data quality. Database URL: http://wwpdb.org PMID:24291661

  5. Synthesis of reference compounds related to Chemical Weapons Convention for verification and drug development purposes – a Brazilian endeavour

    Science.gov (United States)

    Cavalcante, S. F. A.; de Paula, R. L.; Kitagawa, D. A. S.; Barcellos, M. C.; Simas, A. B. C.; Granjeiro, J. M.

    2018-03-01

    This paper deals with challenges that Brazilian Army Organic Synthesis Laboratory has been going through to access reference compounds related to the Chemical Weapons Convention in order to support verification analysis and for research of novel antidotes. Some synthetic procedures to produce the chemicals, as well as Quality Assurance issues and a brief introduction of international agreements banning chemical weapons are also presented.

  6. Pressure dependence of side chain 13C chemical shifts in model peptides Ac-Gly-Gly-Xxx-Ala-NH2.

    Science.gov (United States)

    Beck Erlach, Markus; Koehler, Joerg; Crusca, Edson; Munte, Claudia E; Kainosho, Masatsune; Kremer, Werner; Kalbitzer, Hans Robert

    2017-10-01

    For evaluating the pressure responses of folded as well as intrinsically unfolded proteins detectable by NMR spectroscopy the availability of data from well-defined model systems is indispensable. In this work we report the pressure dependence of 13 C chemical shifts of the side chain atoms in the protected tetrapeptides Ac-Gly-Gly-Xxx-Ala-NH 2 (Xxx, one of the 20 canonical amino acids). Contrary to expectation the chemical shifts of a number of nuclei have a nonlinear dependence on pressure in the range from 0.1 to 200 MPa. The size of the polynomial pressure coefficients B 1 and B 2 is dependent on the type of atom and amino acid studied. For H N , N and C α the first order pressure coefficient B 1 is also correlated to the chemical shift at atmospheric pressure. The first and second order pressure coefficients of a given type of carbon atom show significant linear correlations suggesting that the NMR observable pressure effects in the different amino acids have at least partly the same physical cause. In line with this observation the magnitude of the second order coefficients of nuclei being direct neighbors in the chemical structure also are weakly correlated. The downfield shifts of the methyl resonances suggest that gauche conformers of the side chains are not preferred with pressure. The valine and leucine methyl groups in the model peptides were assigned using stereospecifically 13 C enriched amino acids with the pro-R carbons downfield shifted relative to the pro-S carbons.

  7. Uranium complexes with macrosyclic polyethers. Synthesis and structural chemical analysis

    International Nuclear Information System (INIS)

    Elbasyouny, A.

    1983-01-01

    This dissertation reports about studies on the chemical coordination behaviour of uranium of oxidation stages IV and VI with regard to twelve different macrocyclic ligands. For the preparation of the complexes, for every system a different method has been developed. The elementary analysis of the various complexes including the uranium had been done by X-ray fluorescence analysis, and the structural characterization proceeded via vibrational, uv-vis and emission spectroscopy as well as 1 H-NMR and 13 C-spin-lattice relaxation time studies. Conformational analysis of the polyethers used allowed the structural changes in the complexes to be observed. The structural analysis of the hydrous uranium VI crown ether complexes yielded information of characteristic features of these types of complexes. The first coordination sphere of the uranyl ion with covalently bonded anion remains unchanged. As to the water content, there is a certain range. Depending upon the solvent used, the complexes have two or four H 2 O molecules per formula unit. (orig./EF) [de

  8. Alternate fuels and chemicals from synthesis gas: Vinyl acetate monomer. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Richard D. Colberg; Nick A. Collins; Edwin F. Holcombe; Gerald C. Tustin; Joseph R. Zoeller

    1999-01-01

    There has been a long-standing desire on the part of industry and the U.S. Department of Energy to replace the existing ethylene-based vinyl acetate monomer (VAM) process with an entirely synthesis gas-based process. Although there are a large number of process options for the conversion of synthesis gas to VAM, Eastman Chemical Company undertook an analytical approach, based on known chemical and economic principles, to reduce the potential candidate processes to a select group of eight processes. The critical technologies that would be required for these routes were: (1) the esterification of acetaldehyde (AcH) with ketene to generate VAM, (2) the hydrogenation of ketene to acetaldehyde, (3) the hydrogenation of acetic acid to acetaldehyde, and (4) the reductive carbonylation of methanol to acetaldehyde. This report describes the selection process for the candidate processes, the successful development of the key technologies, and the economic assessments for the preferred routes. In addition, improvements in the conversion of acetic anhydride and acetaldehyde to VAM are discussed. The conclusion from this study is that, with the technology developed in this study, VAM may be produced from synthesis gas, but the cost of production is about 15% higher than the conventional oxidative acetoxylation of ethylene, primarily due to higher capital associated with the synthesis gas-based processes.

  9. Chemical synthesis of a dual branched malto-decaose: A potential substrate for alpha-amylases

    DEFF Research Database (Denmark)

    Damager, Iben; Jensen, Morten; Olsen, Carl Erik

    2005-01-01

    A convergent block strategy for general use in efficient synthesis of complex alpha-(1 -> 4)- and alpha-(1 -> 6)-malto-oligosaccharides is demonstrated with the first chemical synthesis of a malto-oligosaccharide, the decasoccharide 6,6""-bis(alpha-maltosyl)-maltohexaose, with two branch points....... Using this chemically defined branched oligosaccharide as a substrate, the cleavage pattern of seven different alpha-amylases were investigated. alpha-Amylases from human saliva, porcine pancreas, barley alpha-amylose 2 and recombinant barley alpha-amylase 1 all hydrolysed the decasaccharide selectively....... This resulted in a branched hexasaccharide and a branched tetrasoccharide. alpha-Amylases from Asperagillus oryzae, Bacillus licheniformis and Bacillus sp. cleaved the decasoccharide at two distinct sites, either producing two branched pentasoccharides, or a branched hexasoccharide and a branched...

  10. The impact of the chemical synthesis on the magnetic properties of intermetallic PdFe nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Castellanos-Rubio, I.; Insausti, M.; Muro, I. Gil de [Universidad del País Vasco, UPV/EHU, Dpto. de Química Inorgánica (Spain); Arias-Duque, D. Carolina; Hernández-Garrido, Juan Carlos [Universidad de Cadiz, Departamento de Ciencia de los Materiales e Ingeniería Metalúrgica y Química Inorgánica, Facultad de Ciencias (Spain); Rojo, T.; Lezama, L., E-mail: luis.lezama@ehu.es [Universidad del País Vasco, UPV/EHU, Dpto. de Química Inorgánica (Spain)

    2015-05-15

    Palladium-rich Iron nanoparticles in the 4–8 nm range have been produced by a combination of two methods: the thermal decomposition of organometallic precursors and the reduction of metallic salts by a polyol. Herein, it is shown how the details of the synthesis have a striking impact on the magnetic and morphological properties of the final products. In the synthesis of these bimetallic nanoparticles, the use of high reaction temperatures plays an essential role in attaining good chemical homogeneity, which has proved to have a key influence on the magnetic properties. Magnetic characterization has been performed by electron magnetic resonance and magnetization measurements, which have confirmed the superparamagnetic-like behavior at room temperature. No clear traces of magnetic polarization in palladium atoms have been detected. The combination of long-term stability and homogeneous chemical and magnetic properties makes these particles very suitable for a wide range of applications in nanotechnology.

  11. The impact of the chemical synthesis on the magnetic properties of intermetallic PdFe nanoparticles

    International Nuclear Information System (INIS)

    Castellanos-Rubio, I.; Insausti, M.; Muro, I. Gil de; Arias-Duque, D. Carolina; Hernández-Garrido, Juan Carlos; Rojo, T.; Lezama, L.

    2015-01-01

    Palladium-rich Iron nanoparticles in the 4–8 nm range have been produced by a combination of two methods: the thermal decomposition of organometallic precursors and the reduction of metallic salts by a polyol. Herein, it is shown how the details of the synthesis have a striking impact on the magnetic and morphological properties of the final products. In the synthesis of these bimetallic nanoparticles, the use of high reaction temperatures plays an essential role in attaining good chemical homogeneity, which has proved to have a key influence on the magnetic properties. Magnetic characterization has been performed by electron magnetic resonance and magnetization measurements, which have confirmed the superparamagnetic-like behavior at room temperature. No clear traces of magnetic polarization in palladium atoms have been detected. The combination of long-term stability and homogeneous chemical and magnetic properties makes these particles very suitable for a wide range of applications in nanotechnology

  12. Some chemical synthesis of 14C labelled compounds of pharmaceutical or biological interest

    International Nuclear Information System (INIS)

    Pichat, I.; Baret, C.; Audinot, M.; Herbert, M.; Lambin, J.

    1955-01-01

    The recent discovery of the tuberculostatic properties of the hydrazide of isonicotinic acid (so-called 'Isoniazide', 'Rimifon') has raised considerably its interest, as for metabolic studies which it is more interesting to have it labelled with 14 C. We describe in this report the chemical synthesis of 14 C carboxyl labelled isoniazide which were done in the pyridine ring to highlight his metabolic function on the Koch's bacillus. (M.B.)

  13. Some chemical synthesis of {sup 14}C labelled compounds of pharmaceutical or biological interest

    Energy Technology Data Exchange (ETDEWEB)

    Pichat, I; Baret, C; Audinot, M; Herbert, M; Lambin, J [Commissariat a l' Energie Atomique, Lab. du Fort de Chatillon, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1955-07-01

    The recent discovery of the tuberculostatic properties of the hydrazide of isonicotinic acid (so-called 'Isoniazide', 'Rimifon') has raised considerably its interest, as for metabolic studies which it is more interesting to have it labelled with {sup 14}C. We describe in this report the chemical synthesis of {sup 14}C carboxyl labelled isoniazide which were done in the pyridine ring to highlight his metabolic function on the Koch's bacillus. (M.B.)

  14. Chemical synthesis of Cd-free wide band gap materials for solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Sankapal, B.R.; Sartale, S.D.; Ennaoui, A. [Hahn-Meitner-Institut, Berlin (Germany). Department of Solar Energy Research; Lokhande, C.D. [Shivaji University, Kolhapur (India). Department of Physics

    2004-07-01

    Chemical methods are nowadays very attractive, since they are relatively simple, low cost and convenient for larger area deposition of thin films. In this paper, we outline our work related to the synthesis and characterization of some wide band gap semiconducting material thin films prepared by using solution methods, namely, chemical bath deposition and successive ionic layer adsorption and reaction (SILAR). The optimum preparative parameters are given and respective structural, surface morphological, compositional, optical, and electrical properties are described. Some materials we used in solar cells as buffer layers and achieved remarkable results, which are summarized. (author)

  15. Chemical synthesis, phase transformation and magnetic proprieties of FePt and FePd nanoparticles

    International Nuclear Information System (INIS)

    Delattre, Anastasia

    2010-01-01

    This work aims at understanding the chemical synthesis of FePt and FePd nanoparticles (NPs), and at exploring how to implement the phase transformation from the chemically disordered to the L10 phase, without coalescence. Using hexadecanenitrile instead of oleylamine, we obtain NPs with a more homogenous internal composition, instead of core-shell NPs. Through a systematic study (designed experiment relying on Taguchi tables), we developed the FePd synthesis, while evidencing the role of each ligand and of the reductor. To induce the crystalline phase transformation while avoiding coalescence, we explored two ways. In the first one, atomic vacancies are introduced in the NPs through light ion irradiation, atomic mobility being ensured by annealing at moderate temperature (300 C). As a result, the blocking temperature is multiplied by 4, due to anisotropy enhancement. However, strong chemical ordering in the L10 phase cannot be achieved. The second approach relies on the dispersion of the NPs in a salt (NaCl) matrix, prior to annealing at 700 C: high chemical ordering is achieved, and the blocking temperature is beyond 400 C. We then developed a single-step process to remove the salt by dissolution in water and to re-disperse NPs in stable aqueous or organics solutions. These high magnetic anisotropy NPs are then readily available for further chemical or manipulation steps, with applied perspectives in areas such as data storage, or biology. (author)

  16. Selective desulfurization of cysteine in the presence of Cys(Acm) in polypeptides obtained by native chemical ligation.

    Science.gov (United States)

    Pentelute, Brad L; Kent, Stephen B H

    2007-02-15

    Increased versatility for the synthesis of proteins and peptides by native chemical ligation requires the ability to ligate at positions other than Cys. Here, we report that Raney nickel can be used under standard conditions for the selective desulfurization of Cys in the presence of Cys(Acm). This simple and practical tactic enables the more common Xaa-Ala junctions to be used as ligation sites for the chemical synthesis of Cys-containing peptides and proteins. [reaction: see text].

  17. Titanium nitride plasma-chemical synthesis with titanium tetrachloride raw material in the DC plasma-arc reactor

    Science.gov (United States)

    Kirpichev, D. E.; Sinaiskiy, M. A.; Samokhin, A. V.; Alexeev, N. V.

    2017-04-01

    The possibility of plasmochemical synthesis of titanium nitride is demonstrated in the paper. Results of the thermodynamic analysis of TiCl4 - H2 - N2 system are presented; key parameters of TiN synthesis process are calculated. The influence of parameters of plasma-chemical titanium nitride synthesis process in the reactor with an arc plasmatron on characteristics on the produced powders is experimentally investigated. Structure, chemical composition and morphology dependencies on plasma jet enthalpy, stoichiometric excess of hydrogen and nitrogen in a plasma jet are determined.

  18. Synthesis of a cyclic fibrin-like peptide and its analysis by fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Young, J.D.; Costello, C.E.; Langenhove, A. van; Haber, E.; Matsueda, G.R.

    1983-01-01

    For immunochemical purposes, a cyclic 12 peptide was synthesized to model the γ-γ-chain cross-link site in human fibrin. The model was based upon the structure proposed by Chen and Doolittle which is characterized by two reciprocating epsilon-(γ-Glu)Lys bonds between adjacent fibrin γ-chains oriented in an antiparallel manner. To achieve the antiparallel orientation of the peptide backbone, Pro and Gly were inserted at positions 6 and 7 of the linear 12-peptide: acetyl-Gly-Glu-Gln-His-His-Pro-Gly-Gly-Gly-Ala-Lys-Gly-amide. The insertions were made to facilitate a reverse turn of the peptide during the last synthetic step, which was formation of the epsilon-(γ-Glu)Lys bond between Glu at position 2 and Lys at position 11 with diphenylphosphorylazide. The resulting cyclic peptide represented half of the symmetrical cross-linked region in clotted fibrin. Following purification by HPLC, both linear and cyclic 12-peptides were analyzed by fast atom bombardment mass spectrometry. Abundant molecular protonated ions were observed for both peptides. In addition, the amino acid sequence of the linear peptide and the location of the epsilon-(γ-Glu)Lys bond in the cyclized peptide could be verified. (author)

  19. Room temperature chemical synthesis of Cu(OH){sub 2} thin films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Gurav, K.V. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Patil, U.M. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Kim, J.H., E-mail: jinhyeok@chonnam.ac.kr [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of)

    2013-10-05

    Highlights: •Cu(OH){sub 2} is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH){sub 2}. •The hydrous, nanograined Cu(OH){sub 2} shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH){sub 2}] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH){sub 2} thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH){sub 2} thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH){sub 2} thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance.

  20. Room temperature chemical synthesis of Cu(OH)2 thin films for supercapacitor application

    International Nuclear Information System (INIS)

    Gurav, K.V.; Patil, U.M.; Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S.; Lokhande, C.D.; Kim, J.H.

    2013-01-01

    Highlights: •Cu(OH) 2 is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH) 2 . •The hydrous, nanograined Cu(OH) 2 shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH) 2 ] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH) 2 thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH) 2 thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH) 2 thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance

  1. Synthesis of ultra-long cadmium telluride nanotubes via combinational chemical transformation

    Energy Technology Data Exchange (ETDEWEB)

    Park, Kee-Ryung; Cho, Hong-Baek; Choa, Yong-Ho, E-mail: choa15@hanyang.ac.kr

    2017-03-01

    Synthesis of high-throughput cadmium telluride (CdTe) nanotubes with an ultra-long aspect ratio is presented via a combination process concept combined with electrospinning, electrodeposition, and cationic exchange reaction. Ultra-long sacrificial silver (Ag) nanofibers were synthesized by electrospinning involving two-step calcination, and were then electrodeposited to create silver telluride nanotubes. These nanotubes underwent cationic exchange reaction in cadmium nitrate tetrahydrate solution with the aid of a ligand, tributylphosphine (TBP). Analysis showed that ultra-long pure zinc blende CdTe nanotubes were obtained with controlled dimension and uniform morphology. The thermodynamic driving force induced by the coordination of methanol solvent and TBP attributed to overcome the kinetic barrier between Ag{sub 2}Te and CdTe nanotubes, facilitating the synthesis of CdTe nanotubes. This synthetic process involving a topotactic reaction route paves a way for high-throughput extended synthesis of new chalcogenide hollow nanotubes for application in photodetectors and solar cells. - Highlights: • High throughput synthetic route of hollow CdTe nanotubes with ultra-long aspect ratio. • Chemical combination of electrospinning, electrodeposition & cation exchange reaction. • Pure zinc blende CdTe by controlled dimension & structural variation of Ag nanofibers. • Potential for the high throughput synthesis of new exotic chalcogenide nanotubes.

  2. Chemical synthesis of membrane proteins: a model study on the influenza virus B proton channel† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c8sc00004b

    Science.gov (United States)

    Baumruck, A. C.; Tietze, D.; Steinacker, L. K.

    2018-01-01

    In the present study we have developed and optimized a robust strategy for the synthesis of highly hydrophobic peptides, especially membrane proteins, exemplarily using the influenza B M2 proton channel (BM2(1–51)). This strategy is based on the native chemical ligation of two fragments, where the thioester fragment is formed from an oxo-ester peptide, which is synthesized using Fmoc-SPPS, and features an in situ cleavable solubilizing tag (ADO, ADO2 or ADO-Lys5). The nearly quantitative production of the ligation product was followed by an optimized work up protocol, resulting in almost quantitative desulfurization and Acm-group cleavage. Circular dichroism analysis in a POPC lipid membrane revealed that the synthetic BM2(1–51) construct adopts a helical structure similar to that of the previously characterized BM2(1–33). PMID:29719709

  3. Optimality principle for the coupled chemical reactions of ATP synthesis and its molecular interpretation

    Science.gov (United States)

    Nath, Sunil

    2018-05-01

    Metabolic energy obtained from the coupled chemical reactions of oxidative phosphorylation (OX PHOS) is harnessed in the form of ATP by cells. We experimentally measured thermodynamic forces and fluxes during ATP synthesis, and calculated the thermodynamic efficiency, η and the rate of free energy dissipation, Φ. We show that the OX PHOS system is tuned such that the coupled nonequilibrium processes operate at optimal η. This state does not coincide with the state of minimum Φ but is compatible with maximum Φ under the imposed constraints. Conditions that must hold for species concentration in order to satisfy the principle of optimal efficiency are derived analytically and a molecular explanation based on Nath's torsional mechanism of energy transduction and ATP synthesis is suggested. Differences of the proposed principle with Prigogine's principle are discussed.

  4. CdS nanowires formed by chemical synthesis using conjugated single-stranded DNA molecules

    Science.gov (United States)

    Sarangi, S. N.; Sahu, S. N.; Nozaki, S.

    2018-03-01

    CdS nanowires were successfully grown by chemical synthesis using two conjugated single-stranded (ss) DNA molecules, poly G (30) and poly C (30), as templates. During the early stage of the synthesis with the DNA molecules, the Cd 2+ interacts with Poly G and Poly C and produces the (Cd 2+)-Poly GC complex. As the growth proceeds, it results in nanowires. The structural analysis by grazing angle x-ray diffraction and transmission electron microscopy confirmed the zinc-blende CdS nanowires with the growth direction of . Although the nanowires are well surface-passivated with the DNA molecules, the photoluminescence quenching was caused by the electron transfer from the nanowires to the DNA molecules. The quenching can be used to detect and label the DNAs.

  5. Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

    International Nuclear Information System (INIS)

    Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

    2011-01-01

    Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 deg. C down to 450 deg. C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

  6. Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

    Science.gov (United States)

    Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

    2011-06-01

    Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 °C down to 450 °C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

  7. Synthesis of Y-Tip Graphitic Nanoribbons from Alcohol Catalytic Chemical Vapor Deposition on Piezoelectric Substrate

    Directory of Open Access Journals (Sweden)

    Zainab Yunusa

    2015-01-01

    Full Text Available We report the synthesis of Graphitic Nanoribbons (GNRs using Alcohol Catalytic Chemical Vapor Deposition (ACCVD. Bulk GNR was synthesized directly on a piezoelectric substrate using one-step ACCVD. The synthesized GNRs were characterized by X-Ray Diffraction (XRD, Scanning Electron Microscope (SEM, Transmission Electron Microscope (TEM, Energy Dispersive X-Ray (EDX, Atomic Force Microscopy (AFM, and Raman spectroscopy. The characterization results showed Y-tip morphology of bulk and filamentous as-grown GNR having varying width that lies between tens and hundreds of nm and length of several microns. Based on the thickness obtained from the AFM and the analysis from the Raman spectroscopy, it was concluded that the synthesized GNRs are multiple-layered and graphitic in nature. With the direct synthesis of GNR on a piezoelectric substrate, it could have applications in the sensor industries, while the Y-tip GNR could have potentialities in semiconductor applications.

  8. Macrokinetics of carbon nanotubes synthesis by the chemical vapor deposition method

    Science.gov (United States)

    Rukhov, Artem; Dyachkova, Tatyana; Tugolukov, Evgeny; Besperstova, Galina

    2017-11-01

    A new approach to studying and developing basic processes which take place on the surface of a metal catalyst during the thermal decomposition of carbonaceous substances in the carbon nanotubes synthesis by the chemical vapor deposition method was proposed. In addition, an analysis was made of the interrelationships between these thermal, diffusion, hydrodynamic and other synthesis processes. A strong effect of the catalyst regeneration stage on the stage of nanotube formation has been shown. Based on the developed approach, a mathematical model was elaborated. Comparison of the calculation and the experiment carried out with the NiO-MgO catalyst at propane flow rate of 50 mL/min (standard conditions) and ethanol flow rate 0.3 mL/min (liq.) has revealed a discrepancy of less than 10%.

  9. Synthesis of 5-(hydroxymethyl)furfural in Ionic Liquids - Paving the Way to Renewable Chemicals

    DEFF Research Database (Denmark)

    Ståhlberg, Tim; Fu, Wenjing; Woodley, John

    2011-01-01

    The synthesis of 5-(hydroxymethyl)furfural (HMF) in ionic liquids is a field that has grown rapidly in recent years. Unique dissolving properties for crude biomass in combination with a high selectivity for HMF formation from hexose sugars make ionic liquids attractive reaction media for the prod......The synthesis of 5-(hydroxymethyl)furfural (HMF) in ionic liquids is a field that has grown rapidly in recent years. Unique dissolving properties for crude biomass in combination with a high selectivity for HMF formation from hexose sugars make ionic liquids attractive reaction media...... for the production of chemicals from renewable resources. A wide range of new catalytic systems that are unique for the transformation of glucose and fructose to HMF in ionic liquids has been found. However, literature examples of scale-up and process development are still scarce, and future research needs...... directions in process technology....

  10. Synthesis and Characterization of a Gd-DOTA-D-Permeation Peptide for Magnetic Resonance Relaxation Enhancement of Intracellular Targets

    Directory of Open Access Journals (Sweden)

    Andrew M. Prantner

    2003-10-01

    Full Text Available Many MR contrast agents have been developed and proven effective for extracellular nontargeted applications, but exploitation of intracellular MR contrast agents has been elusive due to the permeability barrier of the plasma membrane. Peptide transduction domains can circumvent this permeability barrier and deliver cargo molecules to the cell interior. Based upon enhanced cellular uptake of permeation peptides with D-amino acid residues, an all-D Tat basic domain peptide was conjugated to DOTA and chelated to gadolinium. Gd-DOTA-D-Tat peptide in serum at room temperature showed a relaxivity of 7.94 ± 0.11 mM−1 sec−1 at 4.7 T. The peptide complex displayed no significant binding to serum proteins, was efficiently internalized by human Jurkat leukemia cells resulting in intracellular T1 relaxation enhancement, and in preliminary T1-weighted MRI experiments, significantly enhanced liver, kidney, and mesenteric signals.

  11. Antimicrobial Peptides in 2014

    Directory of Open Access Journals (Sweden)

    Guangshun Wang

    2015-03-01

    Full Text Available This article highlights new members, novel mechanisms of action, new functions, and interesting applications of antimicrobial peptides reported in 2014. As of December 2014, over 100 new peptides were registered into the Antimicrobial Peptide Database, increasing the total number of entries to 2493. Unique antimicrobial peptides have been identified from marine bacteria, fungi, and plants. Environmental conditions clearly influence peptide activity or function. Human α-defensin HD-6 is only antimicrobial under reduced conditions. The pH-dependent oligomerization of human cathelicidin LL-37 is linked to double-stranded RNA delivery to endosomes, where the acidic pH triggers the dissociation of the peptide aggregate to release its cargo. Proline-rich peptides, previously known to bind to heat shock proteins, are shown to inhibit protein synthesis. A model antimicrobial peptide is demonstrated to have multiple hits on bacteria, including surface protein delocalization. While cell surface modification to decrease cationic peptide binding is a recognized resistance mechanism for pathogenic bacteria, it is also used as a survival strategy for commensal bacteria. The year 2014 also witnessed continued efforts in exploiting potential applications of antimicrobial peptides. We highlight 3D structure-based design of peptide antimicrobials and vaccines, surface coating, delivery systems, and microbial detection devices involving antimicrobial peptides. The 2014 results also support that combination therapy is preferred over monotherapy in treating biofilms.

  12. Procedures of amino acid sequencing of peptides in natural proteins collection of knowledge and intelligence for construction of reliable chemical inference system

    OpenAIRE

    Kudo, Yoshihiro; Kanaya, Shigehiko

    1994-01-01

    In order to establish a reliable chemical inference system on amino acid sequencing of natural peptides, as various kinds of relevant knowledge and intelligence as possible are collected. Topics are on didemnins, dolastatin 3, TL-119 and/or A-3302-B, mycosubtilin, patellamide A, duramycin (and cinnamycin), bottoromycin A 2, A19009, galantin I, vancomycin, stenothricin, calf speleen profilin, neocarzinostatin, pancreatic spasmolytic polypeptide, cerebratulus toxin B-IV, RNAase U 2, ferredoxin ...

  13. Synthesis of neodymium hydroxide nanotubes and nanorods by soft chemical process.

    Science.gov (United States)

    Shi, Weidong; Yu, Jiangbo; Wang, Haishui; Yang, Jianhui; Zhang, Hongjie

    2006-08-01

    A facile soft chemical approach using cetyltrimethylammonium bromide (CTAB) as template is successfully designed for synthesis of neodymium hydroxide nanotubes. These nanotubes have an average outer diameter around 20 nm, inner diameter around 2 nm, and length ranging from 100 to 120 nm, high BET surface area of 495.71 m(2) g(-1). We also find that neodymium hydroxide nanorods would be obtained when CTAB absented in reaction system. The Nd(OH)3 nanorods might act as precursors that are converted into Nd2O3 nanorods through dehydration at 550 degrees C. The nanorods could exhibit upconversion emission characteristic under excitation of 591 nm at room temperature.

  14. [Synthesis and physico-chemical properties of lonazolac-Ca, a new antiphlogistic/antirheumatic agent].

    Science.gov (United States)

    Rainer, G; Krüger, U; Klemm, K

    1981-01-01

    Calcium-[3-(p-chlorophenyl)-1-phenylpyrazole-4]-acetate (Lonazolac-Ca, active principle of Irritren) is a new antiinflammatory/antirheumatic agent whose synthesis and physico-chemical properties are described. The physical parameters measured (pKa, partition coefficient P, saturation concentration Cs, surface activity, protein binding) are held against the corresponding values of indomethacin, diclofenac, and phenylbutazone. The size of the permeability coefficient PM of the passive transport through artificial phospholipid collodion membranes as well as the invasion curves calculated from PM indicate a good absorption of lonazolac in man.

  15. Chemical solution synthesis and ferromagnetic resonance of epitaxial thin films of yttrium iron garnet

    Science.gov (United States)

    Lucas, Irene; Jiménez-Cavero, Pilar; Vila-Fungueiriño, J. M.; Magén, Cesar; Sangiao, Soraya; de Teresa, José Maria; Morellón, Luis; Rivadulla, Francisco

    2017-12-01

    We report the fabrication of epitaxial Y3F e5O12 (YIG) thin films on G d3G a5O12 (111) using a chemical solution method. Cubic YIG is a ferrimagnetic material at room temperature, with excellent magneto-optical properties, high electrical resistivity, and a very narrow ferromagnetic resonance, which makes it particularly suitable for applications in filters and resonators at microwave frequencies. But these properties depend on the precise stoichiometry and distribution of F e3 + ions among the octahedral/tetrahedral sites of a complex structure, which hampered the production of high-quality YIG thin films by affordable chemical methods. Here we report the chemical solution synthesis of YIG thin films, with excellent chemical, crystalline, and magnetic homogeneity. The films show a very narrow ferromagnetic resonance (long spin relaxation time), comparable to that obtained from high-vacuum physical deposition methods. These results demonstrate that chemical methods can compete to develop nanometer-thick YIG films with the quality required for spintronic devices and other high-frequency applications.

  16. Design, synthesis and DNA interactions of a chimera between a platinum complex and an IHF mimicking peptide.

    Science.gov (United States)

    Rao, Harita; Damian, Mariana S; Alshiekh, Alak; Elmroth, Sofi K C; Diederichsen, Ulf

    2015-12-28

    Conjugation of metal complexes with peptide scaffolds possessing high DNA binding affinity has shown to modulate their biological activities and to enhance their interaction with DNA. In this work, a platinum complex/peptide chimera was synthesized based on a model of the Integration Host Factor (IHF), an architectural protein possessing sequence specific DNA binding and bending abilities through its interaction with a minor groove. The model peptide consists of a cyclic unit resembling the minor grove binding subdomain of IHF, a positively charged lysine dendrimer for electrostatic interactions with the DNA phosphate backbone and a flexible glycine linker tethering the two units. A norvaline derived artificial amino acid was designed to contain a dimethylethylenediamine as a bidentate platinum chelating unit, and introduced into the IHF mimicking peptides. The interaction of the chimeric peptides with various DNA sequences was studied by utilizing the following experiments: thermal melting studies, agarose gel electrophoresis for plasmid DNA unwinding experiments, and native and denaturing gel electrophoresis to visualize non-covalent and covalent peptide-DNA adducts, respectively. By incorporation of the platinum metal center within the model peptide mimicking IHF we have attempted to improve its specificity and DNA targeting ability, particularly towards those sequences containing adjacent guanine residues.

  17. Skin peptide tyrosine-tyrosine, a member of the pancreatic polypeptide family: isolation, structure, synthesis, and endocrine activity.

    Science.gov (United States)

    Mor, A; Chartrel, N; Vaudry, H; Nicolas, P

    1994-10-25

    Pancreatic polypeptide, peptide tyrosine-tyrosine (PYY), and neuropeptide tyrosine (NPY), three members of a family of structurally related peptides, are mainly expressed in the endocrine pancreas, in endocrine cells of the gut, and in the brain, respectively. In the present study, we have isolated a peptide of the pancreatic polypeptide family from the skin of the South American arboreal frog Phyllomedusa bicolor. The primary structure of the peptide was established as Tyr-Pro-Pro-Lys-Pro-Glu-Ser-Pro-Gly-Glu10-Asp-Ala-Ser-Pro-Glu-Glu- Met-Asn- Lys-Tyr20-Leu-Thr-Ala-Leu-Arg-His-Tyr-Ile-Asn-Leu30-Val-Thr- Arg-Gln-Arg-Tyr-NH2 . This unusual peptide, named skin peptide tyrosine-tyrosine (SPYY), exhibits 94% similarity with PYY from the frog Rana ridibunda. A synthetic replicate of SPYY inhibits melanotropin release from perifused frog neurointermediate lobes in very much the same way as NPY. These results demonstrate the occurrence of a PYY-like peptide in frog skin. Our data also suggest the existence of a pituitary-skin regulatory loop in amphibians.

  18. On-resin N-formylation of peptides: a head-to-head comparison of reagents in solid-phase synthesis of ligands for formyl peptide receptors

    DEFF Research Database (Denmark)

    Christensen, Simon Bendt; Hansen, Anna Mette; Franzyk, Henrik

    2017-01-01

    General conditions for efficient on-resin N-formylation of peptides were identified by screening of a number of reagents comprising aliphatic formates (ethyl formate, 2,2,2-trifluoroethyl formate, and cyanomethyl formate), aromatic esters (phenyl formate and p-nitrophenyl formate), and N-formylim...... available activated ester p-nitrophenyl formate proved to be most convenient and versatile as high formylation degrees were obtained after 1–3 h at room temperature, while either conventional or microwave-assisted heating allowed reduction of the formylation time to 20 min....

  19. Chemical Genomic Screening of a Saccharomyces cerevisiae Genomewide Mutant Collection Reveals Genes Required for Defense against Four Antimicrobial Peptides Derived from Proteins Found in Human Saliva

    Science.gov (United States)

    Bhatt, Sanjay; Schoenly, Nathan E.; Lee, Anna Y.; Nislow, Corey; Bobek, Libuse A.

    2013-01-01

    To compare the effects of four antimicrobial peptides (MUC7 12-mer, histatin 12-mer, cathelicidin KR20, and a peptide containing lactoferricin amino acids 1 to 11) on the yeast Saccharomyces cerevisiae, we employed a genomewide fitness screen of combined collections of mutants with homozygous deletions of nonessential genes and heterozygous deletions of essential genes. When an arbitrary fitness score cutoffs of 1 (indicating a fitness defect, or hypersensitivity) and −1 (indicating a fitness gain, or resistance) was used, 425 of the 5,902 mutants tested exhibited altered fitness when treated with at least one peptide. Functional analysis of the 425 strains revealed enrichment among the identified deletions in gene groups associated with the Gene Ontology (GO) terms “ribosomal subunit,” “ribosome biogenesis,” “protein glycosylation,” “vacuolar transport,” “Golgi vesicle transport,” “negative regulation of transcription,” and others. Fitness profiles of all four tested peptides were highly similar, particularly among mutant strains exhibiting the greatest fitness defects. The latter group included deletions in several genes involved in induction of the RIM101 signaling pathway, including several components of the ESCRT sorting machinery. The RIM101 signaling regulates response of yeasts to alkaline and neutral pH and high salts, and our data indicate that this pathway also plays a prominent role in regulating protective measures against all four tested peptides. In summary, the results of the chemical genomic screens of S. cerevisiae mutant collection suggest that the four antimicrobial peptides, despite their differences in structure and physical properties, share many interactions with S. cerevisiae cells and consequently a high degree of similarity between their modes of action. PMID:23208710

  20. In situ chemical synthesis of ruthenium oxide/reduced graphene oxide nanocomposites for electrochemical capacitor applications.

    Science.gov (United States)

    Kim, Ji-Young; Kim, Kwang-Heon; Yoon, Seung-Beom; Kim, Hyun-Kyung; Park, Sang-Hoon; Kim, Kwang-Bum

    2013-08-07

    An in situ chemical synthesis approach has been developed to prepare ruthenium oxide/reduced graphene oxide (RGO) nanocomposites. It is found that as the C/O ratio increases, the number density of RuO2 nanoparticles decreases, because the chemical interaction between the Ru ions and the oxygen-containing functional groups provides anchoring sites where the nucleation of particles takes place. For electrochemical capacitor applications, the microwave-hydrothermal process was carried out to improve the conductivity of RGO in RuO2/RGO nanocomposites. The significant improvement in capacitance and high rate capability might result from the RuO2 nanoparticles used as spacers that make the interior layers of the reduced graphene oxide electrode available for electrolyte access.

  1. Room temperature synthesis and characterization of CdO nanowires by chemical bath deposition (CBD) method

    International Nuclear Information System (INIS)

    Dhawale, D.S.; More, A.M.; Latthe, S.S.; Rajpure, K.Y.; Lokhande, C.D.

    2008-01-01

    A chemical synthesis process for the fabrication of CdO nanowires is described. In the present work, transparent and conductive CdO films were synthesized on the glass substrate using chemical bath deposition (CBD) at room temperature. These films were annealed in air at 623 K and characterized for the structural, morphological, optical and electrical properties were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), optical and electrical resistivity. The XRD analysis showed that the as-deposited amorphous can be converted in to polycrystalline after annealing. Annealed CdO nanowires are 60-65 nm in diameter and length ranges typically from 2.5 to 3 μm. The optical properties revealed the presence of direct and indirect band gaps with energies 2.42 and 2.04 eV, respectively. Electrical resistivity measurement showed semiconducting behavior and thermoemf measurement showed n-type electrical conductivity

  2. Synthesis of Renewable Lubricant Alkanes from Biomass-Derived Platform Chemicals.

    Science.gov (United States)

    Gu, Mengyuan; Xia, Qineng; Liu, Xiaohui; Guo, Yong; Wang, Yanqin

    2017-10-23

    The catalytic synthesis of liquid alkanes from renewable biomass has received tremendous attention in recent years. However, bio-based platform chemicals have not to date been exploited for the synthesis of highly branched lubricant alkanes, which are currently produced by hydrocracking and hydroisomerization of long-chain n-paraffins. A selective catalytic synthetic route has been developed for the production of highly branched C 23 alkanes as lubricant base oil components from biomass-derived furfural and acetone through a sequential four-step process, including aldol condensation of furfural with acetone to produce a C 13 double adduct, selective hydrogenation of the adduct to a C 13 ketone, followed by a second condensation of the C 13 ketone with furfural to generate a C 23 aldol adduct, and finally hydrodeoxygenation to give highly branched C 23 alkanes in 50.6 % overall yield from furfural. This work opens a general strategy for the synthesis of high-quality lubricant alkanes from renewable biomass. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Novel DOTA-based prochelator for divalent peptide vectorization: synthesis of dimeric bombesin analogues for multimodality tumor imaging and therapy.

    Science.gov (United States)

    Abiraj, Keelara; Jaccard, Hugues; Kretzschmar, Martin; Helm, Lothar; Maecke, Helmut R

    2008-07-28

    Dimeric peptidic vectors, obtained by the divalent grafting of bombesin analogues on a newly synthesized DOTA-based prochelator, showed improved qualities as tumor targeted imaging probes in comparison to their monomeric analogues.

  4. Five Decades with Polyunsaturated Fatty Acids: Chemical Synthesis, Enzymatic Formation, Lipid Peroxidation and Its Biological Effects

    Directory of Open Access Journals (Sweden)

    Angel Catalá

    2013-01-01

    Full Text Available I have been involved in research on polyunsaturated fatty acids since 1964 and this review is intended to cover some of the most important aspects of this work. Polyunsaturated fatty acids have followed me during my whole scientific career and I have published a number of studies concerned with different aspects of them such as chemical synthesis, enzymatic formation, metabolism, transport, physical, chemical, and catalytic properties of a reconstructed desaturase system in liposomes, lipid peroxidation, and their effects. The first project I became involved in was the organic synthesis of [1-14C] eicosa-11,14-dienoic acid, with the aim of demonstrating the participation of that compound as a possible intermediary in the biosynthesis of arachidonic acid “in vivo.” From 1966 to 1982, I was involved in several projects that study the metabolism of polyunsaturated fatty acids. In the eighties, we studied fatty acid binding protein. From 1990 up to now, our laboratory has been interested in the lipid peroxidation of biological membranes from various tissues and different species as well as liposomes prepared with phospholipids rich in PUFAs. We tested the effect of many antioxidants such as alpha tocopherol, vitamin A, melatonin and its structural analogues, and conjugated linoleic acid, among others.

  5. Development of catalytic materials for the synthesis of valuable chemical products via multifunctional and multisite reactions

    International Nuclear Information System (INIS)

    Apesteguia, C.R; Padro, C.L; Diez, V.K; Di Cosimo, J.I; Trasarti, A.F; Marchi, A.J

    2004-01-01

    This work reports on the successful development of solid catalytic materials carried out by our working group to obtain fine high yield chemical products. Specifically, a report is made of i) the development of metal/acid bi-functional catalysts to obtain racemic menthol from citral in a one step liquid phase process. This menthol is one of the most important chemical flavouring compounds in industry; ii) The use of acid zeolites containing a balanced concentration of Bronsted and Lewis heavy acid sites, which allow the selective synthesis of o-hydroxy acetophenone from the gas phase acylation of phenol with acetic acid. The o-hydroxy acetophenone is an intermediate compound in the production of 4-hydroxy coumarin and warfarin that are used as anticoagulants drugs; iii) The use of mixed MgAl x O y oxides containing dual acid-basic sites (Mg 2- O 2- and Al 3+ -O 2- ) to synthesize isoforone from acetone in gas phase. The isoforone is an intermediate key in the synthesis of vitamin E (CW)

  6. Synthesis and Characterization of Carbon nanofibers on Co and Cu Catalysts by Chemical Vapor Deposition

    International Nuclear Information System (INIS)

    Park, Eunsil; Kim, Jongwon; Lee, Changseop

    2014-01-01

    This study reports on the synthesis of carbon nanofibers via chemical vapor deposition using Co and Cu as catalysts. In order to investigate the suitability of their catalytic activity for the growth of nanofibers, we prepared catalysts for the synthesis of carbon nanofibers with Cobalt nitrate and Copper nitrate, and found the optimum concentration of each respective catalyst. Then we made them react with Aluminum nitrate and Ammonium Molybdate to form precipitates. The precipitates were dried at a temperature of 110 .deg. C in order to be prepared into catalyst powder. The catalyst was sparsely and thinly spread on a quartz tube boat to grow carbon nanofibers via thermal chemical vapor deposition. The characteristics of the synthesized carbon nanofibers were analyzed through SEM, EDS, XRD, Raman, XPS, and TG/DTA, and the specific surface area was measured via BET. Consequently, the characteristics of the synthesized carbon nanofibers were greatly influenced by the concentration ratio of metal catalysts. In particular, uniform carbon nanofibers of 27 nm in diameter grew when the concentration ratio of Co and Cu was 6:4 at 700 .deg. C of calcination temperature; carbon nanofibers synthesized under such conditions showed the best crystallizability, compared to carbon nanofibers synthesized with metal catalysts under different concentration ratios, and revealed 1.26 high amorphicity as well as 292 m 2 g -1 high specific surface area

  7. Influence of the synthesis parameters on the physico-chemical and catalytic properties of cerium oxide for application in the synthesis of diethyl carbonate

    International Nuclear Information System (INIS)

    Leino, Ewelina; Kumar, Narendra; Mäki-Arvela, Päivi; Aho, Atte; Kordás, Krisztián; Leino, Anne-Riikka; Shchukarev, Andrey; Murzin, Dmitry Yu.; Mikkola, Jyri-Pekka

    2013-01-01

    Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO 2 properties was discussed. Moreover, the comparison of CeO 2 samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO 2 . Significant variations in physico-chemical properties of CeO 2 by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO 2 catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO 2 using butylene oxide as a dehydrating agent. The dependence of CeO 2 properties on its catalytic activity is evaluated in detail. - Highlights: • Synthesis of cerium (IV) oxide by precipitation method. • Influence of synthesis time, calcination temperature, mode of stirring and solution pH on properties. • Characterization by XRD, SEM, TEM, nitrogen physisorption, XPS, FTIR. • Catalytic performance diethyl carbonate synthesis from ethanol and CO 2

  8. Synthesis of E7 peptide-modified biodegradable polyester with the improving affinity to mesenchymal stem cells

    International Nuclear Information System (INIS)

    Li, Qian; Xing, Dongming; Ma, Lie; Gao, Changyou

    2017-01-01

    As the most promising stem cell, bone marrow-derived mesenchymal stem cells (BMSCs) has attracted many attentions and applied widely in regenerative medicine. A biodegradable polyester with tunable affinity to BMSCs plays critical role in determining the properties of the BMSCs-based constructs. In this study, maleimide functionalized biodegradable polyester (P(MTMC-LA)) was synthesized through ring-opening copolymerization between L-lactide (LA) and furan-maleimide functionalized trimethylene carbonate (FMTMC) and a subsequent retro Diels-Alder reaction. P(MTMC-LA) was modified by different amounts of BMSCs specific affinity peptide (EPLQLKM, E7) through click-chemistry to investigate the effect on BMSCs. The E7 peptide modified P(MTMC-LA) was casted into films on glass slides and BMSCs were seeded onto the films. In vitro study showed that E7 peptide modified P(MTMC-LA) films supported BMSCs adhesion and proliferation compared to unmodified P(MTMC-LA) film. Besides, the adhesion and proliferation were enhanced by the increasing peptide grafting ratio. These results indicated that the novel biodegradable polyester can serve as a biomaterial with great potential application in tissue engineering and regenerative medicine. - Highlights: • P(MTMC-LA) was synthesized through ring-opening copolymerization and retro Diels-Alder reaction. • P(MTMC-LA) was modified by dBMSCs specific affinity peptide (EPLQLKM, E7) through click-chemistry. • E7 peptide modified P(MTMC-LA) films supported BMSCs adhesion and proliferation.

  9. Synthesis of E7 peptide-modified biodegradable polyester with the improving affinity to mesenchymal stem cells

    Energy Technology Data Exchange (ETDEWEB)

    Li, Qian; Xing, Dongming; Ma, Lie, E-mail: liema@zju.edu.cn; Gao, Changyou

    2017-04-01

    As the most promising stem cell, bone marrow-derived mesenchymal stem cells (BMSCs) has attracted many attentions and applied widely in regenerative medicine. A biodegradable polyester with tunable affinity to BMSCs plays critical role in determining the properties of the BMSCs-based constructs. In this study, maleimide functionalized biodegradable polyester (P(MTMC-LA)) was synthesized through ring-opening copolymerization between L-lactide (LA) and furan-maleimide functionalized trimethylene carbonate (FMTMC) and a subsequent retro Diels-Alder reaction. P(MTMC-LA) was modified by different amounts of BMSCs specific affinity peptide (EPLQLKM, E7) through click-chemistry to investigate the effect on BMSCs. The E7 peptide modified P(MTMC-LA) was casted into films on glass slides and BMSCs were seeded onto the films. In vitro study showed that E7 peptide modified P(MTMC-LA) films supported BMSCs adhesion and proliferation compared to unmodified P(MTMC-LA) film. Besides, the adhesion and proliferation were enhanced by the increasing peptide grafting ratio. These results indicated that the novel biodegradable polyester can serve as a biomaterial with great potential application in tissue engineering and regenerative medicine. - Highlights: • P(MTMC-LA) was synthesized through ring-opening copolymerization and retro Diels-Alder reaction. • P(MTMC-LA) was modified by dBMSCs specific affinity peptide (EPLQLKM, E7) through click-chemistry. • E7 peptide modified P(MTMC-LA) films supported BMSCs adhesion and proliferation.

  10. Structure, synthesis, and activity of dermaseptin b, a novel vertebrate defensive peptide from frog skin: relationship with adenoregulin.

    Science.gov (United States)

    Mor, A; Amiche, M; Nicolas, P

    1994-05-31

    A novel antimicrobial peptide, designated dermaseptin b, was isolated from the skin of the arboreal frog Phyllomedusa bicolor. This 27-residue peptide amide is basic, containing 3 lysine residues that punctuate an alternating hydrophobic and hydrophilic sequence. In helix-inducing solvent, dermaseptin b adopts an amphipathic alpha-helical conformation that most closely resembles class L amphipathic helixes, with all lysine residues on the polar face of the helix. The peptide exhibits growth inhibition activity in vitro against a broad spectrum of pathogenic microorganisms including yeast and bacteria as well as various filamentous fungi that are responsible for severe opportunistic infections accompanying acquired immunodeficiency syndrome and the use of immunosuppressive agents. Maximized pairwise sequence alignment of dermaseptin b and dermaseptin s, a 34-residue antimicrobial peptide previously isolated from Phyllomedusa sauvagii, reveals 81% amino acid identity. No other significant similarity was found between dermaseptin b and any prokaryotic or eukaryotic protein, but similarity was found with adenoregulin (38% amino acid postional identity), a 33-residue peptide that enhances binding of agonists to the A1 adenosine receptor. The synthetic replicates of dermaseptin b and adenoregulin displayed similar but nonidentical spectra of antimicrobial activity, and both peptides were devoid of lytic effect on mammalian cells. Accordingly, the observation that adenoregulin enhances binding of agonists to the adenosine receptor may in fact be a consequence of its ability to alter the structure of biological membranes and to produce signal transduction via interactions with the lipid bilayer, bypassing cell surface receptor interactions.

  11. Room temperature synthesis of porous SiO2 thin films by plasma enhanced chemical vapor deposition

    OpenAIRE

    Barranco Quero, Ángel; Cotrino Bautista, José; Yubero Valencia, Francisco; Espinós, J. P.; Rodríguez González-Elipe, Agustín

    2004-01-01

    Synthesis of porous SiO2 thin films in room temperature was carried out using plasma enhanced chemical vapor deposition (CVD) in an electron cyclotron resonance microwave reactor with a downstream configuration.The gas adsorption properties and the type of porosity of the SiO2 thin films were assessed by adsorption isotherms of toluene at room temperature.The method could also permit the tailoring synthesis of thin films when both composition and porosity can be simultaneously and independent...

  12. A review of engineering aspects of intensification of chemical synthesis using ultrasound.

    Science.gov (United States)

    Sancheti, Sonam V; Gogate, Parag R

    2017-05-01

    Cavitation generated using ultrasound can enhance the rates of several chemical reactions giving better selectivity based on the physical and chemical effects. The present review focuses on overview of the different reactions that can be intensified using ultrasound followed by the discussion on the chemical kinetics for ultrasound assisted reactions, engineering aspects related to reactor designs and effect of operating parameters on the degree of intensification obtained for chemical synthesis. The cavitational effects in terms of magnitudes of collapse temperatures and collapse pressure, number of free radicals generated and extent of turbulence are strongly dependent on the operating parameters such as ultrasonic power, frequency, duty cycle, temperature as well as physicochemical parameters of liquid medium which controls the inception of cavitation. Guidelines have been presented for the optimum selection based on the critical analysis of the existing literature so that maximum process intensification benefits can be obtained. Different reactor designs have also been analyzed with guidelines for efficient scale up of the sonochemical reactor, which would be dependent on the type of reaction, controlling mechanism of reaction, catalyst and activation energy requirements. Overall, it has been established that sonochemistry offers considerable potential for green and sustainable processing and efficient scale up procedures are required so as to harness the effects at actual commercial level. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Chemical synthesis of porous web-structured CdS thin films for photosensor applications

    Energy Technology Data Exchange (ETDEWEB)

    Gosavi, S.R., E-mail: srgosavi.taloda@gmail.com [C. H. C. Arts, S. G. P. Commerce, and B. B. J. P. Science College, Taloda, Dist., Nandurbar 425413, M. S. (India); Nikam, C.P. [B.S.S.P.M.S. Arts, Commerce and Science College, Songir, Dist., Dhule 424309, M. S. (India); Shelke, A.R.; Patil, A.M. [Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Ryu, S.-W. [Department of Physics, Chonnam National University, Gwangju 500-757 (Korea, Republic of); Bhat, J.S. [Department of Physics, Karnatak University, Dharwad 580003 (India); Deshpande, N.G., E-mail: nicedeshpande@yahoo.co.in [Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2015-06-15

    The photo-activity of chemically deposited cadmium sulphide (CdS) thin film has been studied. The simple chemical route nucleates the CdS films with size up to the mean free path of the electron. Growth Kinematics of crystalline hexagonal CdS phase in the thin film form was monitored using X-ray diffraction. The time limitation set for the formation of the amorphous/nano-crystalline material is 40 and 60 min. Thereafter enhancement of the crystalline orientation along the desired plane was identified. Web-like porous structured surface morphology of CdS thin film over the entire area is observed. With decrease in synthesis time, increase of band gap energy i.e., a blue spectral shift was seen. The activation energy of CdS thin film at low and high temperature region was examined. It is considered that this activation energy corresponds to the donor levels associated with shallow traps or surface states of CdS thin film. The photo-electrochemical performance of CdS thin films in polysulphide electrolyte showed diode-like characteristics. Exposure of light on the CdS electrode increases the photocurrent. This suggests the possibility of production of free carriers via excited ions and also the light harvesting mechanism due to porous web-structured morphology. These studies hint that the obtained CdS films can work as a photosensor. - Highlights: • Photoactivity of chemically synthesized cadmium sulphide (CdS) thin films was studied. • Web-like porous structured surface morphology of CdS thin film over the entire area was observed. • Blue spectral shift with lowering of the synthesis time suggests films can act as a window layer over the absorber layer. • Porous web-structured CdS thin films can be useful in light harvesting.

  14. Chemical synthesis of porous web-structured CdS thin films for photosensor applications

    International Nuclear Information System (INIS)

    Gosavi, S.R.; Nikam, C.P.; Shelke, A.R.; Patil, A.M.; Ryu, S.-W.; Bhat, J.S.; Deshpande, N.G.

    2015-01-01

    The photo-activity of chemically deposited cadmium sulphide (CdS) thin film has been studied. The simple chemical route nucleates the CdS films with size up to the mean free path of the electron. Growth Kinematics of crystalline hexagonal CdS phase in the thin film form was monitored using X-ray diffraction. The time limitation set for the formation of the amorphous/nano-crystalline material is 40 and 60 min. Thereafter enhancement of the crystalline orientation along the desired plane was identified. Web-like porous structured surface morphology of CdS thin film over the entire area is observed. With decrease in synthesis time, increase of band gap energy i.e., a blue spectral shift was seen. The activation energy of CdS thin film at low and high temperature region was examined. It is considered that this activation energy corresponds to the donor levels associated with shallow traps or surface states of CdS thin film. The photo-electrochemical performance of CdS thin films in polysulphide electrolyte showed diode-like characteristics. Exposure of light on the CdS electrode increases the photocurrent. This suggests the possibility of production of free carriers via excited ions and also the light harvesting mechanism due to porous web-structured morphology. These studies hint that the obtained CdS films can work as a photosensor. - Highlights: • Photoactivity of chemically synthesized cadmium sulphide (CdS) thin films was studied. • Web-like porous structured surface morphology of CdS thin film over the entire area was observed. • Blue spectral shift with lowering of the synthesis time suggests films can act as a window layer over the absorber layer. • Porous web-structured CdS thin films can be useful in light harvesting

  15. Biosynthesis of cardiac natriuretic peptides

    DEFF Research Database (Denmark)

    Goetze, Jens Peter

    2010-01-01

    Cardiac-derived peptide hormones were identified more than 25 years ago. An astonishing amount of clinical studies have established cardiac natriuretic peptides and their molecular precursors as useful markers of heart disease. In contrast to the clinical applications, the biogenesis of cardiac...... peptides has only been elucidated during the last decade. The cellular synthesis including amino acid modifications and proteolytic cleavages has proven considerably more complex than initially perceived. Consequently, the elimination phase of the peptide products in circulation is not yet well....... An inefficient post-translational prohormone maturation will also affect the biology of the cardiac natriuretic peptide system. This review aims at summarizing the myocardial synthesis of natriuretic peptides focusing on B-type natriuretic peptide, where new data has disclosed cardiac myocytes as highly...

  16. [Natriuretic peptides. History of discovery, chemical structure, mechanism of action and the removal routes. Basis of diagnostic and therapeutic use].

    Science.gov (United States)

    Stryjewski, Piotr J; Nessler, Bohdan; Cubera, Katarzyna; Nessler, Jadwiga

    2013-01-01

    Natriuretic peptides (NP) are the group of proteins synthesized and secreted by the mammalian heart. All the NP are synthesized from prohormones and have 17-amino acid cyclic structures containing two cysteine residues linked by internal disulphide bond. They are characterized by a wide range of actions, mainly through their membrane receptors. The NP regulate the water and electrolyte balance, blood pressure through their diuretic, natriuretic, and relaxating the vascular smooth muscles effects. They also affect the endocrine system and the nervous system. The neurohormonal regulation of blood circulation results are mainly based on antagonism with renin--angiotensin--aldosterone system. The NP representatives are: atrial natriuretic peptide (ANP), brain natriuretic peptide (BNP), C-type natriuretic peptide (CNP), urodilatine and (DNP) Dendroaspis natriuretic peptide, not found in the human body. According to the guidelines of the European Society of Cardiology determination of NT-proBNP level have found a use in the diagnosis of acute and chronic heart failure, risk stratification in acute coronary syndromes and pulmonary embolism. There are reports found in the literature, that demonstrate the usefulness of NT-proBNP determination in valvular, atrial fibrillation, and syncopes. Recombinant human ANP--Carperitid and BNP--Nesiritid, have already found a use in the adjunctive therapy of dyspnea in acute heart failure.

  17. SYNTHESIS AND PHYSICAL-CHEMICAL PROPERTIES OF WATER-SOLUBLE 3-BENZYLXANTHINE DERIVATIVES

    Directory of Open Access Journals (Sweden)

    K. V. Аleksandrova

    2015-04-01

    Full Text Available Introduction Nowadays, research of novel biological active compounds with low toxicity, are carried out among different classes of organic compounds of natural and synthetic genesis. One of the main ways of these studies is search of water-soluble compounds – convenient objects for pharmacological researches. In recent years researchers paid attention to xanthine derivatives, because of their high variativity of possible chemical modification and ability to form different salts with wide spectrum of biological action. Thus, among water-soluble xanthine derivatives were found compounds with pronounced antioxidant, diuretic and analeptic properties. Primary methods of obtaining water-soluble xanthine derivatives are direct interaction of bases with xanthine molecule or insertion basic or acidic residues in positions 7 or 8 of xanthine bicycle. According from the above, search of biologically active compounds among water-soluble substituted xanthines is prospective and actual. The aim of the study was development of synthetic ways of obtaining novel water-soluble derivatives of 3-benzyl-8-methylxanthine and studying their physical and chemical properties. Material and methods Melting points of obtained compounds were determined by capillary method on PTP (M device. ІR-spectra of synthesized compounds were recorded on the Bruker Alpha device (company «Bruker» – Germany on 4000-400 sm-1 with using console ATR (direct insertion of compound. 1Н NMR-spectra were recorded on the Varian Mercury VX-200 device (company «Varian» – USA solvent – (DMSO-d6, internal standart – ТМС. Elemental analysis was made on Elementar Vario L cube device. Chromatoraphic studies were made on the plates Sorbfil-AFV-UV (company «Sobrpolimer» –Russia. Systhems for chromatography: «acetone-propanol-2» in ratio 2:3, «propanol-2-benzene» in ratio 10:1 and exersized in UV-light in wave 200-300 nm. Results and discussion We developed methodic of synthesis

  18. Investigation of the role of NaBH4 in the chemical synthesis of gold nanorods

    International Nuclear Information System (INIS)

    Samal, Akshaya K.; Sreeprasad, Theruvakkattil S.; Pradeep, Thalappil

    2010-01-01

    An improvement in the previously reported seed-mediated chemical synthesis of gold nanorods (GNRs) is reported. Monodisperse GNRs have been synthesized in a one-step protocol. The addition of controlled quantity of sodium borohydride (NaBH 4 ) directly into the growth solution produced uniform GNRs, formed by in situ nucleation and growth. In order to arrive at the conclusion, we studied the formation of GNRs with various seeds, of metals of widely differing crystal structures, and there were no variations in the properties of the GNRs formed. The role of NaBH 4 in the growth of GNR, which has not been covered in previous reports, is discussed in detail. The dependence of longitudinal plasmon peak on the concentration of NaBH 4 is compared with the dependence of residual concentration of NaBH 4 in the seed solution, which is added to the growth solution in seed-mediated synthesis. The study shows that NaBH 4 plays an important role in the formation of GNRs. This proposed protocol offers a number of advantages: one-step preparation of GNRs, significant reduction in the preparation time to 10 min, high monodispersity of GNRs, and tailorability of the aspect ratio depending on NaBH 4 concentration. It is suggested that NaBH 4 added to the growth solution leads to in situ formation of the seed particles of the size of 3-5 nm which enables the growth of GNRs. The growth of GNRs suggested here is likely to have an impact on the preparation of other anisotropic structures. Our single-pot methodology makes the procedure directly adaptable for commercial-scale production of GNRs and for their synthesis even in undergraduate laboratories.

  19. Chemical probing of the human sirtuin 5 active site reveals its substrate acyl specificity and peptide-based inhibitors.

    Science.gov (United States)

    Roessler, Claudia; Nowak, Theresa; Pannek, Martin; Gertz, Melanie; Nguyen, Giang T T; Scharfe, Michael; Born, Ilona; Sippl, Wolfgang; Steegborn, Clemens; Schutkowski, Mike

    2014-09-26

    Sirtuins are NAD(+)-dependent deacetylases acting as sensors in metabolic pathways and stress response. In mammals there are seven isoforms. The mitochondrial sirtuin 5 is a weak deacetylase but a very efficient demalonylase and desuccinylase; however, its substrate acyl specificity has not been systematically analyzed. Herein, we investigated a carbamoyl phosphate synthetase 1 derived peptide substrate and modified the lysine side chain systematically to determine the acyl specificity of Sirt5. From that point we designed six potent peptide-based inhibitors that interact with the NAD(+) binding pocket. To characterize the interaction details causing the different substrate and inhibition properties we report several X-ray crystal structures of Sirt5 complexed with these peptides. Our results reveal the Sirt5 acyl selectivity and its molecular basis and enable the design of inhibitors for Sirt5. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Bio-electrochemical synthesis of commodity chemicals by autotrophic acetogens utilizing CO2 for environmental remediation.

    Science.gov (United States)

    Jabeen, Gugan; Farooq, Robina

    2016-09-01

    Bio-electrochemical synthesis (BES) is a technique in which electro-autotrophic bacteria such as Clostridium ljungdahlii utilize electric currents as an electron source from the cathode to reduce CO2 to extracellular, multicarbon, exquisite products through autotrophic conversion. The BES of volatile fatty acids and alcohols directly from CO2 is a sustainable alternative for non-renewable, petroleum-based polymer production. This conversion of CO2 implies reduction of greenhouse gas emissions. The synthesis of heptanoic acid, heptanol, hexanoic acid and hexanol, for the first time, by Clostridium ljungdahlii was a remarkable achievement of BES. In our study, these microorganisms were cultivated on the cathode of a bio-electrochemical cell at -400 mV by a DC power supply at 37 degree Centrigrade, pH 6.8, and was studied for both batch and continuous systems. Pre-enrichment of bio-cathode enhanced the electroactivity of cells and resulted in maximizing extracellular products in less time. The main aim of the research was to investigate the impact of low-cost substrate CO2, and the longer cathode recovery range was due to bacterial reduction of CO2 to multicarbon chemical commodities with electrons driven from the cathode. Reactor design was simplified for cost-effectiveness and to enhance energy efficiencies. The Columbic recovery of ethanoic acid, ethanol, ethyl butyrate, hexanoic acid, heptanoic acid and hexanol being in excess of 80 percent proved that BES was a remarkable technology.

  1. Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Moshalagae Motlatle, Abesach, E-mail: AMotlatle@csir.co.za; Kesavan Pillai, Sreejarani, E-mail: skpillai@csir.co.za; Rudolf Scriba, Manfred, E-mail: MRscriba@csir.co.za; Sinha Ray, Suprakas, E-mail: Rsuprakas@csir.co.za [Council for Scientific and Industrial Research, DST/CSIR Nanotechnology Innovation Centre, National Centre for Nano-Structured Materials (South Africa)

    2016-10-15

    Cu nanoparticles were synthesized using low-temperature aqueous reduction method at pH 3, 5, 7, 9 and 11 in presence of ascorbic acid and polyvinylpyrrolidone. The nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction techniques. Results demonstrated a strong dependence of synthesis pH on the size, shape, chemical composition and structure of Cu nanoparticles. While lower pH conditions of 3 and 5 produced Cu{sup 0}, higher pH levels (more than 7) led to the formation of Cu{sub 2}O/CuO nanoparticles. The reducing capacity of ascorbic acid, capping efficiency of PVP and the resulting particle sizes were strongly affected by solution pH. The results of in vitro disk diffusion tests showed excellent antimicrobial activity of Cu{sub 2}O/CuO nanoparticles against a mixture of bacterial strains (Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa), indicating that the size as well as oxidation state of Cu contributes to the antibacterial efficacy. The results indicate that varying synthesis pH is a strategy to tailor the composition, structure and properties of Cu nanoparticles.

  2. Laser-assisted chemical vapor deposition setup for fast synthesis of graphene patterns

    Science.gov (United States)

    Zhang, Chentao; Zhang, Jianhuan; Lin, Kun; Huang, Yuanqing

    2017-05-01

    An automatic setup based on the laser-assisted chemical vapor deposition method has been developed for the rapid synthesis of graphene patterns. The key components of this setup include a laser beam control and focusing unit, a laser spot monitoring unit, and a vacuum and flow control unit. A laser beam with precision control of laser power is focused on the surface of a nickel foil substrate by the laser beam control and focusing unit for localized heating. A rapid heating and cooling process at the localized region is induced by the relative movement between the focalized laser spot and the nickel foil substrate, which causes the decomposing of gaseous hydrocarbon and the out-diffusing of excess carbon atoms to form graphene patterns on the laser scanning path. All the fabrication parameters that affect the quality and number of graphene layers, such as laser power, laser spot size, laser scanning speed, pressure of vacuum chamber, and flow rates of gases, can be precisely controlled and monitored during the preparation of graphene patterns. A simulation of temperature distribution was carried out via the finite element method, providing a scientific guidance for the regulation of temperature distribution during experiments. A multi-layer graphene ribbon with few defects was synthesized to verify its performance of the rapid growth of high-quality graphene patterns. Furthermore, this setup has potential applications in other laser-based graphene synthesis and processing.

  3. Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

    Science.gov (United States)

    Usman, Muhammad Sani; Ibrahim, Nor Azowa; Shameli, Kamyar; Zainuddin, Norhazlin; Yunus, Wan Md Zin Wan

    2012-12-14

    Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

  4. Properties, synthesis, and growth mechanisms of carbon nanotubes with special focus on thermal chemical vapor deposition.

    Science.gov (United States)

    Nessim, Gilbert D

    2010-08-01

    Carbon nanotubes (CNTs) have been extensively investigated in the last decade because their superior properties could benefit many applications. However, CNTs have not yet made a major leap into industry, especially for electronic devices, because of fabrication challenges. This review provides an overview of state-of-the-art of CNT synthesis techniques and illustrates their major technical difficulties. It also charts possible in situ analyses and new reactor designs that might enable commercialization. After a brief description of the CNT properties and of the various techniques used to synthesize substrate-free CNTs, the bulk of this review analyzes chemical vapor deposition (CVD). This technique receives special attention since it allows CNTs to be grown in predefined locations, provides a certain degree of control of the types of CNTs grown, and may have the highest chance to succeed commercially. Understanding the primary growth mechanisms at play during CVD is critical for controlling the properties of the CNTs grown and remains the major hurdle to overcome. Various factors that influence CNT growth receive a special focus: choice of catalyst and substrate materials, source gases, and process parameters. This review illustrates important considerations for in situ characterization and new reactor designs that may enable researchers to better understand the physical growth mechanisms and to optimize the synthesis of CNTs, thus contributing to make carbon nanotubes a manufacturing reality.

  5. Ultrasonic-assisted chemical reduction synthesis and structural characterization of copper nanoparticles

    Science.gov (United States)

    Anh-Nga, Nguyen T.; Tuan-Anh, Nguyen; Thanh-Quoc, Nguyen; Ha, Do Tuong

    2018-04-01

    Copper nanoparticles, due to their special properties, small dimensions and low-cost preparation, have many potential applications such as in optical, electronics, catalysis, sensors, antibacterial agents. In this study, copper nanoparticles were synthesized by chemical reduction method with different conditions in order to investigate the optimum conditions which gave the smallest (particle diameter) dimensions. The synthesis step used copper (II) acetate salt as precursor, ascorbic acid as reducing agent, glycerin and polyvinylpyrrolidone (PVP) as protector and stabilizer. The assistance of ultrasonic was were considered as the significant factor affecting the size of the synthesized particles. The results showed that the copper nanoparticles have been successfully synthesized with the diameter as small as 20-40 nm and the conditions of ultrasonic waves were 48 kHz of frequency, 20 minutes of treated time and 65-70 °C of temperature. The synthesized copper nanoparticles were characterized by optical absorption spectrum, scanning electron microscopy (SEM), and Fourier Transform Infrared Spectrometry.

  6. Synthesis of Nickel and Nickel Hydroxide Nano powders by Simplified Chemical Reduction

    International Nuclear Information System (INIS)

    Tientong, J.; Garcia, S.; Thurber, C.R.; Golden, T.D.

    2014-01-01

    Nickel nano powders were synthesized by a chemical reduction of nickel ions with hydrazine hydrate at ph ∼ 12.5. Sonication of the solutions created a temperature of 54-65 °C to activate the reduction reaction of nickel nanoparticles. The solution ph affected the composition of the resulting nanoparticles. Nickel hydroxide nanoparticles were formed from an alkaline solution (ph ∼10) of nickel-hydrazine complexed by dropwise titration. X-ray diffraction of the powder and the analysis of the resulting Williamson-Hall plots revealed that the particle size of the powders ranged from 12 to 14 nm. Addition of polyvinylpyrrolidone into the synthesis decreased the nickel nanoparticle size to approximately 7 nm. Dynamic light scattering and scanning electron microscopy confirmed that the particles were in the nanometer range. The structure of the synthesized nickel and nickel hydroxide nanoparticles was identified by X-ray diffraction and Fourier transform infrared spectroscopy.

  7. Chemical synthesis, redox transformation, and identification of sonnerphenolic C, an antioxidant in Acer nikoense.

    Science.gov (United States)

    Iwadate, Takehiro; Nihei, Ken-Ichi

    2017-04-15

    Sonnerphenolic C (3), which was predicted in a redox product of epirhododendrin (1) isolated from Acer nikoense, was synthesized for the first time via the epimeric separation of benzylidene acetal intermediates as a key step. From a similar synthetic route, 1 was obtained concisely. As a result of their antioxidative evaluation, only 3 revealed potent activity. The redox transformation of 1 into 3 was achieved in the presence of tyrosinase and vitamin C. Moreover, 3 was identified in the decoction of A. nikoense by HPLC analysis with the effective use of synthesized 3. Thus, a novel naturally occurring antioxidant 3 was developed through the sequential flow including redox prediction, chemical synthesis, evaluation of the activity, and identification as the natural product. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    Science.gov (United States)

    Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

    2006-11-01

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

  9. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    Energy Technology Data Exchange (ETDEWEB)

    Kale, R.B. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: rb_kale@yahoo.co.in; Sartale, S.D. [Hahn Meitner Institute, Glienicker Strasse-100, D-14109 Berlin (Germany); Ganesan, V. [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452017 (India); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Lin, Y.-F. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China); Lu, S.-Y. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: sylu@mx.nthu.edu.tw

    2006-11-15

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH{sub 3}COO){sub 2} as Pb{sup 2+} and Na{sub 2}SeSO{sub 3} as Se{sup 2-} ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

  10. Size-controlled Synthesis and Characterization of Fe3O4 Nanoparticles by Chemical Coprecipitation Method

    International Nuclear Information System (INIS)

    Chia Chin Hua; Sarani Zakaria; Farahiyan, R.; Liew Tze Khong; Mustaffa Abdullah; Sahrim Ahmad; Nguyen, K.L.

    2008-01-01

    Magnetite (Fe 3 O 4 ) nanoparticles have been synthesized using the chemical coprecipitation method. The Fe 3 O 4 nanoparticles were likely formed via dissolution-recrystallization process. During the precipitation process, ferrihydrite and Fe(OH) 2 particles formed aggregates and followed by the formation of spherical Fe 3 O 4 particles. The synthesized Fe 3 O 4 nanoparticles exhibited superparamagnetic behavior and in single crystal form. The synthesis temperature and the degree of agitation during the precipitation were found to be decisive in controlling the crystallite and particle size of the produced Fe 3 O 4 nanoparticles. Lower temperature and higher degree of agitation were the favorable conditions for producing smaller particle. The magnetic properties (saturation magnetization and coercivity) of the Fe 3 O 4 nanoparticles increased with the particle size. (author)

  11. Alternative chemical-based synthesis routes and characterization of nano-scale particles

    International Nuclear Information System (INIS)

    Brocchi, E.A.; Motta, M.S.; Solorzano, I.G.; Jena, P.K.; Moura, F.J.

    2004-01-01

    Different nano-scale particles have been synthesized by alternative routes: nitrates dehydratation and oxide, or co-formed oxides, reduction by hydrogen. Chemical-based synthesis routes are described and thermodynamics studies and kinetics data are presented to support the feasibility for obtaining single-phase oxides and co-formed two-phase oxides. In addition, the reduction reaction has been applied to successfully produce metal/ceramic nanocomposites. Structural characterization has been carried out by means of X-ray diffraction and, more extensively, transmission electron microscopy operating in conventional diffraction contrast mode (CTEM) and high-resolution mode (HRTEM). Nano-scale size distribution of oxide particles is well demonstrated together with their defect-free structure in the lower range, around 20 nm, size. Structural features related to the synthesized nano-composites are also presented

  12. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    International Nuclear Information System (INIS)

    Kale, R.B.; Sartale, S.D.; Ganesan, V.; Lokhande, C.D.; Lin, Y.-F.; Lu, S.-Y.

    2006-01-01

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH 3 COO) 2 as Pb 2+ and Na 2 SeSO 3 as Se 2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV

  13. The New Mars Synthesis: A New Concept Of Mars Geo-Chemical History

    Science.gov (United States)

    Brandenburg, J. E.

    2005-02-01

    A new concept of Mars climatic and geo-chemical evolution is proposed, called the NMS (New Mars Synthesis) drawing on the full spectrum of available Mars data. The proposed synthesis is that Mars and Earth, having begun with similar surface conditions, did not strongly diverge from their similar paths 4.0 Billion years ago, in the Early Noachian, instead, under the NMS, they diverged much more recently in geologic time, in the Early Amazonian. Under the NMS, biology strongly affected the geo-chemical evolution of Mars, and allowed a stable and persistent greenhouse by producing a large oxygen component in the atmosphere. The NMS assumes Mars held biology form early on, has been geologically active throughout its history, that it had a northern paleo-ocean, that it has high, approximately, 4xLunar, cratering rates and that its climate changed recently in geologic time from being basically terrestrial to its present conditions. The proposed mechanism for the stability of the Mars greenhouse was a large oxygen component in the atmosphere that created acidic and highly oxidized conditions that prevented formation of Carbonates, and the thermal and gas buffering of the paleo-ocean. The greenhouse was thus biologically and hydrologically stabilized. The greenhouse was terminated by a large atmospheric cooling event in the Early Amazonian that killed the biosphere and froze the ocean stabilizing the greenhouse. This cooling event was probably caused by the formation of the Lyot impact basin. Given the long duration of this terrestrial biosphere in this NMS, the possible appearance of fossils in some rover images is not to be unexpected and the colonization of Mars by humanity may be aided extensive fossil biomass to use as raw material.

  14. Modified chemical synthesis of porous α-Sm{sub 2}S{sub 3} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Kumbhar, V.S.; Jagadale, A.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur, (M.S.) 416004 (India); Gaikwad, N.S. [Rayat Shikshan Sanstha, Satara, (M.S.) 415 001 (India); Lokhande, C.D., E-mail: l_chandrakant@yahoo.com [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur, (M.S.) 416004 (India)

    2014-08-15

    Highlights: • A novel chemical route to prepare α-Sm{sub 2}S{sub 3} thin films. • A porous honeycomb like morphology of the α-Sm{sub 2}S{sub 3} thin film. • An application of α-Sm{sub 2}S{sub 3} thin film toward its supercapacitive behaviour. - Abstract: The paper reports synthesis of porous α-Sm{sub 2}S{sub 3} thin films using modified chemical synthesis, also known as successive ionic layer adsorption and reaction (SILAR) method. The X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), atomic force microscopy (AFM), wettability and ultraviolet–visible spectroscopy (UV–vis) techniques are used for the study of structural, elemental, morphological and optical properties of α-Sm{sub 2}S{sub 3} films. An orthorhombic crystal structure of α-Sm{sub 2}S{sub 3} is resulted from XRD study. The SEM and AFM observations showed highly porous α-Sm{sub 2}S{sub 3} film surface. An optical band gap of 2.50 eV is estimated from optical absorption spectrum. The porous α-Sm{sub 2}S{sub 3} thin film tuned for supercapacitive behaviour using cyclic voltammetry and galvanostatic charge discharge showed a specific capacitance and energy density of 294 Fg{sup –1} and 48.9 kW kg{sup –1}, respectively in 1 M LiClO{sub 4}–propylene carbonate electrolyte.

  15. Synthesis of carbon nanotubes using the cobalt nanocatalyst by thermal chemical vapor deposition technique

    Energy Technology Data Exchange (ETDEWEB)

    Madani, S.S. [Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Zare, K. [Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Department of Chemistry, Shahid Beheshti University, Tehran (Iran, Islamic Republic of); Ghoranneviss, M. [Plasma Physics Research Center, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Salar Elahi, A., E-mail: Salari_phy@yahoo.com [Plasma Physics Research Center, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

    2015-11-05

    The three main synthesis methods of Carbon nanotubes (CNTs) are the arc discharge, the laser ablation and the chemical vapour deposition (CVD) with a special regard to the latter one. CNTs were produced on a silicon wafer by Thermal Chemical Vapor Deposition (TCVD) using acetylene as a carbon source, cobalt as a catalyst and ammonia as a reactive gas. The DC-sputtering system was used to prepare cobalt thin films on Si substrates. A series of experiments was carried out to investigate the effects of reaction temperature and deposition time on the synthesis of the nanotubes. The deposition time was selected as 15 and 25 min for all growth temperatures. Energy Dispersive X-ray (EDX) measurements were used to investigate the elemental composition of the Co nanocatalyst deposited on Si substrates. Atomic Force Microscopy (AFM) was used to characterize the surface topography of the Co nanocatalyst deposited on Si substrates. The as-grown CNTs were characterized under Field Emission Scanning Electron Microscopy (FESEM) to study the morphological properties of CNTs. Also, the grown CNTs have been investigated by High Resolution Transmission Electron Microscopy (HRTEM) and Raman spectroscopy. The results demonstrated that increasing the temperature leads to increasing the diameter of CNTs. The ideal reaction temperature was 850 °C and the deposition time was 15 min. - Graphical abstract: FESEM images of CNTs grown on the cobalt catalyst at growth temperatures of (a) 850 °C, (b) 900 °C, (c) 950 °C and (d) 1000 °C during the deposition time of 15 min. - Highlights: • Carbon nanotubes (CNTs) were produced on a silicon wafer by TCVD technique. • EDX and AFM were used to investigate the elemental composition and surface topography. • FESEM was used to study the morphological properties of CNTs. • The grown CNTs have been investigated by HRTEM and Raman spectroscopy.

  16. A rapid room temperature chemical route for the synthesis of graphene: metal-mediated reduction of graphene oxide.

    Science.gov (United States)

    Dey, Ramendra Sundar; Hajra, Saumen; Sahu, Ranjan K; Raj, C Retna; Panigrahi, M K

    2012-02-07

    A rapid and facile route for the synthesis of reduced graphene oxide sheets (rGOs) at room temperature by the chemical reduction of graphene oxide using Zn/acid in aqueous solution is demonstrated. This journal is © The Royal Society of Chemistry 2012

  17. Solid-phase-assisted synthesis of targeting peptide-PEG-oligo(ethane amino)amides for receptor-mediated gene delivery.

    Science.gov (United States)

    Martin, Irene; Dohmen, Christian; Mas-Moruno, Carlos; Troiber, Christina; Kos, Petra; Schaffert, David; Lächelt, Ulrich; Teixidó, Meritxell; Günther, Michael; Kessler, Horst; Giralt, Ernest; Wagner, Ernst

    2012-04-28

    In the forthcoming era of cancer gene therapy, efforts will be devoted to the development of new efficient and non-toxic gene delivery vectors. In this regard, the use of Fmoc/Boc-protected oligo(ethane amino)acids as building blocks for solid-phase-supported assembly represents a novel promising approach towards fully controlled syntheses of effective gene vectors. Here we report on the synthesis of defined polymers containing the following: (i) a plasmid DNA (pDNA) binding domain of eight succinoyl-tetraethylenpentamine (Stp) units and two terminal cysteine residues; (ii) a central polyethylene glycol (PEG) chain (with twenty-four oxyethylene units) for shielding; and (iii) specific peptides for targeting towards cancer cells. Peptides B6 and c(RGDfK), which bind transferrin receptor and α(v)β(3) integrin, respectively, were chosen because of the high expression of these receptors in many tumoral cells. This study shows the feasibility of designing these kinds of fully controlled vectors and their success for targeted pDNA-based gene transfer. This journal is © The Royal Society of Chemistry 2012

  18. Chemically stabilized reduced graphene oxide/zirconia nanocomposite: synthesis and characterization

    Science.gov (United States)

    Sagadevan, Suresh; Zaman Chowdhury, Zaira; Enamul Hoque, Md; Podder, Jiban

    2017-11-01

    In this research, chemical method was used to fabricate reduced graphene oxide/zirconia (rGO/ZrO2) nanocomposite. X-ray Diffraction analysis (XRD) was carried out to examine the crystalline structure of the nanocomposites. The nanocomposite prepared here has average crystallite size of 14 nm. The surface morphology was observed using scanning electron microscopic analysis (SEM) coupled with electron dispersion spectroscopy (EDS) to detect the chemical element over the surface of the nanocomposites. High-resolution Transmission electron microscopic analysis (HR-TEM) was carried out to determine the particle size and shape of the nanocomposites. The optical property of the prepared samples was determined using UV-visible absorption spectrum. The functional groups were identified using FTIR and Raman spectroscopic analysis. Efficient, cost effective and properly optimized synthesis process of rGO/ZrO2 nanocomposite can ensure the presence of infiltrating graphene network inside the ZrO2 matrix to enhance the electrical properties of the hybrid composites up to a greater scale. Thus the dielectric constant, dielectric loss and AC conductivity of the prepared sample was measured at various frequencies and temperatures. The analytical results obtained here confirmed the homogeneous dispersion of ZrO2 nanostructures over the surface of reduced graphene oxide nanosheets. Overall, the research demonstrated that the rGO/ZrO2 nano-hybrid structure fabricated here can be considered as a promising candidate for applications in nanoelectronics and optoelectronics.

  19. Synthesis of ZnO nanopencils using wet chemical method and its investigation as LPG sensor

    International Nuclear Information System (INIS)

    Shimpi, Navinchandra G.; Jain, Shilpa; Karmakar, Narayan; Shah, Akshara; Kothari, D.C.; Mishra, Satyendra

    2016-01-01

    Highlights: • Synthesis using a simple and cost-effective wet chemical process. • Uniform, monodispersed and pure nanoparticles. • Pencil shaped rods with sharp tips. • Understanding of Growth mechanism. • Efficient LPG sensing with high response. • Morphology dependent sensing. - Abstract: ZnO nanopencils (NPCs) were prepared by a novel wet chemical process, using triethanolamine (TEA) as a mild base, which is relatively simple and cost effective method as compared to hydrothermal method. ZnO NPCs were characterized using powder X-ray diffraction (XRD), Fourier Transform Infra-Red (FTIR) spectroscopy in mid-IR and far-IR regions, X-ray Photoelectron Spectroscopy (XPS), UV–vis (UV–vis) absorption spectroscopy, room temperature Photoluminescence (PL) spectroscopy and Field Emission Scanning Electron Microscopy (FESEM). ZnO NPCs obtained, were highly pure, uniform and monodispersed.XRD pattern indicated hexagonal unit cell structure with preferred orientation along the c-axis. Sensing behaviour of ZnO NPCs was studied towards Liquefied Petroleum Gas (LPG) at different operating temperatures. The study shows that ZnO NPCs were most sensitive and promising candidate for detection of LPG at 250 °C with gas sensitivity > 60%. The high response towards LPG is due to high surface area of ZnO NPCs and their parallel alignment.

  20. Synthesis of ZnO nanopencils using wet chemical method and its investigation as LPG sensor

    Energy Technology Data Exchange (ETDEWEB)

    Shimpi, Navinchandra G., E-mail: navin_shimpi@rediffmail.com [Department of Chemistry, University of Mumbai, Santacruz (East), Mumbai-400098 (India); Jain, Shilpa [Department of Chemistry, University of Mumbai, Santacruz (East), Mumbai-400098 (India); Karmakar, Narayan [Department of Physics, University of Mumbai, Santacruz (East), Mumbai-400098 (India); Shah, Akshara [Department of Chemistry, University of Mumbai, Santacruz (East), Mumbai-400098 (India); Kothari, D.C. [Department of Physics, University of Mumbai, Santacruz (East), Mumbai-400098 (India); National Centre for Nanosciences & Nanotechnology, University of Mumbai, Santacruz (East), Mumbai-400098 (India); Mishra, Satyendra [University Institute of Chemical Technology, North Maharashtra University, Jalgaon (India)

    2016-12-30

    Highlights: • Synthesis using a simple and cost-effective wet chemical process. • Uniform, monodispersed and pure nanoparticles. • Pencil shaped rods with sharp tips. • Understanding of Growth mechanism. • Efficient LPG sensing with high response. • Morphology dependent sensing. - Abstract: ZnO nanopencils (NPCs) were prepared by a novel wet chemical process, using triethanolamine (TEA) as a mild base, which is relatively simple and cost effective method as compared to hydrothermal method. ZnO NPCs were characterized using powder X-ray diffraction (XRD), Fourier Transform Infra-Red (FTIR) spectroscopy in mid-IR and far-IR regions, X-ray Photoelectron Spectroscopy (XPS), UV–vis (UV–vis) absorption spectroscopy, room temperature Photoluminescence (PL) spectroscopy and Field Emission Scanning Electron Microscopy (FESEM). ZnO NPCs obtained, were highly pure, uniform and monodispersed.XRD pattern indicated hexagonal unit cell structure with preferred orientation along the c-axis. Sensing behaviour of ZnO NPCs was studied towards Liquefied Petroleum Gas (LPG) at different operating temperatures. The study shows that ZnO NPCs were most sensitive and promising candidate for detection of LPG at 250 °C with gas sensitivity > 60%. The high response towards LPG is due to high surface area of ZnO NPCs and their parallel alignment.

  1. Chemical synthesis of Fe{sub 2}O{sub 3} thin films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Kulal, P.M.; Dubal, D.P.; Lokhande, C.D. [Holography and Material Research Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Fulari, V.J., E-mail: vijayfulari@gmail.com [Holography and Material Research Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2011-02-03

    Research highlights: > Simple chemical synthesis of Fe{sub 2}O{sub 3}. > Formation of amorphous and hydrous Fe{sub 2}O{sub 3}. > Potential candidate for supercapacitors. - Abstract: Fe{sub 2}O{sub 3} thin films have been prepared by novel chemical successive ionic layer adsorption and reaction (SILAR) method. Further these films were characterized for their structural, morphological and optical properties by means of X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrum, scanning electron microscopy (SEM), wettability test and optical absorption studies. The XRD pattern showed that the Fe{sub 2}O{sub 3} films exhibit amorphous in nature. Formation of iron oxide compound was confirmed from FTIR studies. The optical absorption showed existence of direct optical band gap of energy 2.2 eV. Fe{sub 2}O{sub 3} film surface showed superhydrophilic nature with water contact angle less than 10{sup o}. The supercapacitive properties of Fe{sub 2}O{sub 3} thin film investigated in 1 M NaOH electrolyte showed supercapacitance of 178 F g{sup -1} at scan rate 5 mV/s.

  2. Chemical synthesis of magnetic Fe-B and Fe-Co-B particles and chains

    International Nuclear Information System (INIS)

    Fulmer, P.; Kim, J.; Manthiram, A.; Sanchez, J.M.

    1999-04-01

    With an objective to develop magnetic materials with high saturation magnetization for the Magnetically Assisted Chemical Separation (MACS) process the chemical synthesis of Fe-B and Fe-Co-B alloys by reducing iron and cobalt chloride solutions with potassium borohydride has been investigated systematically. The influence of the concentration of the reactants, applied magnetic field, reaction atmosphere, and method of mixing the reactants on the microstructure, particle size, composition and magnetic properties has been studied. Both M-B (M = Fe and Co) particles and elongated chains composed of nanometer size M-B particles have been obtained depending on the reaction conditions. The Fe-B samples exhibit saturation magnetization of M S of 120--190 emu/g, remanent magnetization M r of 10--22 emu/g, and coercive field H c of 400--900 Oe. A high M S value of 190 emu/g, which is close to the theoretical value of 218 emu/g for pure Fe, has been achieved particularly for samples with well-defined chain structures. Increasing the Co content in the Fe-Co-B alloys increases the boron content and thereby decreases the crystallinity and M S values although marginal increase in H c (1,250 Oe) and M r (36 emu/g) values could be made in some Fe-Co-B compositions. The chain structure with high M S may be attractive for other magnetic separation processes as well

  3. The Synthesis of Silver Nanoparticles Produced by Chemical Reduction of Silver Salt Solution

    International Nuclear Information System (INIS)

    Sri Budi Harmani; Dewi Sondari; Agus Haryono

    2008-01-01

    Described in this research are the synthesis of silver nanoparticle produced by chemical reduction of silver salt (silver nitrate AgNO 3 ) solution. As a reducer, sodium citrate (C 6 H 5 O 7 Na 3 ) was used. Preparation of silver colloid is done by using chemical reduction method. In typical experiment 150 ml of 1.10 -3 M AgNO 3 solution was heated with temperature variation such as 90, 100, 110 degree of Celsius. To this solution 15 ml of 1 % trisodium citrate was added into solution drop by drop during heating. During the process, solution was mixed vigorously. Solution was heated until colour's change is evident (pale yellow solution is formed). Then it was removed from the heating element and stirred until cooled to room temperature. Experimental result showed that diameter of silver nanoparticles in colloid solution is about 28.3 nm (Ag colloid, 90 o C); 19.9 nm (Ag colloid, 100 o C)and 26.4 nm (Ag colloid, 110 o C). Characterization of the silver nanoparticle colloid conducted by using UV-Vis Spectroscopy, Particles Size Analyzer (PSA) and Scanning Electron Microscope (SEM) indicate the produced structures of silver nanoparticles. (author)

  4. Synthesis of Mn3O4 nanoparticles via chemical precipitation approach for supercapacitor application

    International Nuclear Information System (INIS)

    Gnana Sundara Raj, Balasubramaniam; Asiri, Abdullah M.; Wu, Jerry J.; Anandan, Sambandam

    2015-01-01

    Highlights: • Facile synthesis of Mn 3 O 4 nanoparticles at room temperature via simple chemical precipitation method. • Fabricated supercapacitor device shows maximum specific capacitance in 1 M Na 2 SO 4 . • 77% of specific capacitance is retained even after 1000 cycles. - Abstract: A simple chemical precipitation method has been used for the preparation of Mn 3 O 4 nanoparticles at room temperature. The crystal structure and morphology studies of the resulting Mn 3 O 4 nanoparticles were characterized by powder X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), N 2 adsorption and desorption and X-ray photoelectron spectroscopy (XPS). The electrochemical properties of the Mn 3 O 4 nanoparticles were then investigated using cyclic voltammetry (CV), galvanostatic charge–discharge and electrochemical impedance spectroscopy (EIS) analysis. The supercapacitive properties of Mn 3 O 4 nanoparticles in the presence of 1 M Na 2 SO 4 exhibited a high specific capacitance of 322 F g −1 at a current density of 0.5 mA cm −2 in the potential range from −0.1 to +0.9 V and about 77% of the initial capacitance was retained after 1000 cycles, indicating that the Mn 3 O 4 electrode owns a good electrochemical stability and capacitance retention capability. The results suggest that the obtained Mn 3 O 4 nanoparticles is a promising electrode material for supercapacitor applications

  5. The Suzuki–Miyaura Cross-Coupling as a Versatile Tool for Peptide Diversification and Cyclization

    Directory of Open Access Journals (Sweden)

    Tom Willemse

    2017-02-01

    Full Text Available The (site-selective derivatization of amino acids and peptides represents an attractive field with potential applications in the establishment of structure–activity relationships and labeling of bioactive compounds. In this respect, bioorthogonal cross-coupling reactions provide valuable means for ready access to peptide analogues with diversified structure and function. Due to the complex and chiral nature of peptides, mild reaction conditions are preferred; hence, a suitable cross-coupling reaction is required for the chemical modification of these challenging substrates. The Suzuki reaction, involving organoboron species, is appropriate given the stability and environmentally benign nature of these reactants and their amenability to be applied in (partial aqueous reaction conditions, an expected requirement upon the derivatization of peptides. Concerning the halogenated reaction partner, residues bearing halogen moieties can either be introduced directly as halogenated amino acids during solid-phase peptide synthesis (SPPS or genetically encoded into larger proteins. A reversed approach building in boron in the peptidic backbone is also possible. Furthermore, based on this complementarity, cyclic peptides can be prepared by halogenation, and borylation of two amino acid side chains present within the same peptidic substrate. Here, the Suzuki–Miyaura reaction is a tool to induce the desired cyclization. In this review, we discuss diverse amino acid and peptide-based applications explored by means of this extremely versatile cross-coupling reaction. With the advent of peptide-based drugs, versatile bioorthogonal conversions on these substrates have become highly valuable.

  6. Use of synthetic peptide libraries for the H-2Kd binding motif identification.

    Science.gov (United States)

    Quesnel, A; Casrouge, A; Kourilsky, P; Abastado, J P; Trudelle, Y

    1995-01-01

    To identify Kd-binding peptides, an approach based on small peptide libraries has been developed. These peptide libraries correspond to all possible single-amino acid variants of a particular Kd-binding peptide, SYIPSAEYI, an analog of the Plasmodium berghei 252-260 antigenic peptide SYIPSAEKI. In the parent sequence, each position is replaced by all the genetically encoded amino acids (except cysteine). The multiple analog syntheses are performed either by the Divide Couple and Recombine method or by the Single Resin method and generate mixtures containing 19 peptides. The present report deals with the synthesis, the purification, the chemical characterization by amino acid analysis and electrospray mass spectrometry (ES-MS), and the application of such mixtures in binding tests with a soluble, functionally empty, single-chain H-2Kd molecule denoted SC-Kd. For each mixture, bound peptides were eluted and analyzed by sequencing. Since the binding tests were realized in noncompetitive conditions, our results show that a much broader set of peptides bind to Kd than expected from previous studies. This may be of practical importance when looking for low affinity peptides such as tumor peptides capable of eliciting protective immune response.

  7. Synthesis and in vitro anti-cancer evaluation of luteinizing hormone-releasing hormone-conjugated peptide.

    Science.gov (United States)

    Deng, Xin; Qiu, Qianqian; Ma, Ke; Huang, Wenlong; Qian, Hai

    2015-11-01

    Luteinizing hormone-releasing hormone (LHRH) is a decapeptide hormone released from the hypothalamus and shows high affinity binding to the LHRH receptors. It is reported that several cancer cells also express LHRH receptors such as breast, ovarian, prostatic, bladder and others. In this study, we linked B1, an anti-cancer peptide, to LHRH and its analogs to improve the activity against cancer cells with LHRH receptor. Biological evaluation revealed that TB1, the peptide contains triptorelin sequence, present favorable anti-cancer activity as well as plasma stability. Further investigations disclosed that TB1 trigger apoptosis by activating the mitochondria-cytochrome c-caspase apoptotic pathway, it also exhibited the anti-migratory effect on cancer cells.

  8. Chemical synthesis of highly stable PVA/PANI films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Patil, D.S.; Shaikh, J.S.; Dalavi, D.S.; Kalagi, S.S. [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Patil, P.S., E-mail: psp_phy@unishivaji.ac.in [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2011-08-15

    Highlights: {yields} Chemical synthesis of PVA/PANI films by spin and dip coating at room temperature. {yields} Thickness dependent supercapacitor behavior of PVA/PANI film. {yields} The synthesized film are highly stable up to 20,000 cycles. - Abstract: Polyvinyl alcohol (PVA)/polyaniline (PANI) thin films were chemically synthesized by adopting two step process: initially a thin layer (200 nm) of PVA was spin coated by using an aqueous PVA solution onto fluorine doped tin oxide (FTO) coated glass substrate, afterwards PANI was chemically polymerized from aniline monomer and dip coated onto the precoated substrate. The thickness of PANI layer was varied from 293 nm to 2367 nm by varying deposition cycles onto the precoated PVA thin film. The resultant PVA/PANI films were characterized for their optical, morphological and electrochemical properties. The FT-IR and Raman spectra revealed characteristic features of the PANI phase. The SEM study showed porous spongy structure. Electrochemical properties were studied by electrochemical impedance measurement and cyclic voltammetry. The electrochemical performance of PVA/PANI thin films was investigated in 1 M H{sub 2}SO{sub 4} aqueous electrolyte. The highest specific capacitance of 571 Fg{sup -1} was observed for the optimized thickness of 880 nm. The film was found to be stable for more than 20,000 cycles. The samples degraded slightly (25% decrement in specific capacitance) for the first 10,000 cycles. The degradation becomes much slower (10.8% decrement in specific capacitance) beyond 10,000 cycles. This dramatic improvement in the electrochemical stability of the PANI samples, without sacrificing specific capacitance was attributed to the optimized PVA layer.

  9. Synthesis and labelling of organo-metallic prosthetic groups used for indirect radioiodination of peptides and proteins

    International Nuclear Information System (INIS)

    Pozzi, Oscar R.; Castiglia, Silvia G.

    1999-01-01

    In the framework of an IAEA co-ordinated research programme the prosthetic compound ATE [N-succidinimil 3-(tri-n-butylstannyl) benzoate] has been synthesized and it has been labelled with 131 I and 125 I. Its structure has been confirmed by NMR and mass spectrometry. The labelled ATE has been conjugated with human immunoglobulin G with a yield of 41%-57%. Indirect radioiodination of peptides is currently prepared. (author)

  10. Evaluation of new radiopharmaceuticals: synthesis, evaluation, and biodistribution of radiolabelled peptide of VCAM-1 and αvβ3

    International Nuclear Information System (INIS)

    Ardisson, V.

    2006-07-01

    The new development of nuclear medicine implies the search of new isotopes but also for new vectors specific of functions or metabolic pathways. We investigated new radiopharmaceuticals intended for new diagnostic approaches of two physiopathological mechanisms frequently met in our populations: the atherosclerosis vulnerable plaque and the tumor angio genesis. We studied and optimized the iodine and 99 m-technetium radiolabelling, of a series of peptides in order to allow the in vivo use of these tracers for imaging studies in animals and possibly in humans. The radioiodination, was carried out by electrophilic substitution, and technetium was linked by a tri-carbonyl B.F.C.A. (Isolink). The reaction parameters were defined so that the labelling reactions presents a high radiochemical purity (>95%), and a high specificity activity. The reactions are fast and reproducible. Various physicochemical properties: lipo-solubility, stability of labelling, and pharmacokinetic properties: non specific binding, metabolization and organ biodistribution of peptides in animal model, were studied. These results indicate which peptide may be a suitable candidate for targeting trials. (author)

  11. Position of residues in transmembrane peptides with respect to the lipid bilayer: A combined lipid NOEs and water chemical exchange approach in phospholipid bicelles

    International Nuclear Information System (INIS)

    Glover, Kerney Jebrell; Whiles, Jennifer A.; Vold, Regitze R.; Melacini, Giuseppe

    2002-01-01

    The model transmembrane peptide P16 was incorporated into small unaligned phospholipid bicelles, which provide a 'native-like' lipid bilayer compatible with high-resolution solution NMR techniques. Using amide-water chemical exchange and amide-lipid cross-relaxation measurements, the interactions between P16 and bicelles were investigated. Distinctive intermolecular NOE patterns observed in band-selective 2D-NOESY spectra of bicellar solutions with several lipid deuteration schemes indicated that P16 is preferentially interacting with the 'bilayered' region of the bicelle rather than with the rim. Furthermore, when amide-lipid NOEs were combined with amide-water chemical exchange cross-peaks of selectively 15 N-labeled P16 peptides, valuable information was obtained about the position of selected residues relative to the membrane-water interface. Specifically, three main classes were identified. Class I residues lie outside the bilayer and show amide-water exchange cross-peaks but no amide-lipid NOEs. Class II residues reside in the bilayer-water interface and show both amide-water exchange cross-peaks and amide-lipid NOEs. Class III residues are embedded within the hydrophobic core of the membrane and show no amide-water exchange cross-peaks but strong amide-lipid NOEs

  12. Cell targeting peptides as smart ligands for targeting of therapeutic or diagnostic agents: a systematic review.

    Science.gov (United States)

    Mousavizadeh, Ali; Jabbari, Ali; Akrami, Mohammad; Bardania, Hassan

    2017-10-01

    Cell targeting peptides (CTP) are small peptides which have high affinity and specificity to a cell or tissue targets. They are typically identified by using phage display and chemical synthetic peptide library methods. CTPs have attracted considerable attention as a new class of ligands to delivery specifically therapeutic and diagnostic agents, because of the fact they have several advantages including easy synthesis, smaller physical sizes, lower immunogenicity and cytotoxicity and their simple and better conjugation to nano-carriers and therapeutic or diagnostic agents compared to conventional antibodies. In this systematic review, we will focus on the basic concepts concerning the use of cell-targeting peptides (CTPs), following the approaches of selecting them from peptide libraries. We discuss several developed strategies for cell-specific delivery of different cargos by CTPs, which are designed for drug delivery and diagnostic applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Helleborus purpurascens—Amino Acid and Peptide Analysis Linked to the Chemical and Antiproliferative Properties of the Extracted Compounds

    Directory of Open Access Journals (Sweden)

    Adina-Elena Segneanu

    2015-12-01

    Full Text Available There is a strong drive worldwide to discover and exploit the therapeutic potential of a large variety of plants. In this work, an alcoholic extract of Helleborus purpurascens (family Ranunculaceae was investigated for the identification of amino acids and peptides with putative antiproliferative effects. In our work, a separation strategy was developed using solvents of different polarity in order to obtain active compounds. Biochemical components were characterized through spectroscopic (mass spectroscopy and chromatographic techniques (RP-HPLC and GC-MS. The biological activity of the obtained fractions was investigated in terms of their antiproliferative effects on HeLa cells. Through this study, we report an efficient separation of bioactive compounds (amino acids and peptides from a plant extract dependent on solvent polarity, affording fractions with unaffected antiproliferative activities. Moreover, the two biologically tested fractions exerted a major antiproliferative effect, thereby suggesting potential anticancer therapeutic activity.

  14. Helleborus purpurascens-Amino Acid and Peptide Analysis Linked to the Chemical and Antiproliferative Properties of the Extracted Compounds.

    Science.gov (United States)

    Segneanu, Adina-Elena; Grozescu, Ioan; Cziple, Florentina; Berki, Daniel; Damian, Daniel; Niculite, Cristina Mariana; Florea, Alexandru; Leabu, Mircea

    2015-12-11

    There is a strong drive worldwide to discover and exploit the therapeutic potential of a large variety of plants. In this work, an alcoholic extract of Helleborus purpurascens (family Ranunculaceae) was investigated for the identification of amino acids and peptides with putative antiproliferative effects. In our work, a separation strategy was developed using solvents of different polarity in order to obtain active compounds. Biochemical components were characterized through spectroscopic (mass spectroscopy) and chromatographic techniques (RP-HPLC and GC-MS). The biological activity of the obtained fractions was investigated in terms of their antiproliferative effects on HeLa cells. Through this study, we report an efficient separation of bioactive compounds (amino acids and peptides) from a plant extract dependent on solvent polarity, affording fractions with unaffected antiproliferative activities. Moreover, the two biologically tested fractions exerted a major antiproliferative effect, thereby suggesting potential anticancer therapeutic activity.

  15. Influence of prosthetic radioiodination on the chemical and biological behavior of chemotactic peptides labeled at high specific activity

    International Nuclear Information System (INIS)

    Pozzi, Oscar R.; Sajaroff, Elisa O.; Edreira, Martin M.

    2006-01-01

    The influence of radioiodination made through prosthetic group N-succinimidyl-3-[ 131 I]iodo-benzoate ([ 131 I]SIB) on the behavior of small peptides was investigated using as model the chemotactic hexapeptide Nα-for-Nle-Leu-Phe-Nle-Tyr-Lys. No carrier added labeled peptide was isolated by reverse-phase HPLC (RP-HPLC) with coupling efficiencies up to 59-75%. Biodistribution in normal and infected C57 mice showed mainly a hepatobiliary clearance, a very low thyroid uptake and the highest uptake at the infection site was within 1h of injection. Superoxide production and competitive binding assays studies in human polymorphonuclear leukocytes showed a preserved biological activity and high-affinity specific binding. However, the results indicated that the changes observed in the receptor-binding properties with an IC 50 almost twice than the unlabeled peptide and the increasing in the hepatobiliary excretion could be the consequence of the increased lipophicity observed due to the presence of the prosthetic group together with a strong influence of the radioisotope per se

  16. Influence of prosthetic radioiodination on the chemical and biological behavior of chemotactic peptides labeled at high specific activity

    Energy Technology Data Exchange (ETDEWEB)

    Pozzi, Oscar R. [National Atomic Energy Commission, Ezeiza Atomic Centre, Buenos Aires (Argentina)]. E-mail: oscar.pozzi@duke.edu; Sajaroff, Elisa O. [National Atomic Energy Commission, Ezeiza Atomic Centre, Buenos Aires (Argentina); Edreira, Martin M. [National Atomic Energy Commission, Ezeiza Atomic Centre, Buenos Aires (Argentina)

    2006-06-15

    The influence of radioiodination made through prosthetic group N-succinimidyl-3-[{sup 131}I]iodo-benzoate ([{sup 131}I]SIB) on the behavior of small peptides was investigated using as model the chemotactic hexapeptide N{alpha}-for-Nle-Leu-Phe-Nle-Tyr-Lys. No carrier added labeled peptide was isolated by reverse-phase HPLC (RP-HPLC) with coupling efficiencies up to 59-75%. Biodistribution in normal and infected C57 mice showed mainly a hepatobiliary clearance, a very low thyroid uptake and the highest uptake at the infection site was within 1h of injection. Superoxide production and competitive binding assays studies in human polymorphonuclear leukocytes showed a preserved biological activity and high-affinity specific binding. However, the results indicated that the changes observed in the receptor-binding properties with an IC{sub 50} almost twice than the unlabeled peptide and the increasing in the hepatobiliary excretion could be the consequence of the increased lipophicity observed due to the presence of the prosthetic group together with a strong influence of the radioisotope per se.

  17. The Cysteine S-Alkylation Reaction as a Synthetic Method to Covalently Modify Peptide Sequences.

    Science.gov (United States)

    Calce, Enrica; De Luca, Stefania

    2017-01-05

    Synthetic methodologies to chemically modify peptide molecules have long been investigated for their impact in the field of chemical biology. They allow the introduction of biochemical probes useful for studying protein functions, for manipulating peptides with therapeutic potential, and for structure-activity relationship investigations. The commonly used approach was the derivatization of an amino acid side chain. In this regard, the cysteine, for its unique reactivity, has been widely employed as the substrate for such modifications. Herein, we report on methodologies developed to modify the cysteine thiol group through the S-alkylation reaction. Some procedures perform the alkylation of cysteine derivatives, in order to prepare building blocks to be used during the peptide synthesis, whilst some others selectively modify peptide sequences containing a cysteine residue with a free thiol group, both in solution and in the solid phase. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. The Synthesis of Calcium Salt from Brine Water by Partial Evaporation and Chemical Precipitation

    Science.gov (United States)

    Lalasari, L. H.; Widowati, M. K.; Natasha, N. C.; Sulistiyono, E.; Prasetyo, A. B.

    2017-02-01

    chemical precipitation using (NH4)2CO3 reagent are recommended in the synthesis of calcium salts from brine water because are simple, flexible and economical.

  19. Ultrasound-assisted acid hydrolysis of cellulose to chemical building blocks: Application to furfural synthesis.

    Science.gov (United States)

    Santos, Daniel; Silva, Ubiratan F; Duarte, Fabio A; Bizzi, Cezar A; Flores, Erico M M; Mello, Paola A

    2018-01-01

    In this work, the use of ultrasound energy for the production of furanic platforms from cellulose was investigated and the synthesis of furfural was demonstrated. Several systems were evaluated, as ultrasound bath, cup horn and probe, in order to investigate microcrystalline cellulose conversion using simply a diluted acid solution and ultrasound. Several acid mixtures were evaluated for hydrolysis, as diluted solutions of HNO 3 , H 2 SO 4 , HCl and H 2 C 2 O 4 . The influence of the following parameters in the ultrasound-assisted acid hydrolysis (UAAH) were studied: sonication temperature (30 to 70°C) and ultrasound amplitude (30 to 70% for a cup horn system) for 4 to 8molL -1 HNO 3 solutions. For each evaluated condition, the products were identified by ultra-performance liquid chromatography with high-resolution time-of-flight mass spectrometry (UPLC-ToF-MS), which provide accurate information regarding the products obtained from biomass conversion. The furfural structure was confirmed by nuclear magnetic resonance ( 1 H and 13 C NMR) spectroscopy. In addition, cellulosic residues from hydrolysis reaction were characterized using scanning electron microscopy (SEM), which contributed for a better understanding of physical-chemical effects caused by ultrasound. After process optimization, a 4molL -1 HNO 3 solution, sonicated for 60min at 30°C in a cup horn system at 50% of amplitude, lead to 78% of conversion to furfural. This mild temperature condition combined to the use of a diluted acid solution represents an important contribution for the selective production of chemical building blocks using ultrasound energy. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Large influence of the synthesis conditions on the physico-chemical properties of nanostructured Fe3O4

    International Nuclear Information System (INIS)

    Franger, S.; Berthet, P.; Dragos, O.; Baddour-Hadjean, R.; Bonville, P.; Berthon, J.

    2007-01-01

    Magnetite synthesized via three different synthesis routes (coprecipitation process in aqueous media, electrochemical synthesis in presence of complexing agents and solid state reaction at high temperature) has been characterized by X-Ray diffraction, scanning electron microscopy, thermal analysis (TGA), FT-IR and Moessbauer spectroscopies. Although each procedure gave homogeneous magnetite powders, many differences could be seen in the physico-chemical properties of the samples mostly depending on the synthesis conditions. For instance, at least two factors seem to have a huge impact onto the Fe 3 O 4 behaviour: the presence of hydration water molecules and the particle size of the powders since a superparamagnetic behaviour was observed with the thinnest particles, at room temperature, on the Moessbauer spectra via the appearance of line broadening and a pronounced central doublet

  1. 1,2,3-Triazole Rings as a Disulfide Bond Mimetic in Chimeric AGRP-Melanocortin Peptides: Design, Synthesis, and Functional Characterization.

    Science.gov (United States)

    Tala, Srinivasa R; Singh, Anamika; Lensing, Cody J; Schnell, Sathya M; Freeman, Katie T; Rocca, James R; Haskell-Luevano, Carrie

    2018-05-16

    The melanocortin system is involved in the regulation of complex physiological functions, including energy and weight homeostasis, feeding behavior, inflammation, sexual function, pigmentation, and exocrine gland function. The five melanocortin receptors that belong to the superfamily of G protein-coupled receptors (GPCRs) are regulated by endogenously expressed agonists and antagonists. The aim of this study was to explore the potential of replacing the disulfide bridge in chimeric AGRP-melanocortin peptide Tyr-c[Cys-His-d-Phe-Arg-Trp-Asn-Ala-Phe-Cys]-Tyr-NH 2 (1) with 1,2,3-triazole moieties. A series of 1,2,3-triazole-bridged peptidomimetics were designed, synthesized, and pharmacologically evaluated at the mouse melanocortin receptors. The ligands possessed nanomolar to micromolar agonist cAMP signaling potency. A key finding was that the disulfide bond in peptide 1 can be replaced with the monotriazole ring with minimal effect on the functional activity at the melanocortin receptors. The 1,5-disubstituted triazole-bridged peptide 6 showed equipotent functional activity at the mMC3R and modest 5-fold decreased agonist potency at the mMC4R compared to those of 1. Interestingly, the 1,4- and 1,5-disubstituted isomers of the triazole ring resulted in different selectivities at the receptor subtypes, indicating subtle structural features that may be exploited in the generation of selective melanocortin ligands. Introducing cyclic and acyclic bis-triazole moieties into chimeric AGRP template 1 generally decreased agonist activity. These results will be useful for the further design of neuronal chemical probes for the melanocortin receptors as well as in other receptor systems.

  2. Nanostructured Thin Film Synthesis by Aerosol Chemical Vapor Deposition for Energy Storage Applications

    Science.gov (United States)

    Chadha, Tandeep S.

    Renewable energy sources offer a viable solution to the growing energy demand while mitigating concerns for greenhouse gas emissions and climate change. This has led to a tremendous momentum towards solar and wind-based energy harvesting technologies driving efficiencies higher and costs lower. However, the intermittent nature of these energy sources necessitates energy storage technologies, which remain the Achilles heel in meeting the renewable energy goals. This dissertation focusses on two approaches for addressing the needs of energy storage: first, targeting direct solar to fuel conversion via photoelectrochemical water-splitting and second, improving the performance of current rechargeable batteries by developing new electrode architectures and synthesis processes. The aerosol chemical vapor deposition (ACVD) process has emerged as a promising single-step approach for nanostructured thin film synthesis directly on substrates. The relationship between the morphology and the operating parameters in the process is complex. In this work, a simulation based approach has been developed to understand the relationship and acquire the ability of predicting the morphology. These controlled nanostructured morphologies of TiO2 , compounded with gold nanoparticles of various shapes, are used for solar water-splitting applications. Tuning of light absorption in the visible-light range along with reduced electron-hole recombination in the composite structures has been demonstrated. The ACVD process is further extended to a novel single-step synthesis of nanostructured TiO2 electrodes directly on the current collector for applications as anodes in lithium-ion batteries, mainly for electric vehicles and hybrid electric vehicles. The effect of morphology of the nanostructures has been investigated via experimental studies and electrochemical transport modelling. Results demonstrate the exceptional performance of the single crystal one-dimensional nanostructures over granular

  3. Hot-wire chemical vapor synthesis for a variety of nano-materials with novel applications

    International Nuclear Information System (INIS)

    Dillon, A.C.; Mahan, A.H.; Deshpande, R.; Alleman, J.L.; Blackburn, J.L.; Parillia, P.A.; Heben, M.J.; Engtrakul, C.; Gilbert, K.E.H.; Jones, K.M.; To, R.; Lee, S-H.; Lehman, J.H.

    2006-01-01

    Hot-wire chemical vapor deposition (HWCVD) has been demonstrated as a simple economically scalable technique for the synthesis of a variety of nano-materials in an environmentally friendly manner. For example we have employed HWCVD for the continuous production of both carbon single- and multi-wall nanotubes (SWNTs and MWNTs). Unanticipated hydrogen storage on HWCVD-generated MWNTs has led insight into the adsorption mechanism of hydrogen on metal/carbon composites at near ambient temperatures that could be useful for developing a vehicular hydrogen storage system. Recent efforts have been focused on growing MWNT arrays on thin nickel films with a simple HWCVD process. New data suggests that these MWNT arrays could replace the gold black coatings currently used in pyroelectric detectors to accurately measure laser power. Finally, we have very recently employed HWCVD for the production of crystalline molybdenum and tungsten oxide nanotubes and nanorods. These metal oxide nanorods and nanotubes could have applications in catalysis, batteries and electrochromic windows or as gas sensors. A summary of the techniques for growing these novel materials and their various potential applications is provided

  4. The nature of outsourced preclinical research--the example of chemical synthesis.

    Science.gov (United States)

    Festel, Gunter W

    2013-09-01

    The possibility to buy standardized external services or even new and innovative methods within drug discovery has increased dramatically during the last decades. Service providers are able to provide timely and efficient solutions to any given problem within preclinical research. The outsourcing behavior depends on the specific company type. Generally, the outsourcing level of emerging pharmaceutical and biotechnology companies is much higher than established companies due to low or missing internal resources. Whereas the "make-or-buy" decisions of large and fully integrated pharmaceutical companies are mainly competency driven, those of mid-size and small pharmaceutical, as well as biotech companies show a specific combination of cost/capacity and competency. The three different cooperation models "price competition", "project selection," and "strategic partnership" were identified. For all types of companies, the cooperation model of "strategic partnership" offers access to high-level expertise while reducing fixed costs and complexity. This was shown using chemical synthesis as an example but is also true for other areas of preclinical research.

  5. Synthesis of Copper Nanoparticles in Ethylene Glycol by Chemical Reduction with Vanadium (+2 Salts

    Directory of Open Access Journals (Sweden)

    Andrea Pietro Reverberi

    2016-09-01

    Full Text Available Copper nanoparticles have been synthesized in ethylene glycol (EG using copper sulphate as a precursor and vanadium sulfate as an atypical reductant being active at room temperature. We have described a technique for a relatively simple preparation of such a reagent, which has been electrolytically produced without using standard procedures requiring an inert atmosphere and a mercury cathode. Several stabilizing agents have been tested and cationic capping agents have been discarded owing to the formation of complex compounds with copper ions leading to insoluble phases contaminating the metallic nanoparticles. The elemental copper nanoparticles, stabilized with polyvinylpyrrolidone (PVP and sodium dodecyl sulphate (SDS, have been characterized for composition by energy dispersive X-ray spectroscopy (EDS, and for size by dynamic light scattering (DLS, and transmission electron microscopy (TEM, giving a size distribution in the range of 40–50 nm for both stabilizing agents. From a methodological point of view, the process described here may represent an alternative to other wet-chemical techniques for metal nanoparticle synthesis in non-aqueous media based on conventional organic or inorganic reductants.

  6. Synthesis of Nickel and Nickel Hydroxide Nanopowders by Simplified Chemical Reduction

    Directory of Open Access Journals (Sweden)

    Jeerapan Tientong

    2014-01-01

    Full Text Available Nickel nanopowders were synthesized by a chemical reduction of nickel ions with hydrazine hydrate at pH ~12.5. Sonication of the solutions created a temperature of 54–65°C to activate the reduction reaction of nickel nanoparticles. The solution pH affected the composition of the resulting nanoparticles. Nickel hydroxide nanoparticles were formed from an alkaline solution (pH~10 of nickel-hydrazine complexed by dropwise titration. X-ray diffraction of the powder and the analysis of the resulting Williamson-Hall plots revealed that the particle size of the powders ranged from 12 to 14 nm. Addition of polyvinylpyrrolidone into the synthesis decreased the nickel nanoparticle size to approximately 7 nm. Dynamic light scattering and scanning electron microscopy confirmed that the particles were in the nanometer range. The structure of the synthesized nickel and nickel hydroxide nanoparticles was identified by X-ray diffraction and Fourier transform infrared spectroscopy.

  7. Synthesis of mono and multidomain YIG particles by chemical coprecipitation or ceramic procedure

    International Nuclear Information System (INIS)

    Fernandez-Garcia, L.; Suarez, M.; Menendez, J.L.

    2010-01-01

    Yttrium iron garnet powders have been synthesized by chemical coprecipitation using two different precursors, nitrates and chlorides, and by an oxides mixture route. It is shown that depending on the precursors and synthesis conditions used pure yttrium iron garnet powders can be obtained with a mono or multidomain magnetic behaviour. The yttrium iron garnet crystalline structure, as studied by Raman spectroscopy, was already formed after calcination at temperatures as low as 800 o C when the nitrate precursors were used. However, calcination temperatures of up to 1100 o C were required to obtain yttrium iron garnet powders when the precursors were chlorides or when the oxides mixture route was chosen. The saturation magnetization of the powders correlates well with the structural characterization: when nitrate precursors were used, the saturation magnetization was already close to the bulk value, 26.8 emu/cm 3 , after calcination at 800 o C. However, the saturation magnetization of the powders obtained by the chlorides and oxides mixture routes was close to zero up to calcination temperatures of 1100 o C. Finally, both the chlorides and the oxides mixture routes yield multidomain micron sized yttrium iron garnet powders, whereas the nitrates route led to monodomain submicron sized powders.

  8. Physico-Chemical and In-vitro Microbial Studies of Newly Synthesis Organometallic Complexes

    Directory of Open Access Journals (Sweden)

    Isam Hussain Al-Karkhi

    2014-05-01

    Full Text Available Drugs normally synthesized to use as medication to treat diseases like cancer and microbial infections, these synthesized drugs were interested more than naturally-derived drugs which have been shows low activity or not as efficient against diseases. A new ligand 3-methylbenzyl (2Z-2-[1-(pyridin-4-ylethylidene]hydrazine carbodithioate (PE3MBC and its Cd(II, Cu(II, Co(II and Zn(II metal complexes. The new ligand and metal complexes were characterized via various physico-chemical and spectroscopic techniques. Cd(II complex show more activity against microbes and against cancer cell line MCF-7, while other complexes does not shows activity like cadmium complex, all the complexes does not shows any activity against MDAMB-231 cell line. The fatal of the cancer and the microbes cell was due to inhibition of DNA synthesis which was probably due to chelating with metals complexes, or could be referred to lipophilicity, presence of hydrophobic moiety in the complex molecule, also could be due to steric effects and electronic effects.

  9. Control of nanoparticle agglomeration through variation of the time-temperature profile in chemical vapor synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Djenadic, Ruzica; Winterer, Markus, E-mail: markus.winterer@uni-due.de [Universität Duisburg-Essen, Nanoparticle Process Technology, Faculty of Engineering and CENIDE (Germany)

    2017-02-15

    The influence of the time-temperature history on the characteristics of nanoparticles such as size, degree of agglomeration, or crystallinity is investigated for chemical vapor synthesis (CVS). A simple reaction-coagulation-sintering model is used to describe the CVS process, and the results of the model are compared to experimental data. Nanocrystalline titania is used as model material. Titania nanoparticles are generated from titanium-tetraisopropoxide (TTIP) in a hot-wall reactor. Pure anatase particles and mixtures of anatase, rutile (up to 11 vol.%), and brookite (up to 29 vol.%) with primary particle sizes from 1.7 nm to 10.5 nm and agglomerate particle sizes from 24.3 nm to 55.6 nm are formed depending on the particle time-temperature history. An inductively heated furnace with variable inductor geometry is used as a novel system to control the time-temperature profile in the reactor externally covering a large wall temperature range from 873 K to 2023 K. An appropriate choice of inductor geometry, i.e. time-temperature profile, can significantly reduce the degree of agglomeration. Other particle characteristics such as crystallinity are also substantially influenced by the time-temperature profile.

  10. Electrical properties of aluminum-doped zinc oxide (AZO) nanoparticles synthesized by chemical vapor synthesis

    International Nuclear Information System (INIS)

    Hartner, Sonja; Schulz, Christof; Wiggers, Hartmut; Ali, Moazzam; Winterer, Markus

    2009-01-01

    Aluminum-doped zinc oxide nanoparticles have been prepared by chemical vapor synthesis, which facilitates the incorporation of a higher percentage of dopant atoms, far above the thermodynamic solubility limit of aluminum. The electrical properties of aluminum-doped and undoped zinc oxide nanoparticles were investigated by impedance spectroscopy. The impedance is measured under hydrogen and synthetic air between 323 and 673 K. The measurements under hydrogen as well as under synthetic air show transport properties depending on temperature and doping level. Under hydrogen atmosphere, a decreasing conductivity with increasing dopant content is observed, which can be explained by enhanced scattering processes due to an increasing disorder in the nanocrystalline material. The temperature coefficient for the doped samples switches from positive temperature coefficient behavior to negative temperature coefficient behavior with increasing dopant concentration. In the presence of synthetic air, the conductivity firstly increases with increasing dopant content by six orders of magnitude. The origin of the increasing conductivity is the generation of free charge carriers upon dopant incorporation. It reaches its maximum at a concentration of 7.7% of aluminum, and drops for higher doping levels. In all cases, the conductivity under hydrogen is higher than under synthetic air and can be changed reversibly by changing the atmosphere.

  11. Electrical properties of aluminum-doped zinc oxide (AZO) nanoparticles synthesized by chemical vapor synthesis.

    Science.gov (United States)

    Hartner, Sonja; Ali, Moazzam; Schulz, Christof; Winterer, Markus; Wiggers, Hartmut

    2009-11-04

    Aluminum-doped zinc oxide nanoparticles have been prepared by chemical vapor synthesis, which facilitates the incorporation of a higher percentage of dopant atoms, far above the thermodynamic solubility limit of aluminum. The electrical properties of aluminum-doped and undoped zinc oxide nanoparticles were investigated by impedance spectroscopy. The impedance is measured under hydrogen and synthetic air between 323 and 673 K. The measurements under hydrogen as well as under synthetic air show transport properties depending on temperature and doping level. Under hydrogen atmosphere, a decreasing conductivity with increasing dopant content is observed, which can be explained by enhanced scattering processes due to an increasing disorder in the nanocrystalline material. The temperature coefficient for the doped samples switches from positive temperature coefficient behavior to negative temperature coefficient behavior with increasing dopant concentration. In the presence of synthetic air, the conductivity firstly increases with increasing dopant content by six orders of magnitude. The origin of the increasing conductivity is the generation of free charge carriers upon dopant incorporation. It reaches its maximum at a concentration of 7.7% of aluminum, and drops for higher doping levels. In all cases, the conductivity under hydrogen is higher than under synthetic air and can be changed reversibly by changing the atmosphere.

  12. Synthesis, structural characterization and quantum chemical studies of silicon-containing benzoic acid derivatives

    Science.gov (United States)

    Zaltariov, Mirela-Fernanda; Cojocaru, Corneliu; Shova, Sergiu; Sacarescu, Liviu; Cazacu, Maria

    2016-09-01

    The present paper is concerned with the synthesis and molecular structure investigation of two new benzoic acid derivatives having trimethylsilyl tails, 4-((trimethylsilyl)methoxy) and 4-(3-(trimethylsilyl)propoxy)benzoic acids. The structures of the novel compounds have been confirmed by X-ray crystallography, Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (1H and 13C NMR). The theoretical studies of molecules were conducted by using the quantum chemical methods, such as Density Functional Theory (DFT B3LYP/6-31 + G**), Hartree-Fock (HF/6-31 + G**) and semiempirical computations (PM3, PM6 and PM7). The optimized molecular geometries have been found to be in good agreement with experimental structures resulted from the X-ray diffraction. The maximum electronic absorption bands observed at 272-287 nm (UV-vis spectra) have been assigned to π → π* transitions, which were in reasonable agreement with the time dependent density functional theory (TD-DFT) calculations. The computed vibrational frequencies by DFT method were assigned and compared with the experimental FTIR spectra. The mapped electrostatic potentials revealed the reactive sites, which corroborated the observation of the dimer supramolecular structures formed in the crystals by hydrogen-bonding. The energies of frontier molecular orbitals (HOMO and LUMO), energy gap, dipole moment and molecular descriptors for the new compounds were calculated and discussed.

  13. Layer-selective synthesis of bilayer graphene via chemical vapor deposition

    Science.gov (United States)

    Yang, Ning; Choi, Kyoungjun; Robertson, John; Park, Hyung Gyu

    2017-09-01

    A controlled synthesis of high-quality AB-stacked bilayer graphene by chemical vapor deposition demands a detailed understanding of the mechanism and kinetics. By decoupling the growth of the two layers via a growth-and-regrowth scheme, we report the kinetics and termination mechanisms of the bilayer graphene growth on copper. We observe, for the first time, that the secondary layer growth follows Gompertzian kinetics. Our observations affirm the postulate of a time-variant transition from a mass-transport-limited to a reaction-limited regimes and identify the mechanistic disparity between the monolayer growth and the secondary-layer expansion underneath the monolayer cover. It is the continuous carbon supply that drives the expansion of the graphene secondary layer, rather than the initially captured carbon amount, suggesting an essential role of the surface diffusion of reactant adsorbates in the interspace between the top graphene layer and the underneath copper surface. We anticipate that the layer selectivity of the growth relies on the entrance energetics of the adsorbed reactants to the graphene-copper interspace across the primary-layer edge, which could be engineered by tailoring the edge termination state. The temperature-reliant saturation area of the secondary-layer expansion is understood as a result of competitive attachment of carbon and hydrogen adatoms to the secondary-layer graphene edge.

  14. Organocatalysts for enantioselective synthesis of fine chemicals: definitions, trends and developments

    Directory of Open Access Journals (Sweden)

    Chiara Palumbo

    2015-02-01

    Full Text Available Organocatalysis, that is the use of small organic molecules to catalyze organic transformations, has been included among the most successful concepts in asymmetric catalysis, and it has been used for the enantioselective construction of C–C, C–N, C–O, C–S, C–P and C–halide bonds. Since the seminal works in early 2000, the scientific community has been paying an ever-growing attention to the use of organocatalysts for the synthesis, with high yields and remarkable stereoselectivities, of optically active fine chemicals of interest for the pharmaceutical industry. A brief overview is here presented about the two main classes of substrate activation by the catalyst: covalent organocatalysis and non-covalent organocatalysis, with a more stringent focus on some recent outcomes in the field of the latter and of hydrogen bond-based catalysis. Finally, some successful examples of heterogenization of organocatalysts are also discussed, in the view of a potential industrial exploitation.

  15. Synthesis and characterization of hydroxyapatite nanoparticles by chemical precipitation method for potential application in water treatment

    Science.gov (United States)

    Joshi, Parth; Patel, Chirag; Vyas, Meet

    2018-05-01

    Hydroxyapatite (HA) is a unique material having high adsorption capacity of heavy metals, high ion exchange capacity, high biological compatibility, low water solubility, high stability under reducing and oxidizing conditions, availability and low cost. As the starting reagents, analytical grade Ca(NO3)2.4H2O, (NH4)2HPO4 and NaOH were used. In order to study the factors that have an important influence on the chemical precipitation process a experimental platform has been designed for hydroxyapatite synthesis. The addition of Phosphorus pentaoxide to Calcium hydroxide was carried out slowly with simultaneous stirring. After addition, solution was aged for maturation. The precipitate was dried at 80°C overnight and further heat treated at 600°C for 2 hours. The dried and calcined particles were characterized by Fourier transform infra-red spectroscopy and Thermo gravimetric analysis. The particle size and morphology were studied using transmission electron microscopy. TEM examination of the treated powders displayed particles of polygon morphology with dimensions 30-70 nm in length. The FT-IR spectra for sample confirmed the formation of hydroxyapatite. Purity of the prepared Hydroxyapatite has been confirmed by XRD analysis.

  16. Functionalized polypyrrole film: synthesis, characterization, and potential applications in chemical and biological sensors.

    Science.gov (United States)

    Dong, Hua; Cao, Xiaodong; Li, Chang Ming

    2009-07-01

    In this paper, we report the synthesis of a carboxyl-functionalized polypyrrole derivative, a poly(pyrrole-N-propanoic acid) (PPPA) film, by electrochemical polymerization, and the investigation of its basic properties via traditional characterization techniques such as confocal-Raman, FTIR, SEM, AFM, UV-vis, fluorescence microscopy, and contact-angle measurements. The experimental data show that the as-prepared PPPA film exhibits a hydrophilic nanoporous structure, abundant -COOH functional groups in the polymer backbone, and high fluorescent emission under laser excitation. On the basis of these unique properties, further experiments were conducted to demonstrate three potential applications of the PPPA film in chemical and biological sensors: a permeable and permselective membrane, a membrane with specific recognition sites for biomolecule immobilization, and a fluorescent conjugated polymer for amplification of fluorescence quenching. Specifically, the permeability and permselectivity of ion species through the PPPA film are detected by means of rotating-disk-electrode voltammetry; the specific recognition sites on the film surface are confirmed with protein immobilization, and the amplification of fluorescence quenching is measured by the addition of a quenching agent with fluorescence microscopy. The results are in good agreement with our expectations.

  17. One-step synthesis of chlorinated graphene by plasma enhanced chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Liwei; Zhang, Hui; Zhang, Pingping; Sun, Xuhui, E-mail: xhsun@suda.edu.cn

    2015-08-30

    Highlights: • We developed a simple approach to synthesize the single layer chlorinated graphene. • CuCl{sub 2} on Cu surface is used as Cl source under the plasma treatment. • The formation of covalent C−Cl bond has been investigated by Raman and XPS. • Raman results indicate the p-type doping effect of chlorination. - Abstract: We developed an approach to synthesize the chlorinated single layer graphene (Cl-G) by one-step plasma enhanced chemical vapor deposition. Copper foil was simply treated with hydrochloric acid and then CuCl{sub 2} formed on the surface was used as Cl source under the assistance of plasma treatment. Compared with other two-step methods by post plasma/photochemical treatment of CVD-grown single layer graphene (SLG), one-step Cl-G synthesis approach is quite straightforward and effective. X-ray photoelectron spectroscopy (XPS) revealed that ∼2.45 atom% Cl remained in SLG. Compared with the pristine SLG, the obvious blue shifts of G band and 2D band along with the appearance of D’ band and D + G band in the Raman spectra indicate p-type doping of Cl-G.

  18. Sequential structural and optical evolution of MoS2 by chemical synthesis and exfoliation

    Science.gov (United States)

    Kim, Ju Hwan; Kim, Jungkil; Oh, Si Duck; Kim, Sung; Choi, Suk-Ho

    2015-06-01

    Various types of MoS2 structures are successfully obtained by using economical and facile sequential synthesis and exfoliation methods. Spherically-shaped lumps of multilayer (ML) MoS2 are prepared by using a conventional hydrothermal method and were subsequently 1st-exfoliated in hydrazine while being kept in autoclave to be unrolled and separated into five-to-six-layer MoS2 pieces of several-hundred nm in size. The MoS2 MLs are 2nd-exfoliated in sodium naphthalenide under an Ar ambient to finally produce bilayer MoS2 crystals of ~100 nm. The sequential exfoliation processes downsize MoS2 laterally and reduce its number of layers. The three types of MoS2 allotropes exhibit particular optical properties corresponding to their structural differences. These results suggest that two-dimensional MoS2 crystals can be prepared by employing only chemical techniques without starting from high-pressure-synthesized bulk MoS2 crystals.

  19. Direct chemical synthesis of MnO2 nanowhiskers on MXene surfaces for supercapacitor applications

    KAUST Repository

    Baby, Rakhi Raghavan

    2016-07-05

    Transition metal carbides (MXenes) are an emerging class of two dimensional (2D) materials with promising electrochemical energy storage performance. Herein, for the first time, by direct chemical synthesis, nanocrystalline ε-MnO2 whiskers were formed on MXene nanosheet surfaces (ε-MnO2/Ti2CTx and ε-MnO2/Ti3C2Tx) to make nanocomposite electrodes for aqueous pseudocapacitors. The ε-MnO2 nanowhiskers increase the surface area of the composite electrode and enhance the specific capacitance by nearly three orders of magnitude compared to pure MXene based symmetric supercapacitors. Combined with enhanced pseudocapacitance, the fabricated ε-MnO2/MXene supercapacitors exhibited excellent cycling stability with ~88% of the initial specific capacitance retained after 10000 cycles which is much higher than pure ε-MnO2 based supercapacitors (~74%). The proposed electrode structure capitalizes on the high specific capacitance of MnO2 and the ability of MXenes to improve conductivity and cycling stability.

  20. Synthesis of Functional Polyester Based on Polylactic Acid and Its Effect on PC12 Cells after Coupling with Small Peptides

    Directory of Open Access Journals (Sweden)

    Na Qiang

    2016-01-01

    Full Text Available Polyesters containing functional groups are a suitable candidate matrix for cell culture in tissue engineering. Three types of semicrystalline copolymer poly(L-lactide-co-β-malic acid [P(LA-co-BMD] with pendent carboxyl groups were synthesized in this study. The functional monomer 3(S-[(benzyloxycarbonylmethyl]-1,4-dioxane-2,5-dione (BMD was synthesized using L-aspartic acid. The copolymer P(LA-co-BMD was then synthesized through ring-opening copolymerization of L-LA and BMD, with dodecanol as initiator and stannous octoate as catalyst. Copolymer structure was characterized by 1H nuclear magnetic resonance (1H NMR, gel permeation chromatography (GPC, and differential scanning calorimetry (DSC analyses. Results of 1H NMR and GPC analyses showed that the copolymers were synthesized successfully. DSC curves showed that the crystal melting peak and enthalpy decreased with increased BMD. The crystallinity of the copolymer was destroyed by the presence of the functional monomer. After deprotection, carboxyl groups were coupled with the isoleucine-lysine-valine-alanine-valine peptide through N-hydroxysuccinimide/dicyclohexylcarbodiimide method. The small peptide was beneficial to the axon growth of PC12 cells.

  1. Synthesis and evaluation of Tc-99m-labeled RRL-containing peptide as a non-invasive tumor imaging agent in a mouse fibrosarcoma model.

    Science.gov (United States)

    Kim, Dae-Weung; Kim, Woo Hyoung; Kim, Myoung Hyoun; Kim, Chang Guhn

    2015-11-01

    Arginine-arginine-leucine (RRL) is considered a tumor endothelial cell-specific binding sequence. RRL-containing peptide targeting tumor vessels is an excellent candidate for tumor imaging. In this study, we developed RRL-containing hexapeptides and evaluated their feasibility as a tumor imaging agent in a HT-1080 fibrosarcoma-bearing murine model. The hexapeptide, glutamic acid-cysteine-glycine (ECG)-RRL was synthesized using Fmoc solid-phase peptide synthesis. Radiolabeling efficiency was evaluated using instant thin-layer chromatography. Uptake of Tc-99m ECG-RRL within HT-1080 cells was evaluated in vitro by confocal microscopy and cellular binding affinity was calculated. Gamma images were acquired In HT-1080 fibrosarcoma tumor-bearing mice, and the tumor-to-muscle uptake ratio was calculated. The inflammatory-to-normal muscle uptake ratio was also calculated in an inflammation mouse model. A biodistribution study was performed to calculate %ID/g. A high yield of Tc-99m ECG-RRL complexes was prepared after Tc-99m radiolabeling. Binding of Tc-99m ECG-RRL to tumor cells had was confirmed by in vitro studies. Gamma camera imaging in the murine model showed that Tc-99m ECG-RRL accumulated substantially in the subcutaneously engrafted tumor and that tumoral uptake was blocked by co-injecting excess RRL. Moreover, Tc-99m ECG-RRL accumulated minimally in inflammatory lesions. We successfully developed Tc-99m ECG-RRL as a new tumor imaging candidate. Specific tumoral uptake of Tc-99m ECG-RRL was evaluated both in vitro and in vivo, and it was determined to be a good tumor imaging candidate. Additionally, Tc-99m ECG-RRL effectively distinguished between cancerous tissue and inflammatory lesions.

  2. Synthesis and evaluation of Tc-99m and fluorescence-labeled elastin-derived peptide, VAPG for multimodal tumor imaging in murine tumor model.

    Science.gov (United States)

    Kim, Myoung Hyoun; Kim, Chang Guhn; Kim, Seul-Gi; Kim, Dae-Weung

    2017-12-01

    We developed a Tc-99m and fluorescence-labeled peptide, Tc-99m TAMRA-GHEG-ECG-VAPG to target tumor cells and evaluated the diagnostic performance as a dual-modality imaging agent for tumor in a murine model. TAMRA-GHEG-ECG-VAPG was synthesized by using Fmoc solid-phase peptide synthesis. Radiolabeling of TAMRA-GHEG-ECG-VAPG with Tc-99m was done by using ligand exchange via tartrate. Binding affinity and in vitro cellular uptake studies were performed. Gamma camera imaging, biodistribution, and ex vivo imaging studies were performed in murine models with SW620 tumors. Tumor tissue slides were prepared and analyzed with immunohistochemistry by using confocal microscopy. After radiolabeling procedures with Tc-99m, Tc-99m TAMRA-GHEG-ECG-VAPG complexes were prepared in high yield (>96%). The K d of Tc-99m TAMRA-GHEG-ECG-VAPG determined by saturation binding was 16.8 ± 3.6 nM. Confocal microscopy images of SW620 cells incubated with TAMRA-GHEG-ECG-VAPG showed strong fluorescence in the cytoplasm. Gamma camera imaging revealed substantial uptake of Tc-99m TAMRA-GHEG-ECG-VAPG in tumors. Tumor uptake was effectively blocked by the coinjection of an excess concentration of VAPG. Specific uptake of Tc-99m TAMRA-GHEG-ECG-VAPG was confirmed by biodistribution, ex vivo imaging, and immunohistochemistry stain studies. In vivo and in vitro studies revealed substantial uptake of Tc-99m TAMRA-GHEG-ECG-VAPG in tumor cells. Tc-99m TAMRA-GHEG-ECG-VAPG has potential as a dual-modality tumor imaging agent. Copyright © 2017 John Wiley & Sons, Ltd.

  3. Synthesis and biological evaluation of a 99mTc-labelled cyclic RGD peptide for imaging the αvβ3 expression

    International Nuclear Information System (INIS)

    Haubner, F.; Bock, M.; Schwaiger, M.; Wester, H.J.; Bruchertseifer, F.; Kessler, H.

    2004-01-01

    Aim: The αvβ3 integrin is involved in tumour induced angiogenesis and tumour metastasis. We describe the synthesis and evaluation of a 99m Tc-labelled RGD analogue for the visualisation of αvβ3 integrin expression. Methods: The linear peptides were assembled on a solid support. Cyclisation was performed under high dilution conditions. For conjugation with the chelator peptide, a water soluble carbodiimide was used. Radiolabelling was carried out due to standard procedures with high radiochemical yield and radiochemical purity. For in vivo evaluation, nude mice bearing αvβ3-positive human melanoma M21 and αv-negative human melanoma M21-L or Balb / c mice bearing αv-positive murine osteosarcoma were used. Results: Activity accumulation of 99m Tc-DKCK-RGD 240 min p.i. was 1.1% ID/g in the αvβ3-positive melanoma and 0.3% ID/g in the negative control tumour. In the osteosarcoma model 2.2% ID/g was found 240 min p.i. Planar gamma camera images allowed contrasting visualisation of αvβ3-positive tumours 240 min p.i. Blocking of the tumour using the αvβ3-selective pentapeptide cyclo(-Arg-Gly-Asp-D-Phe-Val-) reduces activity accumulation in the tumour to background level. However, 240 min p.i. highest activity concentration was found in kidneys resulting in low tumour / kidney ratios. Metabolite analysis 240 min p.i. showed approximately 60% intact tracer in kidneys and 80% in the tumour. Only 24% intact tracer was found in blood 30 min p.i. Conclusion: 99m Tc-DKCK-RGD allows imaging of αvβ3-positive tumours in mice. However, pharmacokinetics as well as metabolic stability of the tracer have to be improved for potential clinical application. (orig.)

  4. Synthesis and Physical and Chemical Properties of Hypergolic Chemicals such as N,N,N-Trimethylhydrazinium and 1-Ethyl-4-Methyl-1,2,4-Triazolium Salts

    Directory of Open Access Journals (Sweden)

    Young-Seok Kim

    2015-12-01

    Full Text Available Hypergolic chemicals N,N,N-trimethylhydrazinium iodide, [TMH]+[I]−, and 1-ethyl-4-methyl-1,2,4-triazolium iodide, [EMT]+[I]− were firstly synthesized by nucleophilic substitution (SN2. The successful synthesis of hypergolic chemicals [TMH]+[I]− and [EMT]+[I]− was confirmed by IR and 1H-NMR spectroscopy and, GC-mass spectrometry. Subsequently the hypergolic chemicals [TMH]+[X]− (X = CN−, N3−, NO3−, NO2−, ClO4−, AlCl4− were prepared via an ion exchange reaction from [TMH]+[I]− and [EMT]+[I]−, respectively. After that, a mixture of hypergolic chemicals was prepared by dissolving the synthesized hypergolic chemicals in 2-hydroxyethylhydrazine (HOCH2CH2NHNH2. The physical and chemical properties of the mixture such as decomposition temperature (Td, density (d, viscosity (η, and decomposition energy (ΔHd was then evaluated to determine suitability for use as liquid rocket fuels. The ignition delay (ID time of the mixture of hypergolic chemicals with [TMH]+[N3]− and [TMH]+[CN]− using H2O2 as an oxidizer was determined as 55.6 ms and 97.4 ms; respectively. The ID time of the mixture of hypergolic chemicals with [EMT]+[N3]−; [EMT]+[CN]−; [EMT]+[AlCl4]−; and [EMT]+[I]− using H2O2 as an oxidizer was also determined as 18.0 ms; 32.6 ms; 27.6 ms; and 7.96 ms; respectively. The synthesized mixture of hypergolic chemicals could thus be used as a rocket propellant liquid fuel.

  5. The role of the chemical composition of monetite on the synthesis and properties of α-tricalcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Duncan, Jo, E-mail: jo.duncan@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); MacDonald, James F., E-mail: J.F.MacDonald@warwick.ac.uk [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Hanna, John V., E-mail: J.V.Hanna@warwick.ac.uk [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry CV4 7AL (United Kingdom); Shirosaki, Yuki, E-mail: yukis@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Hayakawa, Satoshi, E-mail: satoshi@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Osaka, Akiyoshi, E-mail: a-osaka@cc.okayama-u.ac.jp [Graduate School of Natural Science and Technology, Okayama University, 3-1-1 Tsushima, Kita-ku, Okayama 700-8530 (Japan); Skakle, Janet M.S., E-mail: j.skakle@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); Gibson, Iain R., E-mail: i.r.gibson@abdn.ac.uk [Department of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE (United Kingdom); School of Medical Sciences, Institute of Medical Sciences, University of Aberdeen, Foresterhill, Aberdeen AB25 2ZD (United Kingdom)

    2014-01-01

    There has been a resurgence of interest in alpha-tricalcium phosphate (α-TCP), with use in cements, polymer composites and in bi- and tri-phasic calcium phosphate bone grafts. The simplest and most established method for preparing α-TCP is the solid state reaction of monetite (CaHPO{sub 4}) and calcium carbonate at high temperatures, followed by quenching. In this study, the effect of the chemical composition of reagents used in the synthesis of α-TCP on the local structure of the final product is reported and findings previously reported pertaining to the phase composition and stability are also corroborated. Chemical impurities in the monetite reagents were identified and could be correlated to the calcium phosphate products formed; magnesium impurities favoured the formation of β-TCP, whereas single phase α-TCP was favoured when magnesium levels were low. Monetite synthesised in-house exhibited a high level of chemical purity; when this source was used to produce an α-TCP sample, the α-polymorph could be obtained by both quenching and by cooling to room temperature in the furnace at rates between 1 and 10 °C/min, thereby simplifying the synthesis process. It was only when impurities were minimised that the 12 phosphorus environments in the α-TCP structure could be resolved by {sup 31}P nuclear magnetic resonance; samples containing chemical impurity showed differing degrees of line-broadening. Reagent purity should therefore be considered a priority when synthesising/characterising the α-polymorph of TCP. - Highlights: • Most commercial sources of monetite contain impurities that affect synthesis of phase pure α-TCP. • Ratio of α:β-TCP polymorphs formed by solid state reaction is dependent on reactant chemical purity. • If reagents in α-TCP synthesis are chemically pure, quenching is not required to obtain α-polymorph. • 12 unique P sites in α-TCP were only fully realised by {sup 31}P NMR when chemically pure reagents are used.

  6. Synthesis and characterization of CoPt nanoparticles prepared by room temperature chemical reduction with PAMAM dendrimer as template.

    Science.gov (United States)

    Wan, Haiying; Shi, Shifan; Bai, Litao; Shamsuzzoha, Mohammad; Harrell, J W; Street, Shane C

    2010-08-01

    We describe an approach to synthesize monodisperse CoPt nanoparticles with dendrimer as template by a simple chemical reduction method in aqueous solution using NaBH4 as reducing agent at room temperature. The as-made CoPt nanoparticles buried in the dendrimer matrix have the chemically disordered fcc structure and can be transformed to the fct phase after annealing at 700 degrees C. This is the first report of dendrimer-mediated room temperature synthesis of monodisperse magnetic nanoparticles in aqueous solution.

  7. Chemical and Electrochemical Synthesis of Polypyrrole Using Carrageenan as a Dopant: Polypyrrole/Multi-Walled Carbon Nanotube Nanocomposites

    Directory of Open Access Journals (Sweden)

    Mostafizur Rahaman

    2018-06-01

    Full Text Available In this article, iota-carrageenan (IC and kappa-carrageenan (KC are used as dopants for the chemical and electrochemical synthesis of polypyrrole (PPy. The composites of chemically synthesized PPy with multi-walled carbon nanotubes (MWNTs were prepared using an in situ technique. Both the dialyzed and non-dialyzed IC and KC were used as dopants for electrochemical polymerization of pyrrole. Chemically synthesized PPy and PPy/MWNTs composites were studied by ultraviolet visible (UV-vis absorption spectra to investigate the effect of the concentration and the incorporation of MWNTs. In addition, the electrical, thermal, mechanical, and microscopic characterizations of these films were performed to examine the effect of the dopants and MWNTs on these properties, along with their surface morphology. The films of electrochemically polymerized PPy were characterized using UV-vis absorption spectra, scanning electron microscopy, and cyclic voltammetry (CV. The results were then compared with the chemical polymerized PPy.

  8. Unscheduled DNA synthesis in human hair follicles after in vitro exposure to 11 chemicals: comparison with unscheduled DNA synthesis in rat hepatocytes.

    Science.gov (United States)

    van Erp, Y H; Koopmans, M J; Heirbaut, P R; van der Hoeven, J C; Weterings, P J

    1992-06-01

    A new method is described to investigate unscheduled DNA synthesis (UDS) in human tissue after exposure in vitro: the human hair follicle. A histological technique was applied to assess cytotoxicity and UDS in the same hair follicle cells. UDS induction was examined for 11 chemicals and the results were compared with literature findings for UDS in rat hepatocytes. Most chemicals inducing UDS in rat hepatocytes raised DNA repair at comparable concentrations in the hair follicle. However, 1 of 9 chemicals that gave a positive response in the rat hepatocyte UDS test, 2-acetylaminofluorene, failed to induce DNA repair in the hair follicle. Metabolizing potential of hair follicle cells was shown in experiments with indirectly acting compounds, i.e., benzo[a]pyrene, 7,12-dimethylbenz[a]anthracene and dimethylnitrosamine. The results support the conclusion that the test in its present state is valuable as a screening assay for the detection of unscheduled DNA synthesis. Moreover, the use of human tissues may result in a better extrapolation to man.

  9. Synthesis, chemical and biological properties of the new mono- and bis-derivatives of imidazoles

    Directory of Open Access Journals (Sweden)

    E. V. Welchinska

    2014-12-01

    Full Text Available The aim of research. The problem of finding effective antitumour medical preparation with low toxicity is an important issue of medical and pharmaceutical chemistry. Knowledge of cancer cell features and its metabolism enables to predict the direction of chemical and biological research, to conduct a targeted synthesis of potential drugs, and to assess their applicability in oncological practice as antitumor agents. The purpose of work is to explain preformed heterocycles as purines, its synthesis and investigation of chemical and biological properties. After construction of the potential active structures we proposed the new method of original derivatives synthesis which are received on the base of imidazole, from one side, and fluorocontaining common anesthetic halothane (2-bromo-1,1,1-trifluoro-2-chloroethane from other side. Molecular complex of more perspective biologically active bis-imidazole with antitumour bacterial lectine has been received. With the purpose to synthesize potential antitumour compounds on the base of halothane and imidazole, new convenient methods for the preparation of original heterocyclic derivatives of imidazole have been described. The structure and composition of synthesized compound has been confirmed by the methods of elemental analysis, IR- and NMRІН-spectra. Materials and methods. The majority of the absolute organic solvents (benzene, dimethylformamide, ethyl ester employed in the present studies were distilled before their use. Organic solvents were dried over anhydrous magnesium sulfate or metallic sodium. Gas-liquid chromatography was carried out by Perkin Elmer chromatograph with UV-detector ("Perkin", Germany. IR spectra were recorded in a UR-20 spectrometer ("Charles Ceise Hena", Germany. The 1HNMR spectra were recorded in DMSO-d6 on a 200 MHz BrakerWP-200 ("Braker", Switzerland or Varian T-60 spectrometer ("Varian", USA. Investigation of critical toxicity of new compounds was carried out at

  10. Process Parameters for Successful Synthesis of Carbon Nanotubes by Chemical Vapor Deposition: Implications for Chemical Mechanisms and Life-cycle Assessment

    Science.gov (United States)

    Xue, Ke

    Manufacturing of carbon nanotubes (CNTs) via chemical vapor deposition (CVD) calls for thermal treatment associated with gas-phase rearrangement and catalyst deposition to achieve high cost efficiency and limited influence on environmental impact. Taking advantage of higher degree of structure control and economical efficiency, catalytic chemical vapor deposition (CCVD) has currently become the most prevailing synthesis approach for the synthesis of large-scale pure CNTs in past years. Because the synthesis process of CNTs dominates the potential ecotoxic impacts, materials consumption, energy consumption and greenhouse gas emissions should be further limited to efficiently reduce life cycle ecotoxicity of carbon naotubes. However, efforts to reduce energy and material requirements in synthesis of CNTs by CCVD are hindered by a lack of mechanistic understanding. In this thesis, the effect of operating parameters, especially the temperature, carbon source concentration, and residence time on the synthesis were studied to improve the production efficiency in a different angle. Thus, implications on the choice of operating parameters could be provided to help the synthesis of carbon nanotubes. Here, we investigated the typical operating parameters in conditions that have yielded successful CNT production in the published academic literature of over seventy articles. The data were filtered by quality of the resultant product and deemed either "successful" or "unsuccessful" according to the authors. Furthermore, growth rate data were tabulated and used as performance metric for the process whenever possible. The data provided us an opportunity to prompt possible and common methods for practioners in the synthesis of CNTs and motivate routes to achieve energy and material minimization. The statistical analysis revealed that methane and ethylene often rely on thermal conversion process to form direct carbon precursor; further, methane and ethylene could not be the direct

  11. Synthesis, physical-chemical and biological properties of 7-benzyl-3-methyl-8-thioxanthine derivatives

    Directory of Open Access Journals (Sweden)

    D. H. Ivanchenko

    2017-12-01

    Full Text Available Introduction . Interest to the problem of creating new effective antimicrobial agents among xanthine derivatives does not decrease. Primarily, this is due to the increasing of microbial resistance to conventional antimicrobial agents and the emergence of their new strains. In recent years interest to the therapeutic use of antioxidants in the treatment of diseases associated with oxidative stress has increased. The aim of this work is to elaborate simple laboratory methods of 7-benzyl-3-methyl-8-thioxanthine derivatives synthesis, unspecified in scientific papers earlier, and to study their physical, chemical and biological properties. Materials and methods. The melting point has been determined with the help of an open capillary method with PTP-M device. Elemental analysis has been performed with the help of the instrument Elementar Vario L cube, NMR-spectra have been taken on a spectrometer Bruker SF-400 (operating frequency of 400 MHz, solvent DMSO, internal standard – TMS. Study of antimicrobial and antifungal activity of synthesized compounds has been performed by two-fold serial dilution method. Standard test strains have been used for the study: Escherichia coli ATCC 25922, Staphylococcus aureus ATCC 25923, Pseudomonas aeruginosa ATCC 27853, Candida albicans ATCC 885-653. Dimethylsulfoxide was used as the solvent of the compounds. Results. Under short-time heating up of the initial 7-benzyl-3-methyl-8-thioxanthine with alkyl, alkenyl, benzyl halides or heteroalkylchlorides in a water-propanol-2 mixture in the presence of an equimolar amount of sodium hydroxide leads to the formation of 8-S-substituted of 7-benzyl-3-methylxanthines. Structure of synthesized compounds was definitely proved by NMR-spectroscopy. We conducted primary screening research of antimicrobial activity of 7-benzyl-3-methyl-8-thioxanthine derivatives, which revealed moderate and weak activity in concentrations 50-100 mcg/ml. Most of the obtained compounds showed a

  12. Control of peptide nanotube diameter by chemical modifications of an aromatic residue involved in a single close contact

    OpenAIRE

    Tarabout, Christophe; Roux, Stéphane; Gobeaux, Frédéric; Fay, Nicolas; Pouget, Emilie; Meriadec, Cristelle; Ligeti, Melinda; Thomas, Daniel; IJsselstijn, Maarten; Besselievre, François; Buisson, David-Alexandre; Verbavatz, Jean-Marc; Petitjean, Michel; Valéry, Céline; Perrin, Lionel

    2011-01-01

    Supramolecular self-assembly is an attractive pathway for bottom-up synthesis of novel nanomaterials. In particular, this approach allows the spontaneous formation of structures of well-defined shapes and monodisperse characteristic sizes. Because nanotechnology mainly relies on size-dependent physical phenomena, the control of monodispersity is required, but the possibility of tuning the size is also essential. For self-assembling systems, shape, size, and monodispersity are mainly settled b...

  13. Synthesis of tumor necrosis factor α for use as a mirror-image phage display target.

    Science.gov (United States)

    Petersen, Mark E; Jacobsen, Michael T; Kay, Michael S

    2016-06-21

    Tumor Necrosis Factor alpha (TNFα) is an inflammatory cytokine that plays a central role in the pathogenesis of chronic inflammatory disease. Here we describe the chemical synthesis of l-TNFα along with the mirror-image d-protein for use as a phage display target. The synthetic strategy utilized native chemical ligation and desulfurization to unite three peptide segments, followed by oxidative folding to assemble the 52 kDa homotrimeric protein. This synthesis represents the foundational step for discovering an inhibitory d-peptide with the potential to improve current anti-TNFα therapeutic strategies.

  14. New Gastrin Releasing Peptide Receptor-Directed [99mTc]Demobesin 1 Mimics: Synthesis and Comparative Evaluation.

    Science.gov (United States)

    Nock, Berthold A; Charalambidis, David; Sallegger, Werner; Waser, Beatrice; Mansi, Rosalba; Nicolas, Guillaume P; Ketani, Eleni; Nikolopoulou, Anastasia; Fani, Melpomeni; Reubi, Jean-Claude; Maina, Theodosia

    2018-04-12

    We have previously reported on the gastrin releasing peptide receptor (GRPR) antagonist [ 99m Tc]1, ([ 99m Tc]demobesin 1, 99m Tc-[N 4 '-diglycolate-dPhe 6 ,Leu-NHEt 13 ]BBN(6-13)). [ 99m Tc]1 has shown superior biological profile compared to analogous agonist-based 99m Tc-radioligands. We herein present a small library of [ 99m Tc]1 mimics generated after structural modifications in (a) the linker ([ 99m Tc]2, [ 99m Tc]3, [ 99m Tc]4), (b) the peptide chain ([ 99m Tc]5, [ 99m Tc]6), and (c) the C-terminus ([ 99m Tc]7 or [ 99m Tc]8). The effects of above modifications on the biological properties of analogs were studied in PC-3 cells and tumor-bearing SCID mice. All analogs showed subnanomolar affinity for the human GRPR, while most receptor-affine 4 and 8 behaved as potent GRPR antagonists in a functional internalization assay. In mice bearing PC-3 tumors, [ 99m Tc]1-[ 99m Tc]6 exhibited GRPR-specific tumor uptake, rapidly clearing from normal tissues. [ 99m Tc]4 displayed the highest tumor uptake (28.8 ± 4.1%ID/g at 1 h pi), which remained high even after 24 h pi (16.3 ± 1.8%ID/g), well surpassing that of [ 99m Tc]1 (5.4 ± 0.7%ID/g at 24 h pi).

  15. Synthesis Characterization and Decomposition Studies of tris[N-N-dibenzyidithocarbaso)Indium (III) Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

    Science.gov (United States)

    Hehemann, David G.; Lau, J. Eva; Harris, Jerry D.; Hoops, Michael D.; Duffy, Norman V.

    2005-01-01

    This paper presents the results of the synthesis characterization and decomposition studies of tris[N-N-dibenzyidithocarbaso)Indium (III) with chemical spray deposition of polycrystalline CuInS2 on Copper Films.

  16. Controlled fabrication of the strong emission YVO4:Eu3+ nanoparticles and nanowires by microwave assisted chemical synthesis

    International Nuclear Information System (INIS)

    Huong, Tran Thu; Vinh, Le Thi; Phuong, Ha Thi; Khuyen, Hoang Thi; Anh, Tran Kim; Tu, Vu Duc; Minh, Le Quoc

    2016-01-01

    In this report, we are presenting the controlled fabrication results of the strong emission YVO 4 : Eu 3+ nanoparticles and nanowires by microwave which is assisted chemical synthesis. The effects of incorporated synthesis conditions such as microwave irradiated powers, pH values and concentration of chemical composition on properties of nanomaterials are also investigated to obtain the controllable size and homogenous morphology. Morphological and optical properties of YVO 4 : Eu 3+ prepared products which have been characterized by X-ray diffraction (XRD), field emission micrcroscopy (FESEM) and photoluminescence spectroscopy. As based from result of synthesized samples, we found that the changing of pH values, microwave irradiated powers and chemical composition rise to change reform the size and shape of materials from nanoparticles (diameter about 20 nm) to wires shape (with about 500÷800 nm length and 10÷20 nm width). The photoluminescence (PL) spectroscopy measurements of YVO 4 : Eu 3+ nanostructure materials under UV excitation showed that: the strong luminescence in red region with narrow lines corresponding to the intra-4f transitions of 5 D 0 – 7 F j (j=1, 2, 3, and 4) of Eu 3+ ions with the highest luminescence intensity of 5 D 0 → 7 F 2 transition. - Highlights: • The strong emission YVO 4 :Eu 3+ nanostructure materials were successfully synthesized by microwave assisted chemical synthesis. • The size, morphology and luminescence of the YVO 4 :Eu 3+ nanostructure materials can be controlled by the solution pH, microwave irradiated powers and chemical composition. • These YVO 4 :Eu 3+ nanostructure materials above can potentially applied in various fields of application, especially in luminescent labeling and visualization in biomedical application.

  17. Peptides and proteins

    Energy Technology Data Exchange (ETDEWEB)

    Bachovchin, W.W.; Unkefer, C.J.

    1994-12-01

    Advances in magnetic resonance and vibrational spectroscopy make it possible to derive detailed structural information about biomolecular structures in solution. These techniques are critically dependent on the availability of labeled compounds. For example, NMR techniques used today to derive peptide and protein structures require uniformity {sup 13}C-and {sup 15}N-labeled samples that are derived biosynthetically from (U-6-{sup 13}C) glucose. These experiments are possible now because, during the 1970s, the National Stable Isotope Resource developed algal methods for producing (U-6-{sup 13}C) glucose. If NMR techniques are to be used to study larger proteins, we will need sophisticated labelling patterns in amino acids that employ a combination of {sup 2}H, {sup 13}C, and {sup 15}N labeling. The availability of these specifically labeled amino acids requires a renewed investment in new methods for chemical synthesis of labeled amino acids. The development of new magnetic resonance or vibrational techniques to elucidate biomolecular structure will be seriously impeded if we do not see rapid progress in labeling technology. Investment in labeling chemistry is as important as investment in the development of advanced spectroscopic tools.

  18. Synthesis and characterization of nano ZnO rods via microwave assisted chemical precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Uma Sangari, N., E-mail: umasangariselvakumar@gmail.com [Department of Chemistry, S.F.R. College for Women, Sivakasi 626123 (India); Chitra Devi, S. [Department of Chemistry, S.F.R. College for Women, Sivakasi 626123 (India)

    2013-01-15

    A microwave assisted chemical precipitation method has been employed for the synthesis of nano zinc oxide rods by reacting zinc nitrate and potassium hydroxide. The amount of potassium hydroxide was adjusted for three different pHs to achieve ZnO nano rods with varying aspect ratio. The mechanism of growth of nano rods is explained briefly. The average crystallite size of the as synthesized samples was analyzed by means of powder XRD pattern and estimated to vary from 25.6 nm to 43.1 nm. The existence of rods was confirmed using scanning electron microscopy (SEM). The samples were also analyzed using FT-IR. The optical properties of the samples were also studied by means of UV-visible spectra and Room Temperature Photo Luminescence studies. The band gap of the samples was determined from the DRS spectrum. A strong near band emission peaks due to surface defects are observed in the PL spectrum. - Graphical abstract: At the solution pH of 11 and 9, tetrapod-like and flower-like ZnO nano rods were formed along with separated rods respectively due to the formation of activated nuclei of different sizes. Highlights: Black-Right-Pointing-Pointer Increase in alkalinity of the precursor solution results in longer rods. Black-Right-Pointing-Pointer Beyond a saturation limit, the excess of added OH{sup -} ions inhibited the growth of rods. Black-Right-Pointing-Pointer Keeping all parameters the same, the alkalinity can only modify the aspect ratio of the rods and not their morphology.

  19. Microwave plasma chemical synthesis of nanocrystalline carbon film structures and study their properties

    Science.gov (United States)

    Bushuev, N.; Yafarov, R.; Timoshenkov, V.; Orlov, S.; Starykh, D.

    2015-08-01

    The self-organization effect of diamond nanocrystals in polymer-graphite and carbon films is detected. The carbon materials deposition was carried from ethanol vapors out at low pressure using a highly non-equilibrium microwave plasma. Deposition processes of carbon film structures (diamond, graphite, graphene) is defined. Deposition processes of nanocrystalline structures containing diamond and graphite phases in different volume ratios is identified. The solid film was obtained under different conditions of microwave plasma chemical synthesis. We investigated the electrical properties of the nanocrystalline carbon films and identified it's from various factors. Influence of diamond-graphite film deposition mode in non-equilibrium microwave plasma at low pressure on emission characteristics was established. This effect is justified using the cluster model of the structure of amorphous carbon. It was shown that the reduction of bound hydrogen in carbon structures leads to a decrease in the threshold electric field of emission from 20-30 V/m to 5 V/m. Reducing the operating voltage field emission can improve mechanical stability of the synthesized film diamond-graphite emitters. Current density emission at least 20 A/cm2 was obtained. Nanocrystalline carbon film materials can be used to create a variety of functional elements in micro- and nanoelectronics and photonics such as cold electron source for emission in vacuum devices, photonic devices, cathodoluminescent flat display, highly efficient white light sources. The obtained graphene carbon net structure (with a net size about 6 μm) may be used for the manufacture of large-area transparent electrode for solar cells and cathodoluminescent light sources

  20. Synthesis of chemical vapor deposition graphene on tantalum wire for supercapacitor applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Guo, Wenlong [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Hongji, E-mail: hongjili@yeah.net [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Xu, Sheng [School of Precision Instrument and Optoelectronics Engineering, Tianjin University, Tianjin 300072 (China); Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2014-10-30

    Highlights: • The capacitance of graphene/tantalum (Ta) wire electrodes is firstly reported. • Graphene was grown on the Ta surface by hot-filament chemical vapor deposition. • Graphene/Ta wire structure is favorable for fast ion and electron transfer. • The graphene/Ta wire electrode shows high capacitive properties. - Abstract: This paper studies the synthesis and electrochemical characterization of graphene/tantalum (Ta) wires as high-performance electrode material for supercapacitors. Graphene on Ta wires is prepared by the thermal decomposition of methane under various conditions. The graphene nanosheets on the Ta wire surface have an average thickness of 1.3–3.4 nm and consist typically of a few graphene monolayers, and TaC buffer layers form between the graphene and Ta wire. A capacitor structure is fabricated using graphene/Ta wire with a length of 10 mm and a diameter of 0.6 mm as the anode and Pt wire of the same size as the cathode. The electrochemical behavior of the graphene/Ta wires as supercapacitor electrodes is characterized by cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy in 1 M Na{sub 2}SO{sub 4} aqueous electrolyte. The as-prepared graphene/Ta electrode has highest capacitance of 345.5 F g{sup −1} at current density of 0.5 A g{sup −1}. The capacitance remains at about 84% after 1000 cycles at 10 A g{sup −1}. The good electrochemical performance of the graphene/Ta wire electrode is attributed to the unique nanostructural configuration, high electrical conductivity, and large specific surface area of the graphene layer. This suggests that graphene/Ta wire electrode materials have potential applications in high-performance energy storage devices.

  1. Synthesis of chemical vapor deposition graphene on tantalum wire for supercapacitor applications

    International Nuclear Information System (INIS)

    Li, Mingji; Guo, Wenlong; Li, Hongji; Xu, Sheng; Qu, Changqing; Yang, Baohe

    2014-01-01

    Highlights: • The capacitance of graphene/tantalum (Ta) wire electrodes is firstly reported. • Graphene was grown on the Ta surface by hot-filament chemical vapor deposition. • Graphene/Ta wire structure is favorable for fast ion and electron transfer. • The graphene/Ta wire electrode shows high capacitive properties. - Abstract: This paper studies the synthesis and electrochemical characterization of graphene/tantalum (Ta) wires as high-performance electrode material for supercapacitors. Graphene on Ta wires is prepared by the thermal decomposition of methane under various conditions. The graphene nanosheets on the Ta wire surface have an average thickness of 1.3–3.4 nm and consist typically of a few graphene monolayers, and TaC buffer layers form between the graphene and Ta wire. A capacitor structure is fabricated using graphene/Ta wire with a length of 10 mm and a diameter of 0.6 mm as the anode and Pt wire of the same size as the cathode. The electrochemical behavior of the graphene/Ta wires as supercapacitor electrodes is characterized by cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy in 1 M Na 2 SO 4 aqueous electrolyte. The as-prepared graphene/Ta electrode has highest capacitance of 345.5 F g −1 at current density of 0.5 A g −1 . The capacitance remains at about 84% after 1000 cycles at 10 A g −1 . The good electrochemical performance of the graphene/Ta wire electrode is attributed to the unique nanostructural configuration, high electrical conductivity, and large specific surface area of the graphene layer. This suggests that graphene/Ta wire electrode materials have potential applications in high-performance energy storage devices

  2. The on-line synthesis of enzyme functionalized silica nanoparticles in a microfluidic reactor using polyethylenimine polymer and R5 peptide

    International Nuclear Information System (INIS)

    He Ping; Greenway, Gillian; Haswell, Stephen J

    2008-01-01

    A simple microfluidic reactor system is described for the effective synthesis of enzyme functionalized nanoparticles which offers many advantages over batch reactions, including excellent enzyme efficiencies. Better control of the process parameters in the microfluidic reactor system over batch based methodology enables the production of silica nanoparticles with the optimum size for efficient enzyme immobilization with long-term stability. The synthetic approach is demonstrated with glucose oxidase (GOD) and two different nucleation catalysts of similar molecular mass: the natural R5 peptide, and polyethylenimine (PEI) polymer. Near-quantitative immobilization of GOD in the nanoparticles is obtained using PEI; the immobilization is attributed to electrostatic interaction between PEI and GOD. This interaction, however, limits the mobility of the immobilized enzyme, producing orientation hindrance of the enzyme's active sites as compared to free GOD in solution. In contrast, when the GOD is immobilized inside the silica nanoparticles using R5, lower enzyme immobilization efficiencies are obtained compared to using PEI polymers; however, similar Michaelis-Menten kinetic parameters (i.e. Michaelis constant and turnover number) to those of free GOD are observed. Reactions were monitored in situ using simple, rapid, separation-free amperometric detection

  3. Design and synthesis of 4'-((5-benzylidene-2,4-dioxothiazolidin-3-yl)methyl)biphenyl-2-carbonitrile analogs as bacterial peptide deformylase inhibitors.

    Science.gov (United States)

    Khan, Firoz A Kalam; Patil, Rajendra H; Shinde, Devanand B; Sangshetti, Jaiprakash N

    2016-12-01

    Herein, we report the synthesis and screening of 4'-((5-benzylidene-2,4-dioxothiazolidin-3-yl)methyl)biphenyl-2-carbonitrile analogs 11(a-j) as bacterial peptide deformylase (PDF) enzyme inhibitors. The compounds 11b (IC 50 value = 139.28 μm), 11g (IC 50 value = 136.18 μm), and 11h (IC 50 value = 131.65 μm) had shown good PDF inhibition activity. The compounds 11b (MIC range = 103.36-167.26 μg/mL), 11g (MIC range = 93.75-145.67 μg/mL), and 11h (MIC range = 63.61-126.63 μg/mL) had also shown potent antibacterial activity when compared with standard ampicillin (MIC range = 100.00-250.00 μg/mL). Thus, the active derivatives were not only PDF inhibitors but also efficient antibacterial agents. To gain more insight on the binding mode of the compounds with PDF enzyme, the synthesized compounds 11(a-j) were docked against PDF enzyme of Escherichia coli and compounds exhibited good binding properties. The results suggest that this class of compounds has potential for development and use in future as antibacterial drugs. © 2016 John Wiley & Sons A/S.

  4. Bacterial Peptide deformylase inhibition of cyano substituted biaryl analogs: Synthesis, in vitro biological evaluation, molecular docking study and in silico ADME prediction.

    Science.gov (United States)

    Khan, Firoz A Kalam; Patil, Rajendra H; Shinde, Devanand B; Sangshetti, Jaiprakash N

    2016-08-15

    Herein, we report the synthesis and screening of cyano substituted biaryl analogs 5(a-m) as Peptide deformylase (PDF) enzyme inhibitors. The compounds 5a (IC50 value=13.16μM), 5d (IC50 value=15.66μM) and 5j (IC50 value=19.16μM) had shown good PDF inhibition activity. The compounds 5a (MIC range=11.00-15.83μg/mL), 5b (MIC range=23.75-28.50μg/mL) and 5j (MIC range=7.66-16.91μg/mL) had also shown potent antibacterial activity when compared with ciprofloxacin (MIC range=25-50μg/mL). Thus, the active derivatives were not only potent PDF inhibitors but also efficient antibacterial agents. In order to gain more insight on the binding mode of the compounds with PDF, the synthesized compounds 5(a-m) were docked against PDF enzyme of Escherichia coli and compounds exhibited good binding properties. In silico ADME properties of synthesized compounds were also analyzed and showed potential to develop as good oral drug candidates. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Bacteria–zinc co-localization implicates enhanced synthesis of cysteine-rich peptides in zinc detoxification when Brassica juncea is inoculated with Rhizobium leguminosarum

    Science.gov (United States)

    Adediran, Gbotemi A; Ngwenya, Bryne T; Mosselmans, J Frederick W; Heal, Kate V

    2016-01-01

    Some plant growth promoting bacteria (PGPB) are enigmatic in enhancing plant growth in the face of increased metal accumulation in plants. Since most PGPB colonize the plant root epidermis, we hypothesized that PGPB confer tolerance to metals through changes in speciation at the root epidermis. We employed a novel combination of fluorophore-based confocal laser scanning microscopic imaging and synchrotron based microscopic X-ray fluorescence mapping with X-ray absorption spectroscopy to characterize bacterial localization, zinc (Zn) distribution and speciation in the roots of Brassica juncea grown in Zn contaminated media (400 mg kg−1 Zn) with the endophytic Pseudomonas brassicacearum and rhizospheric Rhizobium leguminosarum. PGPB enhanced epidermal Zn sequestration relative to PGBP-free controls while the extent of endophytic accumulation depended on the colonization mode of each PGBP. Increased root accumulation of Zn and increased tolerance to Zn was associated predominantly with R. leguminosarum and was likely due to the coordination of Zn with cysteine-rich peptides in the root endodermis, suggesting enhanced synthesis of phytochelatins or glutathione. Our mechanistic model of enhanced Zn accumulation and detoxification in plants inoculated with R. leguminosarum has particular relevance to PGPB enhanced phytoremediation of soils contaminated through mining and oxidation of sulphur-bearing Zn minerals or engineered nanomaterials such as ZnS. PMID:26263508

  6. Fiscal 1993 report on results of R and D on innovative technology for producing advanced biomaterial. Peptide applied carbon dioxide fixation/effective utilization technology (Second volume: comprehensive investigation and research); 1993 nendo senshin bio zairyo no sosei kako gijutsu no kenkyu kaihatsu seika hokokusho (sogo chosa kenkyu). 2. Peptide oyo nisanka tanso koteika yuko riyo gijutsu

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-03-01

    Technology was developed for preparing functional materials by synthesizing new functional peptides in which non-natural amino acid needed for the functional manifestation was introduced, and by fixing the peptides to the surface of a base plate such as silica glass or modifying the surface with them. As the related technological investigation, the following six areas were surveyed. (1) Structural design of peptides, (2) synthesis of peptides by chemical and enzyme methods, (3) synthesis of non-natural amino acid and its introduction into peptides, (4) structural analysis of peptides, (5) physiological activity of peptides, and (6) materialization and functional manifestation of peptides. With the exception of the area (5) consisting of one advanced research case, other areas were constituted of analysis, general remarks and research cases. The area (6) was constituted of materialization technique 1 and 2, film function and peptide, catalytic action 1 and 2, and one research case; the materialization technique was defined as a technique for modifying the surface of a synthetic resin, metallic or silica glass substrate with functional peptides; and an explanation was given to the present state of the fixation, pattern formation and integration technologies. (NEDO)

  7. Enzymes as modular catalysts for redox half-reactions in H2-powered chemical synthesis: from biology to technology.

    Science.gov (United States)

    Reeve, Holly A; Ash, Philip A; Park, HyunSeo; Huang, Ailun; Posidias, Michalis; Tomlinson, Chloe; Lenz, Oliver; Vincent, Kylie A

    2017-01-15

    The present study considers the ways in which redox enzyme modules are coupled in living cells for linking reductive and oxidative half-reactions, and then reviews examples in which this concept can be exploited technologically in applications of coupled enzyme pairs. We discuss many examples in which enzymes are interfaced with electronically conductive particles to build up heterogeneous catalytic systems in an approach which could be termed synthetic biochemistry We focus on reactions involving the H + /H 2 redox couple catalysed by NiFe hydrogenase moieties in conjunction with other biocatalysed reactions to assemble systems directed towards synthesis of specialised chemicals, chemical building blocks or bio-derived fuel molecules. We review our work in which this approach is applied in designing enzyme-modified particles for H 2 -driven recycling of the nicotinamide cofactor NADH to provide a clean cofactor source for applications of NADH-dependent enzymes in chemical synthesis, presenting a combination of published and new work on these systems. We also consider related photobiocatalytic approaches for light-driven production of chemicals or H 2 as a fuel. We emphasise the techniques available for understanding detailed catalytic properties of the enzymes responsible for individual redox half-reactions, and the importance of a fundamental understanding of the enzyme characteristics in enabling effective applications of redox biocatalysis. © 2017 The Author(s).

  8. Synthesis of Intrinsically Disordered Fluorinated Peptides for Modular Design of High-Signal 19 F MRI Agents.

    Science.gov (United States)

    Kirberger, Steven E; Maltseva, Sofia D; Manulik, Joseph C; Einstein, Samuel A; Weegman, Bradley P; Garwood, Michael; Pomerantz, William C K

    2017-06-01

    19 F MRI is valuable for in vivo imaging due to the only trace amounts of fluorine in biological systems. Because of the low sensitivity of MRI however, designing new fluorochemicals remains a significant challenge for achieving sufficient 19 F signal. Here, we describe a new class of high-signal, water-soluble fluorochemicals as 19 F MRI imaging agents. A polyamide backbone is used for tuning the proteolytic stability to avoid retention within the body, which is a limitation of current state-of-the-art perfluorochemicals. We show that unstructured peptides containing alternating N-ϵ-trifluoroacetyllysine and lysine provide a degenerate 19 F NMR signal. 19 F MRI phantom images provide sufficient contrast at micromolar concentrations, showing promise for eventual clinical applications. Finally, the degenerate high signal characteristics were retained when conjugated to a large protein, indicating potential for in vivo targeting applications, including molecular imaging and cell tracking. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Peptide dendrimer-conjugates of ketoprofen: Synthesis and ex vivo and in vivo evaluations of passive diffusion, sonophoresis and iontophoresis for skin delivery.

    Science.gov (United States)

    Hegde, Aswathi R; Rewatkar, Prarthana V; Manikkath, Jyothsna; Tupally, Karnaker; Parekh, Harendra S; Mutalik, Srinivas

    2017-05-01

    The aim of this study was to evaluate skin delivery of ketoprofen when covalently tethered to mildly cationic (2 + or 4 + ) peptide dendrimers prepared wholly by solid phase peptide synthesis. The amino acids glycine, arginine and lysine formed the dendrimer with ketoprofen tethered either to the lysine side-arm (N ε ) or periphery of dendrimeric branches. Passive diffusion, sonophoresis- and iontophoresis-assisted permeation of each peptide dendrimer-drug conjugate (D1-D4) was studied across mouse skin, both in vitro and in vivo. In addition, skin toxicity of dendrimeric conjugates when trialed with iontophoresis or sonophoresis was also evaluated. All dendrimeric conjugates improved aqueous solubility at least 5-fold, compared to ketoprofen alone, while also exhibiting appreciable lipophilicity. In vitro passive diffusion studies revealed that ketoprofen in its native form was delivered to a greater extent, compared with a dendrimer-conjugated form at the end of 24h (Q 24h (μg/cm 2 ): ketoprofen (68.06±3.62)>D2 (49.62±2.92)>D4 (19.20±0.89)>D1 (6.45±0.40)>D3 (2.21±0.19). However, sonophoresis substantially increased the skin permeation of ketoprofen-dendrimer conjugates in 30min (Q 30min (μg/cm 2 ): D4 (122.19±7.14)>D2 (66.74±3.86)>D1 (52.10±3.22)>D3 (41.66±3.22)) although ketoprofen alone again proved superior (Q 30min : 167.99±9.11μg/cm 2 ). Next, application of iontophoresis was trialed and shown to considerably increase permeation of dendrimeric ketoprofen in 6h (Q 6h (μg/cm 2 ): D2 (711.49±39.14)>D4 (341.23±16.43)>D3 (89.50±4.99)>D1 (50.91±2.98), with a Q 6h value of 96.60±5.12μg/cm 2 for ketoprofen alone). In vivo studies indicated that therapeutically relevant concentrations of ketoprofen could be delivered transdermally when iontophoresis was paired with D2 (985.49±43.25ng/mL). Further, histopathological analysis showed that the dendrimeric approach was a safe mode as ketoprofen alone. The present study successfully demonstrates that

  10. Toward Peptide Nucleic Acid (PNA) Directed Peptide Translation Using Ester Based Aminoacyl Transfer

    DEFF Research Database (Denmark)

    Singhal, Abhishek; Bagnacani, Valentina; Corradini, Roberto

    2014-01-01

    Peptide synthesis is a fundamental feature of life. However, it still remains unclear how the contemporary translation apparatus evolved from primitive prebiotic systems and at which stage of the evolution peptide synthesis emerged. Using simple molecular architectures, in which aminoacyl transfe...

  11. Quantum chemical analysis explains hemagglutinin peptide-MHC Class II molecule HLA-DRβ1*0101 interactions

    International Nuclear Information System (INIS)

    Cardenas, Constanza; Villaveces, Jose Luis; Bohorquez, Hugo; Llanos, Eugenio; Suarez, Carlos; Obregon, Mateo; Patarroyo, Manuel Elkin

    2004-01-01

    We present a new method to explore interactions between peptides and major histocompatibility complex (MHC) molecules using the resultant vector of the three principal multipole terms of the electrostatic field expansion. Being that molecular interactions are driven by electrostatic interactions, we applied quantum chemistry methods to better understand variations in the electrostatic field of the MHC Class II HLA-DRβ1*0101-HA complex. Multipole terms were studied, finding strong alterations of the field in Pocket 1 of this MHC molecule, and weak variations in other pockets, with Pocket 1 >> Pocket 4 > Pocket 9 ∼ Pocket 7 > Pocket 6. Variations produced by 'ideal' amino acids and by other occupying amino acids were compared. Two types of interactions were found in all pockets: a strong unspecific one (global interaction) and a weak specific interaction (differential interaction). Interactions in Pocket 1, the dominant pocket for this allele, are driven mainly by the quadrupole term, confirming the idea that aromatic rings are important in these interactions. Multipolar analysis is in agreement with experimental results, suggesting quantum chemistry methods as an adequate methodology to understand these interactions

  12. Synthesis of Monodispersed Spherical Single Crystalline Silver Particles by Wet Chemical Process; Shisshiki kagakuho ni yoru tanbunsankyujo tankesshoginryushi no gose

    Energy Technology Data Exchange (ETDEWEB)

    Ueyama, Ryousuke.; Harada, Masahiro.; Ueyama, Tamotsu.; Harada, Akio. [Daiken Chemistry Industry Corporation, Osaka (Japan); Yamamoto, Takashi. [National Defence Academy, Kanagawa (Japan). Dept. of Electrical Engineering; Shiosaki, Tadashi. [Nara Institute of Science and Technology, Nara (Japan). Graduate School of Materials Science; Kuribayashi, Kiyoshi. [Teikyo University of Science and Technology, Yamanashi (Japan). Dept. of Materials

    1999-01-01

    Ultrafine silver monodispersed particle were prepared by wet chemical process. To decrease the reduction speed, an important factor in generating monodispersed particles is to control the following three factors: synthesis temperature, concentration of aggregation-relaxing agent added, and concentration of silver nitrate solution. Synthesis of monodispersed spherical Ag particles, used as metal powders for electrode, became possible using the nucleus grouwth reaction method. This process also allowed the control of the diameter of the powder particles. The silver particles were distributed in ta narrow particle diameter range with on average of 0.5 {mu}m. Transmission electron microscopy (TEM) revealed that single-crystalline silver particles were prepared by the present method. (author)

  13. Bringing the science of proteins into the realm of organic chemistry: total chemical synthesis of SEP (synthetic erythropoiesis protein).

    Science.gov (United States)

    Kent, Stephen B H

    2013-11-11

    Erythropoietin, commonly known as EPO, is a glycoprotein hormone that stimulates the production of red blood cells. Recombinant EPO has been described as "arguably the most successful drug spawned by the revolution in recombinant DNA technology". Recently, the EPO glycoprotein molecule has re-emerged as a major target of synthetic organic chemistry. In this article I will give an account of an important body of earlier work on the chemical synthesis of a designed EPO analogue that had full biological activity and improved pharmacokinetic properties. The design and synthesis of this "synthetic erythropoiesis protein" was ahead of its time, but has gained new relevance in recent months. Here I will document the story of one of the major accomplishments of synthetic chemistry in a more complete way than is possible in the primary literature, and put the work in its contemporaneous context. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Chemical control of the characteristics of Mo-doped carbon xerogels by surfactant-mediated synthesis

    Czech Academy of Sciences Publication Activity Database

    Maldonado-Hódar, F. J.; Jirglová, Hana; Pérez-Cadenas, A. F.; Morales-Torres, S.

    2013-01-01

    Roč. 51, JAN 2013 (2013), s. 213-223 ISSN 0008-6223 Institutional support: RVO:61388955 Keywords : synthesis * molybdenum * carbon xerogels Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 6.160, year: 2013

  15. Chiral Symmetry Breaking in Peptide Systems During Formation of Life on Earth

    Science.gov (United States)

    Konstantinov, Konstantin K.; Konstantinova, Alisa F.

    2018-03-01

    Chiral symmetry breaking in complex chemical systems with a large number of amino acids and a large number of similar reactions was considered. It was shown that effective averaging over similar reaction channels may result in very weak effective enantioselectivity of forward reactions, which does not allow most of the known models to result in chiral symmetry breaking during formation of life on Earth. Models with simple and catalytic synthesis of a single amino acid, formation of peptides up to length five, and sedimentation of insoluble pair of substances were considered. It was shown that depending on the model and the values of the parameters, chiral symmetry breaking may occur in up to about 10% out of all possible unique insoluble pair combinations even in the absence of any catalytic synthesis and that minimum total number of amino acids in the pair is 5. If weak enantioselective forward catalytic synthesis of amino acids is present, then the number of possible variants, in which chiral symmetry breaking may occur, increases substantially. It was shown that that the most interesting catalysts have zero or one amino acid of "incorrect" chirality. If the parameters of the model are adjusted in such a way to result in an increase of concentration of longer peptides, then catalysts with two amino acids of incorrect chirality start to appear at peptides of length five. Models of chiral symmetry breaking in the presence of epimerization were considered for peptides up to length three. It was shown that the range of parameters in which chiral symmetry breaking could occur significantly shrinks in comparison to previously considered models with peptides up to length two. An experiment of chiral symmetry breaking was proposed. The experiment consists of a three-step cycle: reversible catalytic synthesis of amino acids, reversible synthesis of peptides, and irreversible sedimentation of insoluble substances.

  16. Synthesis of silver nanoparticles by chemical reduction at various fraction of MSA and their structure characterization

    Energy Technology Data Exchange (ETDEWEB)

    Diantoro, Markus, E-mail: m-diantoror@yahoo.com; Fitrianingsih, Rina, E-mail: m-diantoror@yahoo.com; Mufti, Nandang, E-mail: m-diantoror@yahoo.com; Fuad, Abdulloh, E-mail: m-diantoror@yahoo.com [Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Negeri Malang (UM), Jl. Semarang No. 5 Malang 65145 (Indonesia)

    2014-03-24

    Nanosilver is currently one of the most common engineered nanomaterials and is used in many applications that lead to the release of silver nanoparticles and silver ions into aqueous systems. Nanosilver also possesses enhanced antimicrobial activity and bioavailability that may less environmental risk compared with other manufactured nanomaterials. Described in this research are the synthesis of silver nanoparticle produced by chemical reduction from silver nitrate (AgNO{sub 3}) solution. As a reducing agent, Sodium Borohydride (NaBH{sub 4}) was used and mercaptosuccinic Acid (MSA) as stabilizer to prevent the nanoparticle from aglomerating. It was also used two kinds of solvent, they are water and methanol. In typical experiment MSA was dissolve in methanol with a number of variation of molarity i.e. 0,03 M, 0,06 M, 0,12 M, 0,15 M, and the mixture was kept under vigorous stirring in an ice bath. A solution of silver nitrate of 340 mg in 6,792 ml water was added. A freshly prepared aqueous solution of sodium borohydride (756,6 mL in 100 mL of water) was added drop wisely. The solution was kept for half an hour for stirring and were allowed to settle down in methanol. The obtained samples then characterized by means of x-ray diffractometer, and scanning electron microscopy, as well as transmission electron microscopy to obtain their structures of silver nanoparticles, morphology, and sizes. It is shown that diameter of silver nanoparticle sized about 24.3 nm (Ag@MSA 0.03 M), 20.4 nm (Ag@MSA 0.06 M), 16.8 nm (Ag@MSA 0.12 M), 16.9 nm (Ag@MSA 0.15 M) which was calculated by Scherrer formula by taking the FWHM from fitting to Gaussian. The phases and lattice parameter showed that there is no significant change in its volume by increasing molarity of stabilizer. In contrast, the size of particles is decreasing.

  17. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    Energy Technology Data Exchange (ETDEWEB)

    Sankapal, B.R., E-mail: brsankapal@rediffmail.com [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K. [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Gupta, V.; Chand, S. [Organic and Hybrid Solar Cell, Physics of Energy Harvesting Division, Dr. K.S. Krishnan Marg, National Physical Laboratory, New Delhi 110012 (India)

    2011-10-13

    Highlights: > Simple, inexpensive and room temperature chemical synthesis route. > Highly oriented PbSe nanotubes from Cd(OH){sub 2} nanowires through lead hydroxination. > The process was template free without the use of any capping agent. > Reaction kinetics was accomplished due to more negative free energy of formation. > The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd{sup 2+} with Pb{sup 2+} ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  18. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    International Nuclear Information System (INIS)

    Sankapal, B.R.; Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K.; Gupta, V.; Chand, S.

    2011-01-01

    Highlights: → Simple, inexpensive and room temperature chemical synthesis route. → Highly oriented PbSe nanotubes from Cd(OH) 2 nanowires through lead hydroxination. → The process was template free without the use of any capping agent. → Reaction kinetics was accomplished due to more negative free energy of formation. → The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd 2+ with Pb 2+ ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  19. Pressure dependence of backbone chemical shifts in the model peptides Ac-Gly-Gly-Xxx-Ala-NH2.

    Science.gov (United States)

    Erlach, Markus Beck; Koehler, Joerg; Crusca, Edson; Kremer, Werner; Munte, Claudia E; Kalbitzer, Hans Robert

    2016-06-01

    For a better understanding of nuclear magnetic resonance (NMR) detected pressure responses of folded as well as unstructured proteins the availability of data from well-defined model systems are indispensable. In this work we report the pressure dependence of chemical shifts of the backbone atoms (1)H(α), (13)C(α) and (13)C' in the protected tetrapeptides Ac-Gly-Gly-Xxx-Ala-NH2 (Xxx one of the 20 canonical amino acids). Contrary to expectation the chemical shifts of these nuclei have a nonlinear dependence on pressure in the range from 0.1 to 200 MPa. The polynomial pressure coefficients B 1 and B 2 are dependent on the type of amino acid studied. The coefficients of a given nucleus show significant linear correlations suggesting that the NMR observable pressure effects in the different amino acids have at least partly the same physical cause. In line with this observation the magnitude of the second order coefficients of nuclei being direct neighbors in the chemical structure are also weakly correlated.

  20. Pressure dependence of backbone chemical shifts in the model peptides Ac-Gly-Gly-Xxx-Ala-NH{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Erlach, Markus Beck; Koehler, Joerg [University of Regensburg, Institute of Biophysics and Physical Biochemistry and Centre of Magnetic Resonance in Chemistry and Biomedicine (Germany); Crusca, Edson [University of São Paulo, Physics Institute of São Carlos (Brazil); Kremer, Werner [University of Regensburg, Institute of Biophysics and Physical Biochemistry and Centre of Magnetic Resonance in Chemistry and Biomedicine (Germany); Munte, Claudia E. [University of São Paulo, Physics Institute of São Carlos (Brazil); Kalbitzer, Hans Robert, E-mail: hans-robert.kalbitzer@biologie.uni-regensburg.de [University of Regensburg, Institute of Biophysics and Physical Biochemistry and Centre of Magnetic Resonance in Chemistry and Biomedicine (Germany)

    2016-06-15

    For a better understanding of nuclear magnetic resonance (NMR) detected pressure responses of folded as well as unstructured proteins the availability of data from well-defined model systems are indispensable. In this work we report the pressure dependence of chemical shifts of the backbone atoms {sup 1}H{sup α}, {sup 13}C{sup α} and {sup 13}C′ in the protected tetrapeptides Ac-Gly-Gly-Xxx-Ala-NH{sub 2} (Xxx one of the 20 canonical amino acids). Contrary to expectation the chemical shifts of these nuclei have a nonlinear dependence on pressure in the range from 0.1 to 200 MPa. The polynomial pressure coefficients B{sub 1} and B{sub 2} are dependent on the type of amino acid studied. The coefficients of a given nucleus show significant linear correlations suggesting that the NMR observable pressure effects in the different amino acids have at least partly the same physical cause. In line with this observation the magnitude of the second order coefficients of nuclei being direct neighbors in the chemical structure are also weakly correlated.Graphical Abstract.

  1. A fast chemical route for the synthesis of TBHQ functionalized reduced graphene oxide and its electrochemical performances

    Energy Technology Data Exchange (ETDEWEB)

    Rana, Subhasis; Sen, Pintu, E-mail: psen@vecc.gov.in; Bandyopadhyay, S.K.

    2016-02-01

    A fast chemical route for the synthesis of tertiary butyl hydroquinone (TBHQ) functionalized reduced graphene oxide (FRGO) and their application as high performance electrode materials for supercapacitors have been reported. Reductions of chemically exfoliated graphene oxides (GO) in the presence of small amount of TBHQ (1–2 wt % with respect to GO) at various time periods were investigated through XRD, FTIR and Raman studies. Reappearance of broad diffraction peak close to graphite peak (002) reveals an efficient method of reduction of different oxygen containing functional groups present in GO/FGO resulting in a decrease of interlayer d-spacing (∼3.5 Å). Absence of the absorption peaks in FTIR for –C=O, t-O–H, epoxide and alkoxy groups supports the complete reduction of GO to FRGO by hydrazine hydrate within a short time period of 4 h reduction under reflux condition. A large red shift in UV spectrum of FRGO – 4 h (270 nm) reveals the complete reduction of graphene oxide. The average crystallite sp{sup 2} domains sizes have been estimated through Raman spectroscopy. Plausible mechanism of TBHQ assisted fast chemical reduction of FGO has been enumerated. 1.5 wt % TBHQ in FRGO shows the best electrochemical performance where TBHQ not only acts as a reducing agent during functionalization, but also plays as an active redox molecule for enhanced capacitance of 200 F/g. - Highlights: • A fast chemical route has been adopted for the synthesis of TBHQ functionalized RGO. • The kinetics of chemical reduction becomes faster in the presence of TBHQ. • The FTIR spectrum of functionalized RGO supports the complete reduction process. • TBHQ also plays a vital role for enhancing capacitance of functionalized RGO.

  2. Cancer therapy with alpha-emitters labeled peptides.

    Science.gov (United States)

    Dadachova, Ekaterina

    2010-05-01

    Actively targeted alpha-particles offer specific tumor cell killing action with less collateral damage to surrounding normal tissues than beta-emitters. During the last decade, radiolabeled peptides that bind to different receptors on the tumors have been investigated as potential therapeutic agents both in the preclinical and clinical settings. Advantages of radiolabeled peptides over antibodies include relatively straightforward chemical synthesis, versatility, easier radiolabeling, rapid clearance from the circulation, faster penetration and more uniform distribution into tissues, and less immunogenicity. Rapid internalization of the radiolabeled peptides with equally rapid re-expression of the cell surface target is a highly desirable property that enhances the total delivery of these radionuclides into malignant sites. Peptides, such as octreotide, alpha-melanocyte-stimulating hormone analogues, arginine-glycine-aspartic acid-containing peptides, bombesin derivatives, and others may all be feasible for use with alpha-emitters. The on-going preclinical work has primarily concentrated on octreotide and octreotate analogues labeled with Bismuth-213 and Astatine-211. In addition, alpha-melanocyte-stimulating hormone analogue has been labeled with Lead-212/Bismuth-212 in vivo generator and demonstrated the encouraging therapeutic efficacy in treatment of experimental melanoma. Obstacles that continue to obstruct widespread acceptance of alpha-emitter-labeled peptides are primarily the supply of these radionuclides and concerns about potential kidney toxicity. New sources and methods for production of these medically valuable radionuclides and better understanding of mechanisms related to the peptide renal uptake and clearance should speed up the introduction of alpha-emitter-labeled peptides into the clinic. Copyright 2010 Elsevier Inc. All rights reserved.

  3. Peptide dendrimers

    Czech Academy of Sciences Publication Activity Database

    Niederhafner, Petr; Šebestík, Jaroslav; Ježek, Jan

    2005-01-01

    Roč. 11, - (2005), 757-788 ISSN 1075-2617 R&D Projects: GA ČR(CZ) GA203/03/1362 Institutional research plan: CEZ:AV0Z40550506 Keywords : multiple antigen peptides * peptide dendrimers * synthetic vaccine * multipleantigenic peptides Subject RIV: CC - Organic Chemistry Impact factor: 1.803, year: 2005

  4. Synthesis of silver nanoparticles by radiolysis, photolysis and chemical reduction of AgNO3 in Hibiscus sabdariffa infusion (karkade)

    International Nuclear Information System (INIS)

    Cataldo, Franco; Ursini, Ornella; Angelini, Giancarlo

    2016-01-01

    Silver nanoparticles of different average diameters were synthesized by γ-radiolysis, UV-photolysis and chemical reduction of AgNO 3 solutions in Hibiscus sabdariffa infusion commonly known as 'karkade'. The UV-photolysis was performed either by using a conventional Hg low pressure lamp emitting at 254 nm and also by using a new compact UV-LED source emitting at 360 nm. The kinetics rate constant of silver nanoparticles synthesis produced by γ-radiolysis and UV photolysis were determined and the average diameter of the resulting nanoparticles was estimated. (author)

  5. Synthesis of dispersive iron or iron–silver nanoparticles on engineered capsid pVIII of M13 virus with electronegative terminal peptides

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Shuai; Nakano, Kazuhiko; Zhang, Shu-liang; Yu, Hui-min, E-mail: yuhm@tsinghua.edu.cn [Tsinghua University, Key Laboratory of Industrial Biocatalysis of the Ministry of Education, Department of Chemical Engineering (China)

    2015-10-15

    M13 is a filamentous Escherichia coli virus covered with five types of capsid proteins, in which pVIII with ∼2700 copies was around the cylindered surface and pIII with five copies located at one end of the phage particle. The pIII-engineered M13 phages with enhanced binding specificity toward Fe were screened after five rounds of biopanning, and the one containing ATPTVAMSLSPL peptide at pIII-terminus was selected for mediated synthesis of zero valent (ZV) Fe nanoparticles (NPs) with the wild M13 as control. Under a reducing environment, uniformly dispersed ZVFeNPs with diameter of 5–10 nm were both synthesized and the morphologies after annealing were confirmed to be face-centered cubic type. The synthesized FeNPs mediated by the two phages showed no significant difference, revealing that the pVIII capsid did dominant contribution to metal binding in comparison with the pIII. A novel pVIII-engineered M13 containing AAEEEDPAK at terminus, named as 4ED-pVIII-M13, was constructed and it carried one more negatively charged residue than the wild one (AEGDDPAK). Metal adsorption quantification showed that the binding affinity of the 4ED-pVIII-M13 toward Ag and Ni ions improved to 62 and 18 % from original 21 and 6 %, respectively. The binding affinity toward Fe remained constant (∼85 %). ZVFe–Ag bi-NPs were successfully synthesized through mediation of 4ED-pVIII-M13. Particularly, the Fe:Ag ratio in the bi-NPs was conveniently controlled through changing the molar concentration of FeCl{sub 2} and AgNO{sub 3} solution before reduction.

  6. Antisense Oligonucleotides Internally Labeled with Peptides Show Improved Target Recognition and Stability to Enzymatic Degradation

    DEFF Research Database (Denmark)

    Taskova, Maria; Madsen, Charlotte S.; Jensen, Knud J.

    2017-01-01

    Specific target binding and stability in diverse biological media is of crucial importance for applications of synthetic oligonucleotides as diagnostic and therapeutic tools. So far, these issues have been addressed by chemical modification of oligonucleotides and by conjugation with a peptide, m...... and makes internally labeled POCs an exciting object of study, i.e., showing high target specificity and simultaneous stability in biological media.......Specific target binding and stability in diverse biological media is of crucial importance for applications of synthetic oligonucleotides as diagnostic and therapeutic tools. So far, these issues have been addressed by chemical modification of oligonucleotides and by conjugation with a peptide......, most often at the terminal position of the oligonucleotide. Herein, we for the first time systematically investigate the influence of internally attached short peptides on the properties of antisense oligonucleotides. We report the synthesis and internal double labeling of 21-mer oligonucleotides...

  7. Systematic methods for synthesis and design of sustainable chemical and biochemical processes

    DEFF Research Database (Denmark)

    Gani, Rafiqul

    Chemical and biochemical process design consists of designing the process that can sustainably manufacture an identified chemical product through a chemical or biochemical route. The chemical product tree is potentially very large; starting from a set of basic raw materials (such as petroleum...... for process intensification, sustainable process design, identification of optimal biorefinery models as well as integrated process-control design, and chemical product design. The lecture will present the main concepts, the decomposition based solution approach, the developed methods and tools together...

  8. Chemical structure, biosynthesis and synthesis of free and glycosylated pyridinolines formed by cross-link of bone and synovium collagen.

    Science.gov (United States)

    Anastasia, Luigi; Rota, Paola; Anastasia, Mario; Allevi, Pietro

    2013-09-21

    This review focuses on the chemical structure, biosynthesis and synthesis of free and glycosylated pyridinolines (Pyds), fluorescent collagen cross-links, with a pyridinium salt structure. Pyds derive from the degradation of bone collagen and have attracted attention for their use as biochemical markers of bone resorption and to assess fracture risk prediction in persons suffering from osteoporosis, bone cancer and other bone or collagen diseases. We consider and critically discuss all reported syntheses of free and glycosylated Pyds evidencing an unrevised chemistry, original and of general utility, analysis of which allows us to also support a previously suggested non-enzymatic formation of Pyds in collagen better rationalizing and justifying the chemical events.

  9. Design, Synthesis and Evaluation of Branched RRWQWR-Based Peptides as Antibacterial Agents Against Clinically Relevant Gram-Positive and Gram-Negative Pathogens

    Directory of Open Access Journals (Sweden)

    Sandra C. Vega

    2018-03-01

    Full Text Available Multidrug resistance of pathogenic bacteria has become a public health crisis that requires the urgent design of new antibacterial drugs such as antimicrobial peptides (AMPs. Seeking to obtain new, lactoferricin B (LfcinB-based synthetic peptides as viable early-stage candidates for future development as AMPs against clinically relevant bacteria, we designed, synthesized and screened three new cationic peptides derived from bovine LfcinB. These peptides contain at least one RRWQWR motif and differ by the copy number (monomeric, dimeric or tetrameric and structure (linear or branched of this motif. They comprise a linear palindromic peptide (RWQWRWQWR, a dimeric peptide (RRWQWR2KAhx and a tetrameric peptide (RRWQWR4K2Ahx2C2. They were screened for antibacterial activity against Enterococcus faecalis (ATCC 29212 and ATCC 51575 strains, Pseudomonas aeruginosa (ATCC 10145 and ATCC 27853 strains and clinical isolates of two Gram-positive bacteria (Enterococcus faecium and Staphylococcus aureus and two Gram-negative bacteria (Klebsiella pneumoniae and Pseudomonas aeruginosa. All three peptides exhibited greater activity than did the reference peptide, LfcinB (17–31, which contains a single linear RRWQWR motif. Against the ATCC reference strains, the three new peptides exhibited minimum inhibitory concentration (MIC50 values of 3.1–198.0 μM and minimum bactericidal concentration (MBC values of 25–200 μM, and against the clinical isolates, MIC50 values of 1.6–75.0 μM and MBC values of 12.5–100 μM. However, the tetrameric peptide was also found to be strongly hemolytic (49.1% at 100 μM. Scanning Electron Microscopy (SEM demonstrated that in the dimeric and tetrameric peptides, the RRWQWR motif is exposed to the pathogen surface. Our results may inform the design of new, RRWQWR-based AMPs.

  10. Parametric study of waste chicken fat catalytic chemical vapour deposition for controlled synthesis of vertically aligned carbon nanotubes

    Science.gov (United States)

    Suriani, A. B.; Dalila, A. R.; Mohamed, A.; Rosmi, M. S.; Mamat, M. H.; Malek, M. F.; Ahmad, M. K.; Hashim, N.; Isa, I. M.; Soga, T.; Tanemura, M.

    2016-12-01

    High-quality vertically aligned carbon nanotubes (VACNTs) were synthesised using ferrocene-chicken oil mixture utilising a thermal chemical vapour deposition (TCVD) method. Reaction parameters including vaporisation temperature, catalyst concentration and synthesis time were examined for the first time to investigate their influence on the growth of VACNTs. Analysis via field emission scanning electron microscopy and micro-Raman spectroscopy revealed that the growth rate, diameter and crystallinity of VACNTs depend on the varied synthesis parameters. Vaporisation temperature of 570°C, catalyst concentration of 5.33 wt% and synthesis time of 60 min were considered as optimum parameters for the production of VACNTs from waste chicken fat. These parameters are able to produce VACNTs with small diameters in the range of 15-30 nm and good quality (ID/IG 0.39 and purity 76%) which were comparable to those synthesised using conventional carbon precursor. The low turn on and threshold fields of VACNTs synthesised using optimum parameters indicated that the VACNTs synthesised using waste chicken fat are good candidate for field electron emitter. The result of this study therefore can be used to optimise the growth and production of VACNTs from waste chicken fat in a large scale for field emission application.

  11. Synthesis and characterization of M-type barium hexferrite by ultrasonic inter-dispersion of chemical precipitate

    International Nuclear Information System (INIS)

    Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T.

    2010-01-01

    This work is concerned with the study the synthesis and characterization of M-type barium hexaferrite powder by chemical precipitation type and ultrasonic interdispersion of precursor materials Fe(OH) 3 and Ba(OH) 2 ,separately and ultrasonic inter-dispersion, followed by drying and calcining. In order to guide the experimental work was carried out a preliminary thermodynamic analysis of the system Ba-Fe-H 2 O at 25 deg C. The study shows that the phase formation of M-type barium hexaferrite is obtained at a calcination at 1000 deg C, characterized by X-ray diffraction, the grain growth of the final product of synthesis depending on the calcination temperature is visible by SEM. The synthesis method developed in this research is an option to achieve the results that would be obtained if the co-precipitation of ferric and barium hydroxide was thermodynamically possible, where you can get crystallization of barium hexaferrite in a calcination at 1000 deg C. (author)

  12. Inhibition of DNA synthesis by chemical carcinogens in cultures of initiated and normal proliferating rat hepatocytes

    International Nuclear Information System (INIS)

    Novicki, D.L.; Rosenberg, M.R.; Michalopoulos, G.

    1985-01-01

    Rat hepatocytes in primary culture can be stimulated to replicate under the influence of rat serum and sparse plating conditions. Higher replication rates are induced by serum from two-thirds partially hepatectomized rats. The effects of carcinogens and noncarcinogens on the ability of hepatocytes to synthesize DNA were examined by measuring the incorporation of [3H]thymidine by liquid scintillation counting and autoradiography. Hepatocyte DNA synthesis was not decreased by ethanol or dimethyl sulfoxide at concentrations less than 0.5%. No effect was observed when 0.1 mM ketamine, Nembutal, hypoxanthine, sucrose, ascorbic acid, or benzo(e)pyrene was added to cultures of replicating hepatocytes. Estrogen, testosterone, tryptophan, and vitamin E inhibited DNA synthesis by approximately 50% at 0.1 mM, a concentration at which toxicity was noticeable. Several carcinogens requiring metabolic activation as well as the direct-acting carcinogen N-methyl-N'-nitro-N-nitrosoguanidine interfered with DNA synthesis. Aflatoxin B1 inhibited DNA synthesis by 50% (ID50) at concentrations between 1 X 10(-8) and 1 X 10(-7) M. The ID50 for 2-acetylaminofluorene was between 1 X 10(-7) and 1 X 10(-6) M. Benzo(a)pyrene and 3'-methyl-4-dimethylaminoazobenzene inhibited DNA synthesis 50% between 1 X 10(-5) and 1 X 10(-4) M. Diethylnitrosamine and dimethylnitrosamine (ID50 between 1 X 10(-4) and 5 X 10(-4) M) and 1- and 2-naphthylamine (ID50 between 1 X 10(-5) and 5 X 10(-4) M) caused inhibition of DNA synthesis at concentrations which overlapped with concentrations that caused measurable toxicity

  13. Influence of the dopant during the one step mechano-chemical synthesis of sodium alanate

    International Nuclear Information System (INIS)

    Rongeat, C; Geipel, C; Llamas-Jansa, I; Schultz, L; Gutfleisch, O

    2009-01-01

    High-pressure reactive milling under hydrogen atmosphere is used for the one-step synthesis of doped sodium alanate. In-situ monitoring of the pressure and the temperature inside the vial gives a direct feedback about the reactions occurring during the milling. This information is used to study the influence of the dopant during synthesis, e.g. the amount of dopant added. The study of the pressure variations during milling is a reliable tool for screening the efficiency of different dopants.

  14. The direct conversion of synthesis gas to chemicals / Ernest du Toit

    OpenAIRE

    Du Toit, Ernest

    2002-01-01

    The catalytic conversion of synthesis gas, obtainable from the processing of coal, biomass or natural gas, to a complex hydrocarbon product stream can be achieved via the Fischer-Tropsch process. The Fischer-Tropsch synthesis process has evolved from being mainly a fuel producing process in the early 1950's to that of a solvent and speciality wax production process towards the end of the 1970's. From the early 1980's there has been a clear shift towards the production of commod...

  15. Implication of C-type natriuretic peptide-3 signaling in glycosaminoglycan synthesis and chondrocyte hypertrophy during TGF-β1 induced chondrogenic differentiation of chicken bone marrow-derived mesenchymal stem cells.

    Science.gov (United States)

    Kocamaz, Erdogan; Gok, Duygu; Cetinkaya, Ayse; Tufan, A Cevik

    2012-10-01

    This study investigated the involvement of CNP-3, chick homologue for human C-type natriuretic peptide (CNP), in TGF-β1 induced chondrogenic differentiation of chicken bone marrow-derived mesenchymal stem cells (MSCs). Chondrogenic differentiation of MSCs in pellet cultures was induced by TGF-β1. Chondrogenic differentiation and glycosaminoglycan synthesis were analyzed on the basis of basic histology, collagen type II expression, and Alcian blue staining. Antibodies against CNP and NPR-B were used to block their function during these processes. Results revealed that expression of CNP-3 and NPR-B in MSCs were regulated by TGF-β1 in monolayer cultures at mRNA level. In pellet cultures of MSCs, TGF-β1 successfully induced chondrogenic differentiation and glycosaminoglycan synthesis. Addition of CNP into the TGF-β1 supplemented chondrogenic differentiation medium further induced the glycosaminoglycan synthesis and hypertrophy of differentiated chondrocytes in these pellets. Pellets induced with TGF-β1 and treated with antibodies against CNP and NPR-B, did show collagen type II expression, however, Alcian blue staining showing glycosaminoglycan synthesis was significantly suppressed. In conclusion, CNP-3/NPR-B signaling may strongly be involved in synthesis of glycosaminoglycans of the chondrogenic matrix and hypertrophy of differentiated chondrocytes during TGF-β1 induced chondrogenic differentiation of MSCs.

  16. Synthesis of Three-dimensional Polymer Nanostructures via Chemical Vapor Deposition

    Science.gov (United States)

    Cheng, Kenneth

    Chemical vapor deposition (CVD) is a widely practiced methodology for preparing thin film polymer coatings, and the coatings can be applied to a broad range of materials, including three-dimensional solid structures and low-vapor pressure liquids. Reactive poly(p-xylylene) (PPX) coatings prepared by CVD can be used as a powerful tool for surface functionalization and bio-conjugation. The first portion of this dissertation serves to extend the use of CVD-based reactive PPX coatings as a surface functionalization strategy for the conjugation of biomolecules. Micro-structured PPX coatings having multiple surface reactive groups were fabricated. Multiple orthogonal click reactions were then employed to selectively immobilize galactose and mannobiose to the micro-structured polymer coatings. The presence of different types of carbohydrate enables lectins binding for examining ligands/cell receptor interactions. This dissertation also demonstrates the use of CVD-based reactive PPX coatings as intermediate layers to immobilize adenoviral vectors onto tissue scaffolds. The ability to tether adenoviral vectors on tissue scaffolds localizes the transduction near the scaffold surface and reduces acute toxicity and hepatic pathology cause by direct administration of the viral vector, providing a safe and efficient gene therapy delivery strategy. In the second portion of this dissertation, we explore the CVD of PPX onto surfaces coated with a thin layer of liquid crystal (LC). Instead of forming a conformal PPX coating encapsulating the LC layer, PPX assembled into an array of high-aspect ratio nanofibers inside the LC layer. The LC layer was demonstrated to act as a template where the anisotropic internal ordering of the LC facilitated the formation of nanofibers. The diameter of the nanofibers was in the range of 100 nm and could be tuned by type of LC template used, and the length of the nanofibers could be precisely controlled by varying the thickness of the LC film. The

  17. Bibliographic report on the synthesis, the chemical and physical properties and the applications of the TBP phosphate

    International Nuclear Information System (INIS)

    Azzouz, A.; Attou, M.

    1985-02-01

    This work consists of a bibliographic synthesis concerning the tri-n-butylphosphate (TBP) technology. It gathers briefly in 56 references on a table, the multiple applications of TBP such as extraction, spectroscopy and various other uses. Then, it deals with chemical instability different causes of this substance as well as its physical and chemical properties. In this way, for instance, the thermal degradation occurs well before the TBP boiling point. It comes out of this, several decomposition products such as the mono-n-butyl-phosphate (MBP), the di-n-butylphosphate (DBP) and some olefins. The acids and some impurities are known to have effects on TBP degradation. Later on, some processes of the TBP synthesis and their principles are stated. In the major cases, the POCl 3 process seems to be the best way, probably because of convenient efficiencies and moderate conditions of its making. Some purification processes according to the TBP use are also invoqued. In this case as well, Alcock et al. method is often stated in the literature. Moreover, five analysis methods corresponding to the most common situations are described

  18. Homogeneous ZnO nanostructure arrays on GaAs substrates by two-step chemical bath synthesis

    International Nuclear Information System (INIS)

    Huang, Chun-Yuan; Wu, Tzung-Han; Cheng, Chiao-Yang; Su, Yan-Kuin

    2012-01-01

    ZnO nanostructures, including nanowires, nanorods, and nanoneedles, have been deposited on GaAs substrates by the two-step chemical bath synthesis. It was demonstrated that the O 2 -plasma treatment of GaAs substrates prior to the sol–gel deposition of seed layers was essential to conformally grow the nanostructures instead of 2D ZnO bunches and grains on the seed layers. Via adjusting the growth time and concentration of precursors, nanostructures with different average diameter (26–225 nm), length (0.98–2.29 μm), and density (1.9–15.3 × 10 9 cm −2 ) can be obtained. To the best of our knowledge, this is the first demonstration of ZnO nanostructure arrays grown on GaAs substrates by the two-step chemical bath synthesis. As an anti-reflection layer on GaAs-based solar cells, the array of ZnO nanoneedles with an average diameter of 125 nm, a moderate length of 2.29 μm, and the distribution density of 9.8 × 10 9 cm −2 has increased the power conversion efficiency from 7.3 to 12.2 %, corresponding to a 67 % improvement.

  19. Total synthesis and structural validation of cyclodepsipeptides solonamide A and B

    DEFF Research Database (Denmark)

    Kitir, Betül; Baldry, Mara; Ingmer, Hanne

    2014-01-01

    , autoinducing peptide I (AIP-I). To enable more comprehensive studies, we embarked on the chemical synthesis of solonamides A and B. The key synthetic steps were formation of the (R)-β-hydroxy-fatty-acids by stereo-selective aldol reactions and a cyclative macrolactamization, which proceeded under highly dilute...

  20. Quantum Chemical and Experimental Studies on the Mechanism of Alkylation of β-Dicarbonyl Compounds. The Synthesis of Five and Six Membered Heterocyclic Spiro Derivatives

    Directory of Open Access Journals (Sweden)

    Ali Hüseyinli

    2004-11-01

    Full Text Available The alkylation of β-dicarbonyl compounds in a K2CO3/DMSO system wasfound to afford O- and C-alkylated derivatives, depending on the type of the β-dicarbonylcompound involved. The alkyl derivatives obtained were used in the synthesis of some newspiro barbituric acid derivatives. Quantum chemical calculations were carried out toelucidate the reaction mechanisms for some typical synthesis.

  1. Agro-waste as source of fine and industrial chemicals: synthesis of 2 ...

    African Journals Online (AJOL)

    This paper reports on the synthesis of 2-formyl-6-hydroxybenzoic acid (8) and 4 methoxyisobenzofuran-1,3-dione (10) from a renewable natural material Cashew Nut Shell Liquid (CNSL) achieved in five and seven steps, respectively. Anacardic acid was isolated from CNSL, dimethoxylated into (E)-methyl ...

  2. Chemically Modified Starch; Allyl- and Epoxy-Starch Derivatives: Their Synthesis and Characterization

    NARCIS (Netherlands)

    Franssen, M.C.R.; Boeriu, C.

    2014-01-01

    Both native and modified starches, such as starch that is pregelatinized, extruded, acid-converted, cross-linked, and substituted, are widely used in industry. This chapter describes a mild two-step process for the synthesis of novel, highly reactive granular epoxy-starch derivatives. Via this

  3. Understanding Microstructural Properties of Perovskite Ceramics through Their Wet-Chemical Synthesis

    NARCIS (Netherlands)

    Stawski, Tomasz

    2011-01-01

    This thesis comprises of seven full research chapters on the morphology, properties and processing of sol-gel precursor systems of barium titanate and lead zirconate titanate thin films and powders. In all the considered problems, the synthesis leading to nano-sized perovskite ceramics constitutes

  4. Novel synthetic approach to the prion protein: Kinetic study optimization of a native chemical ligation

    Czech Academy of Sciences Publication Activity Database

    Zawada, Zbigniew; Šebestík, Jaroslav; Bouř, Petr; Hlaváček, Jan; Stibor, Ivan

    2008-01-01

    Roč. 14, č. 8 (2008), s. 76-77 ISSN 1075-2617. [European Peptide Symposium /30./. 31.08.2008-05.09.2008, Helsinki] R&D Projects: GA ČR GA203/07/1517 Institutional research plan: CEZ:AV0Z40550506 Keywords : prion protein * neurodegenerative diseases * chemical synthesis * ligation conditions Subject RIV: CC - Organic Chemistry

  5. Nuclear DNA synthesis rate and labelling index: effects of carcinogenic and non-carcinogenic chemicals on its behaviour in the organism of growing CBA mice

    International Nuclear Information System (INIS)

    Amlacher, E.; Rudolph, C.

    1978-01-01

    Well known bioassays have been compared with the author's thymidine incorporation-screening system and other assays based on biochemical quantification of DNA synthesis as a possibility of identification of carcinogens. The partial inhibition of the whole DNA synthesis in a proliferating cell population after treatment with toxic and carcinogenic chemicals is an early common response especially in hepatectomized animal, livers caused by the effects of those substances. However, by quantitative evaluation of the nuclear DNA synthesis rate as a basic parameter, using autoradiographs of kidney and liver of juvenile growing CBA mice, it is possible to differentiate carcinogenic from non-carcinogenic chemicals by means of silver grain counting after 3 H-TdR incorporation. On the contrary, the whole DNA synthesis, expressed by the 3 H-labelling index (in per cent) of kidney and liver, did not permit such a differentiation in the experimental arrangement used. It could be demonstrated that carcinogenic compounds of different chemical classes partially inhibit the nuclear DNA synthesis rate significantly over a period of more than 24 hours. The tested non-carcinogenic compounds did not show this suppressive effect on the nuclear DNA synthesis rate. (author)

  6. Sensitivity to the two-peptide bacteriocin lactococcin G is dependent on UppP, an enzyme involved in cell-wall synthesis

    NARCIS (Netherlands)

    Kjos, Morten; Oppegård, Camilla; Diep, Dzung B; Nes, Ingolf F; Veening, Jan-Willem; Nissen-Meyer, Jon; Kristensen, Tom

    Most bacterially produced antimicrobial peptides (bacteriocins) are thought to kill target cells by a receptor-mediated mechanism. However, for most bacteriocins the receptor is unknown. For instance, no target receptor has been identified for the two-peptide bacteriocins (class IIb), whose activity

  7. Industrial Scale Synthesis of Carbon Nanotubes Via Fluidized Bed Chemical Vapor Deposition: A Senior Design Project

    Science.gov (United States)

    Smith, York R.; Fuchs, Alan; Meyyappan, M.

    2010-01-01

    Senior year chemical engineering students designed a process to produce 10 000 tonnes per annum of single wall carbon nanotubes (SWNT) and also conducted bench-top experiments to synthesize SWNTs via fluidized bed chemical vapor deposition techniques. This was an excellent pedagogical experience because it related to the type of real world design…

  8. The quantum chemical causality of pMHC-TCR biological avidity: Peptide atomic coordination data and the electronic state of agonist N termini

    Directory of Open Access Journals (Sweden)

    Georgios S.E. Antipas

    2015-06-01

    Full Text Available The quantum state of functional avidity of the synapse formed between a peptide-Major Histocompatibility Complex (pMHC and a T cell receptor (TCR is a subject not previously touched upon. Here we present atomic pair correlation meta-data based on crystalized tertiary structures of the Tax (HTLV-1 peptide along with three artificially altered variants, all of which were presented by the (Class I HLA-A201 protein in complexation with the human (CD8+ A6TCR. The meta-data reveal the existence of a direct relationship between pMHC-TCR functional avidity (agonist/antagonist and peptide pair distribution function (PDF. In this context, antagonist peptides are consistently under-coordinated in respect to Tax. Moreover, Density Functional Theory (DFT datasets in the BLYP/TZ2P level of theory resulting from relaxation of the H species on peptide tertiary structures reveal that the coordination requirement of agonist peptides is also expressed as a physical observable of the protonation state of their N termini: agonistic peptides are always found to retain a stable ammonium (NH3+ terminal group while antagonist peptides are not.

  9. Antimicrobial Peptides: A Promising Therapeutic Strategy in Tackling Antimicrobial Resistance.

    Science.gov (United States)

    Nuti, Ramya; Goud, Nerella S; Saraswati, A Prasanth; Alvala, Ravi; Alvala, Mallika

    2017-01-01

    Antimicrobial resistance (AMR) has posed a serious threat to global public health and it requires immediate action, preferably long term. Current drug therapies have failed to curb this menace due to the ability of microbes to circumvent the mechanisms through which the drugs act. From the drug discovery point of view, the majority of drugs currently employed for antimicrobial therapy are small molecules. Recent trends reveal a surge in the use of peptides as drug candidates as they offer remarkable advantages over small molecules. Newer synthetic strategies like organometalic complexes, Peptide-polymer conjugates, solid phase, liquid phase and recombinant DNA technology encouraging the use of peptides as therapeutic agents with a host of chemical functions, and tailored for specific applications. In the last decade, many peptide based drugs have been successfully approved by the Food and Drug Administration (FDA). This success can be attributed to their high specificity, selectivity and efficacy, high penetrability into the tissues, less immunogenicity and less tissue accumulation. Considering the enormity of AMR, the use of Antimicrobial Peptides (AMPs) can be a viable alternative to current therapeutics strategies. AMPs are naturally abundant allowing synthetic chemists to develop semi-synthetics peptide molecules. AMPs have a broad spectrum of activity towards microbes and they possess the ability to bypass the resistance induction mechanisms of microbes. The present review focuses on the potential applications of AMPs against various microbial disorders and their future prospects. Several resistance mechanisms and their strategies have also been discussed to highlight the importance in the current scenario. Breakthroughs in AMP designing, peptide synthesis and biotechnology have shown promise in tackling this challenge and has revived the interest of using AMPs as an important weapon in fighting AMR. Copyright© Bentham Science Publishers; For any queries

  10. Structural organization and spectroscopy of peptide-actinide(IV) complexes

    International Nuclear Information System (INIS)

    Dahou, S.

    2010-01-01

    The contamination of living organisms by actinide elements is at the origin of both radiological and chemical toxicity that may lead to severe dysfunction. Most of the data available on the actinide interaction with biological systems are macroscopic physiological measurements and are lacking a molecular description of the systems. Because of the intricacy of these systems, classical biochemical methods are difficult to implement. Our strategy consisted in designing simplified biomimetic peptides, and describing the corresponding intramolecular interactions with actinides. A carboxylic pentapeptide of the form DDPDD has been at the starting point of this work in order to further assess the influence of the peptide sequence on the topology of the complexes.To do so, various linear (Asp/Ala permutations, peptoids) and cyclic analogues have been synthesized. Furthermore, in order to include the hydroxamic function (with a high affinity for Fe(III)) in the peptide, both desferrioxamine and acetohydroxamic acid have been investigated. However because of difficulties in synthesis, we have not been able to test these peptides. Three actinide cations have been considered at oxidation state +IV (Th, Np, Pu) and compared to Fe(III), often considered as a biological surrogate of Pu(IV). The spatial arrangement of the peptide around the cation has been probed by spectrophotometry and X-ray Absorption Spectroscopy. The spectroscopic data and EXAFS data adjustment lead us to rationalize the topology of the complexes as a function of the peptide sequence: mix hydroxy polynuclear species for linear and cyclic peptides, mononuclear for the desferrioxamine complexes. Furthermore, significant differences have appeared between Fe(III) and actinide(IV), related to differences of reactivity in aqueous medium. (author)

  11. On the chemical synthesis route to bulk-scale skutterudite materials

    DEFF Research Database (Denmark)

    Tafti, Mohsen Y.; Saleemi, Mohsin; Han, Li

    2016-01-01

    In this article an alternative high yield route for the synthesis of CoSb3-based unfilled skutterudites is presented. Using low-melting temperature salts of the constituents, melting and mixing them homogeneously in a hydrophobic liquid with postprocessing of the powders we achieve a more intimat......, compaction of the powders with SPS technique provided a safe route to maintaining the nanopowder size and achieving low thermal conductivity (3 W/mK). The proposed method can easily be scaled up and adopted by the industry.......In this article an alternative high yield route for the synthesis of CoSb3-based unfilled skutterudites is presented. Using low-melting temperature salts of the constituents, melting and mixing them homogeneously in a hydrophobic liquid with postprocessing of the powders we achieve a more...

  12. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, Vasile; Chiper, Diana

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three preparation methods of deuterized chloroform are presented. In the first method the direct chlorination of methane (CH 4 + 3Cl 2 ) in the presence of light and in an oxygen-free atmosphere results in CHCl 3 + 3HCl. The method's drawback is that the resulting product is impure, being obtained also secondary chlorinated compounds, such as CHCl, CH 2 Cl 2 and CCl 4 . The second method consists in chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in the presence of chlorinated lime. This method makes use of decarbolyzing of trichlor acetate acid (as a sodium salt), what results in CL 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis, since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water of 99.87% purity, according to the following reaction: Cl 3 C-COONa → (D 2 O) → Cl 2 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products, which could entail additional purifications (distillations, rectification, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid to liquid separating funnel. After separation, deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out by nuclear magnetic resonance spectrometry. (authors)

  13. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, V.; Olteanu-Chiper, D.

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three methods for obtaining deuterized chloroform are presented. 1. The direct chlorination of methane, in presence of light and in oxygen-free atmosphere: CH 4 + 3 Cl 2 + ℎν→ CHCl 3 + 3 HCl. The method's drawback is that the product obtained is impure, as other chlorinated compounds such as CH 3 Cl, CH 2 Cl 2 , CCl 4 also result. 2. Chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in presence of chlorinated lime: CH 3 CHO (Cl 2 /HO - )/(-HCl)Cl 3 C-CHO (CaCl 2 /HOH)/(-(HCOO) 2 Ca) CHCl 3 and CH 3 -CO-CH 3 (Cl 2 /HO)/(-HCl) Cl 3 C-CO-CH 3 (NaOH)/(-CH 3 COONa) CHCl 3 . 3. Decarboxylizing of trichloroacetate acid (as sodium salt): Cl 3 C-COONa (t deg C)/(H 2 O) Cl 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water 99,87% purity, according to the following reaction: Cl 3 C-COONa (t deg C)/(D 2 O) Cl 3 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products which could entail additional purifications (distillations, rectifications, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid-to-liquid separating funnel. After separation, the deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out through Nuclear Magnetic Resonance Spectrometry. (authors)

  14. Chemical changes in non-reduced catalysts used for ammonia synthesis

    International Nuclear Information System (INIS)

    Peev, T.M.; Kyrova, Z.; Bojinova, A.I.

    1980-01-01

    Samples of non-reduced industrial catalysts CA-1 for ammonia synthesis were studied by using Moessbauer spectroscopy. The conditions of the normal storing of this catalyst were changed. After 6 months it was found that under the influence of moisture and air oxygen a considerable part of the magnetite was converted to α-Fe 2 O 3 , α-FeOOH and γ-FeOOH. (author)

  15. The assembly and use of continuous flow systems for chemical synthesis.

    Science.gov (United States)

    Britton, Joshua; Jamison, Timothy F

    2017-11-01

    The adoption of and opportunities in continuous flow synthesis ('flow chemistry') have increased significantly over the past several years. Continuous flow systems provide improved reaction safety and accelerated reaction kinetics, and have synthesised several active pharmaceutical ingredients in automated reconfigurable systems. Although continuous flow platforms are commercially available, systems constructed 'in-lab' provide researchers with a flexible, versatile, and cost-effective alternative. Herein, we describe the assembly and use of a modular continuous flow apparatus from readily available and affordable parts in as little as 30 min. Once assembled, the synthesis of a sulfonamide by reacting 4-chlorobenzenesulfonyl chloride with dibenzylamine in a single reactor coil with an in-line quench is presented. This example reaction offers the opportunity to learn several important skills including reactor construction, charging of a back-pressure regulator, assembly of stainless-steel syringes, assembly of a continuous flow system with multiple junctions, and yield determination. From our extensive experience of single-step and multistep continuous flow synthesis, we also describe solutions to commonly encountered technical problems such as precipitation of solids ('clogging') and reactor failure. Following this protocol, a nonspecialist can assemble a continuous flow system from reactor coils, syringes, pumps, in-line liquid-liquid separators, drying columns, back-pressure regulators, static mixers, and packed-bed reactors.

  16. Rational design and synthesis of altered peptide ligands based on human myelin oligodendrocyte glycoprotein 35-55 epitope: inhibition of chronic experimental autoimmune encephalomyelitis in mice.

    Science.gov (United States)

    Tselios, Theodore; Aggelidakis, Mihalis; Tapeinou, Anthi; Tseveleki, Vivian; Kanistras, Ioannis; Gatos, Dimitrios; Matsoukas, John

    2014-11-04

    Experimental autoimmune encephalomyelitis (EAE) is a demyelinating disease of the central nervous system and is an animal model of multiple sclerosis (MS). Although the etiology of MS remains unclear, there is evidence T-cell recognition of immunodominant epitopes of myelin proteins, such as the 35-55 epitope of myelin oligodendrocyte glycoprotein (MOG), plays a pathogenic role in the induction of chronic EAE. Cyclization of peptides is of great interest since the limited stability of linear peptides restricts their potential use as therapeutic agents. Herein, we have designed and synthesized a number of linear and cyclic peptides by mutating crucial T cell receptor (TCR) contact residues of the human MOG35-55 epitope. In particular, we have designed and synthesized cyclic altered peptide ligands (APLs) by mutating Arg41 with Ala or Arg41 and Arg46 with Ala. The peptides were synthesized in solid phase on 2-chlorotrityl chloride resin (CLTR-Cl) using the Fmoc/t-Bu methodology. The purity of final products was verified by RP-HPLC and their identification was achieved by ESI-MS. It was found that the substitutions of Arg at positions 41 and 46 with Ala results in peptide analogues that reduce the severity of MOG-induced EAE clinical symptoms in C57BL/6 mice when co-administered with mouse MOG35-55 peptide at the time of immunization.

  17. Novel peptide-based protease inhibitors

    DEFF Research Database (Denmark)

    Roodbeen, Renée

    of novel peptide-based protease inhibitors, efforts were made towards improved methods for peptide synthesis. The coupling of Fmoc-amino acids onto N-methylated peptidyl resins was investigated. These couplings can be low yielding and the effect of the use of microwave heating combined with the coupling...

  18. δ-Peptides from RuAAC-Derived 1,5-Disubstituted Triazole Units

    KAUST Repository

    Johansson, Johan R.

    2014-02-14

    Non-natural peptides with structures and functions similar to natural peptides have emerged lately in biomedical as well as nanotechnological contexts. They are interesting for pharmaceutical applications since they can adopt structures with new targeting potentials and because they are generally not prone to degradation by proteases. We report here a new set of peptidomimetics derived from δ-peptides, consisting of n units of a 1,5-disubstituted 1,2,3-triazole amino acid (5Tzl). The monomer was prepared using ruthenium-catalyzed azide-alkyne cycloaddition (RuAAC) chemistry using [RuCl2Cp]x as the catalyst, allowing for simpler purification and resulting in excellent yields. This achiral monomer was used to prepare peptide oligomers that are water soluble independent of peptide chain length. Conformational analysis and structural investigations of the oligomers were performed by 2D NOESY NMR experiments, and by quantum chemical calculations using the ωB97X-D functional. These data indicate that several conformations may co-exist with slight energetic differences. Together with their increased hydrophilicity, this feature of homo-5Tzl may prove essential for mimicking natural peptides composed of α-amino acids, where the various secondary structures are achieved by side chain effects and not by the rigidity of the peptide backbone. The improved synthetic method allows for facile variation of the 5Tzl amino acid side chains, further increasing the versatility of these compounds. A new set of non-natural peptides composed of 1,5-disubstituted 1,2,3-triazole amino acids is presented. These peptides benefit from: a) modular synthesis of the monomers, allowing variation of the side chains; b) increased solubility of the oligomers in water, irrespective of peptide length; c) flexibility of the backbone allowing these foldamers to adopt several conformations. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Engineering cell factories for producing building block chemicals for bio-polymer synthesis

    OpenAIRE

    Tsuge, Yota; Kawaguchi, Hideo; Sasaki, Kengo; Kondo, Akihiko

    2016-01-01

    Synthetic polymers are widely used in daily life. Due to increasing environmental concerns related to global warming and the depletion of oil reserves, the development of microbial-based fermentation processes for the production of polymer building block chemicals from renewable resources is desirable to replace current petroleum-based methods. To this end, strains that efficiently produce the target chemicals at high yields and productivity are needed. Recent advances in metabolic engineerin...

  20. Purposeful synthesis of chemical elements and ecologically pure mobile sources of energy

    International Nuclear Information System (INIS)

    Krivitsky, V. A.; Gareev, F. A.

    2007-01-01

    It is well known [1] that the natural geo-transmutation of chemical elements occurs in the atmosphere and earth in the regions of a strong change in geo-, bio-, acoustic-, and electromagnetic fields. The mineral row materials contain the same accompanying chemical combinations which are independent of mineral deposit [2]. This means that the formation of chemical elements occurs in the same physical and chemical conditions. These conditions were simulated on the fundamental cooperative resonance synchronization principle [1]. The experimental facility was constructed on the basis of our model which provided with the calculated final chemical elements. These experimental results indicate new possibilities for, simulating, inducing and controlling nuclear reactions by low energy external fields. The borrowing from the geo-transmutation mechanisms of chemical elements creates the fundamental directions in low energy nuclear reaction researches for construction of new ecologically pure mobile sources of energy independent of oil, gas and coal, new substances, and technologies. References [1] F.A. Gareev, I.E. Zhidkova, E-print arXiv Nucl-th/0610002 2006. [2] V.A. Krivzskii, Transmutazija ximicheskix elementov v evolyuzii Semli (in Russian), Moscow 2003

  1. From Mollusks to Medicine: A Venomics Approach for the Discovery and Characterization of Therapeutics from Terebridae Peptide Toxins

    Directory of Open Access Journals (Sweden)

    Aida Verdes

    2016-04-01

    Full Text Available Animal venoms comprise a diversity of peptide toxins that manipulate molecular targets such as ion channels and receptors, making venom peptides attractive candidates for the development of therapeutics to benefit human health. However, identifying bioactive venom peptides remains a significant challenge. In this review we describe our particular venomics strategy for the discovery, characterization, and optimization of Terebridae venom peptides, teretoxins. Our strategy reflects the scientific path from mollusks to medicine in an integrative sequential approach with the following steps: (1 delimitation of venomous Terebridae lineages through taxonomic and phylogenetic analyses; (2 identification and classification of putative teretoxins through omics methodologies, including genomics, transcriptomics, and proteomics; (3 chemical and recombinant synthesis of promising peptide toxins; (4 structural characterization through experimental and computational methods; (5 determination of teretoxin bioactivity and molecular function through biological assays and computational modeling; (6 optimization of peptide toxin affinity and selectivity to molecular target; and (7 development of strategies for effective delivery of venom peptide therapeutics. While our research focuses on terebrids, the venomics approach outlined here can be applied to the discovery and characterization of peptide toxins from any venomous taxa.

  2. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Yongzhong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Chen, Jian, E-mail: wuhangzs@163.com [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Fu, Qingshan [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Li, Binghong [China Rubber Group Carbon Black Industry Research and Design Institute, 643000 Zigong, Sichuan (China); Zhang, Huazhi; Gong, Yong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China)

    2015-01-01

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C{sub 4}H{sub 4}CuO{sub 6} → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

  3. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    International Nuclear Information System (INIS)

    Jin, Yongzhong; Chen, Jian; Fu, Qingshan; Li, Binghong; Zhang, Huazhi; Gong, Yong

    2015-01-01

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C 4 H 4 CuO 6 → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system

  4. Synthesis, three-dimensional structure, conformation and correct chemical shift assignment determination of pharmaceutical molecules by NMR and molecular modeling

    Energy Technology Data Exchange (ETDEWEB)

    Azeredo, Sirlene O.F. de; Sales, Edijane M.; Figueroa-Villar, José D., E-mail: jdfv2009@gmail.com [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Grupo de Ressonância Magnética Nuclear e Química Medicinal

    2017-07-01

    This work includes the synthesis of phenanthrenequinone guanylhydrazone and phenanthro[9,10-e][1,2,4]triazin-3-amine to be tested as intercalate with DNA for treatment of cancer. The other synthesized product, 2-[(4-chlorophenylamino)methylene]malononitrile, was designed for future determination of its activity against leishmaniasis. A common problem about some articles on the literature is that some previously published compounds display error of their molecular structures. In this article it is shown the application of several procedures of nuclear magnetic resonance (NMR) to determine the complete molecular structure and the non questionable chemical shift assignment of the synthesized compounds, and also their analysis by molecular modeling to confirm the NMR results. To determine the capacity of pharmacological compounds to interact with biological targets is determined by docking. This work is to motivate the application of NMR and molecular modeling on organic synthesis, being a process that is very important for the study of the prepared compounds as interactions with biological targets by NMR. (author)

  5. Synthesis, three-dimensional structure, conformation and correct chemical shift assignment determination of pharmaceutical molecules by NMR and molecular modeling

    International Nuclear Information System (INIS)

    Azeredo, Sirlene O.F. de; Sales, Edijane M.; Figueroa-Villar, José D.

    2017-01-01

    This work includes the synthesis of phenanthrenequinone guanylhydrazone and phenanthro[9,10-e][1,2,4]triazin-3-amine to be tested as intercalate with DNA for treatment of cancer. The other synthesized product, 2-[(4-chlorophenylamino)methylene]malononitrile, was designed for future determination of its activity against leishmaniasis. A common problem about some articles on the literature is that some previously published compounds display error of their molecular structures. In this article it is shown the application of several procedures of nuclear magnetic resonance (NMR) to determine the complete molecular structure and the non questionable chemical shift assignment of the synthesized compounds, and also their analysis by molecular modeling to confirm the NMR results. To determine the capacity of pharmacological compounds to interact with biological targets is determined by docking. This work is to motivate the application of NMR and molecular modeling on organic synthesis, being a process that is very important for the study of the prepared compounds as interactions with biological targets by NMR. (author)

  6. Chemical and electrochemical synthesis of nano-sized TiO{sub 2} anatase for large-area photon conversion

    Energy Technology Data Exchange (ETDEWEB)

    Babasaheb, Raghunath Sankapal; Shrikrishna, Dattatraya Sartale; Lux-Steiner, M.Ch.; Ennaoui, A. [Hahn-Meitner-Institut, Div. of Solar Energy Research, Berlin (Germany)

    2006-05-15

    We report on the synthesis of nanocrystalline titanium dioxide thin films and powders by chemical and electrochemical deposition methods. Both methods are simple, inexpensive and suitable for large-scale production. Air-annealing of the films and powders at T = 500 C leads to densely packed nanometer sized anatase TiO{sub 2} particles. The obtained layers are characterized by different methods such as: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Titanium dioxide TiO{sub 2} (anatase) phase with (101) preferred orientation has been obtained for the films deposited on glass; indium doped tin oxide (ITO) and quartz substrates. The powder obtained as the byproduct consists of TiO{sub 2} with anatase-phase as well. (authors)

  7. Chemical and electrochemical synthesis of nano-sized TiO2 anatase for large-area photon conversion

    International Nuclear Information System (INIS)

    Babasaheb, Raghunath Sankapal; Shrikrishna, Dattatraya Sartale; Lux-Steiner, M.Ch.; Ennaoui, A.

    2006-01-01

    We report on the synthesis of nanocrystalline titanium dioxide thin films and powders by chemical and electrochemical deposition methods. Both methods are simple, inexpensive and suitable for large-scale production. Air-annealing of the films and powders at T = 500 C leads to densely packed nanometer sized anatase TiO 2 particles. The obtained layers are characterized by different methods such as: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Titanium dioxide TiO 2 (anatase) phase with (101) preferred orientation has been obtained for the films deposited on glass; indium doped tin oxide (ITO) and quartz substrates. The powder obtained as the byproduct consists of TiO 2 with anatase-phase as well. (authors)

  8. Synthesis, physico-chemical properties and complexing abilities of new amphiphilic ligands from D-galacturonic acid.

    Science.gov (United States)

    Allam, Anas; Behr, Jean-Bernard; Dupont, Laurent; Nardello-Rataj, Véronique; Plantier-Royon, Richard

    2010-04-19

    This paper describes a convenient and efficient synthesis of new complexing surfactants from d-galacturonic acid and n-octanol as renewable raw materials in a two-step sequence. In the first step, simultaneous O-glycosidation-esterification under Fischer conditions was achieved. The anomeric ratio of the products was studied based on the main experimental parameters and the activation mode (thermal or microwave). In the second step, aminolysis of the n-octyl ester was achieved with various functionalized primary amines under standard thermal or microwave activation. The physico-chemical properties of these new amphiphilic ligands were measured and these compounds were found to exhibit interesting surface properties. Complexing abilities of one uronamide ligand functionalized with a pyridine moiety toward Cu(II) ions was investigated in solution by EPR titrations. A solid compound was also synthesized and characterized, its relative structure was deduced from spectroscopic data. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

  9. Synthesis of poly(D,L-lactide-co-glycolide) copolymers and its chemical characterization by NMR and FTIR

    International Nuclear Information System (INIS)

    Erbetta, Cynthia D.C.; Viegas, Carla C.B.; Freitas, Roberto F.S.; Sousa, Ricardo G.

    2011-01-01

    Poly(D,L-lactide-co-glycolide) copolymer is of great interest for medical applications. This interest is justified by the fact that it is bioreabsorbable, biocompatible and non-toxic, while its degradation kinetics can be modified by the copolymerization ratio of the monomers. In this study, copolymers were synthesized at 175 deg C by opening the rings of the cyclic dimers of the D,L-lactide and glycolide monomers in the presence of stannous octoate initiator and lauryl alcohol co-initiator. The efficient application of a vacuum to the reaction medium, coupled with adequate stirring, is fundamental for the success of the synthesis. The following analysis techniques were used to characterize the synthesized copolymers: Nuclear Magnetic Resonance Spectroscopy (NMR) and Fourier Transform Infrared Spectroscopy (FTIR). The chemical composition and the ratio of the monomers in the synthesized copolymer were determined. (author)

  10. Post-synthesis amine borane functionalization of metal-organic framework and its unusual chemical hydrogen release phenomenon

    KAUST Repository

    Berke, Heinz

    2017-05-11

    We report a novel strategy for post-synthesis amine borane functionalization of MOFs under gas-solid phase transformation utilizing gaseous diborane. The covalently confined amine borane derivative decorated on the framework backbone is stable when preserved at low temperature, but spontaneously liberates soft chemical hydrogen at room temperature leading to the development of an unusual borenium type species (-NH=BH2+) ion-paired with hydroborate anion. Furthermore, the unsaturated amino borane (-NH=BH2) and the -iminodiborane ((--NHB2H5) were detected as final products. A combination of DFT based molecular dynamics simulations and solid state NMR spectroscopy, utilizing isotopically enriched materials, were undertaken to unequivocally elucidate the mechanistic pathways for H2 liberation.

  11. Synthesis of suspended carbon nanotubes on silicon inverse-opal structures by laser-assisted chemical vapour deposition

    International Nuclear Information System (INIS)

    Shi, J; Lu, Y F; Wang, H; Yi, K J; Lin, Y S; Zhang, R; Liou, S H

    2006-01-01

    Suspended single-walled carbon nanotubes (SWNTs) have been synthesized on Si inverse-opal structures by laser-assisted chemical vapour deposition (LCVD). A CW CO 2 laser at 10.6 μm was used to directly irradiate the substrates during the LCVD process. At a laser power density of 14.3 MW m -2 , suspended SWNT networks were found predominantly rooted at the sharp edges in the Si inverse-opal structures. Raman spectroscopy indicated that the SWNT networks were composed of high-quality defect-free SWNTs with an average diameter of 1.3 nm. At a lower laser power density (6.4 MW m -2 ), multi-walled carbon nanotubes (MWNTs) were grown on the entire surface of the substrates. The preference for the synthesis of SWNTs or MWNTs was attributed to the difference in the catalyst sizes as well as the growth temperature in the LCVD process

  12. Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

    Science.gov (United States)

    Gao, Huiying; Li, Zhiyong; Zhao, Peng

    2018-03-01

    Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

  13. Chemical synthesis of composite HML / PDMcT / PAni and its application as the trhiodan adsorbent in aqueous solutions

    International Nuclear Information System (INIS)

    Girotto, L.G.; Pacheco, I.; Freitas, L.L. de; Oliveira, R.S.; Amaral, F.A. do; Canobre, S.C.

    2016-01-01

    The mixed hydroxide lamellar [Co -Al- Cl] was synthesize by the co- precipitation method constant pH 8. The synthesis composite HML/PDMcT/PAni was carried out via chemical. The DRX composite HML/PDMcT/PAni showed that one amorphicity in the conductor polymer doesn't hid the diffraction peaks characteristic of HML. The MEV micrographs of composite HDL / PDMcT / PAni showed a large number of crystallites compacts with several shapes characteristic to PDMcT and nanofibers of polyaniline indicating an association between the different constituents forming the composite. The results of the adsorption was 98% of the pesticide in the composite HML / PDMcT / PAni , the composite can contribute so significantly to one Thiodon withdrawal in contaminated pesticide waters. (author)

  14. 1,5-Anhydro-D-Fructose – Efficient Synthesis and Chemical Uses

    DEFF Research Database (Denmark)

    Lundt, Inge; Dekany, Gyula; Stütz, Arnold E.

    as well as for derivatives and analogues thereof. The potential of AF will be highlighted as will be the use of AF as a chiral building block for the preparation of other interesting compounds with biological activities such as, for example, Deoxymannojirimycin (DMJ). [1] S.M. Andersen, I. Lundt, J......1,5-Anhydro-D-fructose (AF) is a valuable chiral building block for organic synthesis.[1] However, the antioxidant and antimicrobial properties of AF are equally important.[1] Due to these interesting properties AF is heavily patented for the use in pharmaceuticals, foods and cosmetics. However...

  15. Design and synthesis of a new peptide derived from Fasciola gigantica cathepsin L1 with potential application in serodiagnosis of fascioliasis.

    Science.gov (United States)

    Meshgi, Behnam; Jalousian, Fatemeh; Fathi, Saeid; Jahani, Zahra

    2018-06-01

    Fascioliasis is a global parasitic disease that affects domestic animals and causes considerable economic losses in the process of domestic animal breeding in endemic regions. The cause of the disease involves a liver trematode of the genus Fasciola, which secretes materials into a host's body (mainly proteins) in order to protect it from the host's immune system. These materials can be involved in the migration, growth, and nutrition of the parasite. Among the expressive proteins of Fasciola, proteases have been introduced as the appropriate targets for diagnosis, treatment, and vaccination against parasites. Cathepsin L (CL) is a member of cysteine proteases; it is widely expressed in the Fasciola species. The aim of this study was to evaluate two synthetic peptides from F. gigantica CL1 for improving serological diagnosis of the Fasciola infection. Therefore, the potential diagnostic value of the surface epitopes of CL1 was assessed using ELISA. In the current study, bioinformatics tools were applied to select two appropriate epitopes of Fasciola Cathepsin L1 as synthetic antigens. Their diagnostic values were evaluated by two methods of indirect ELISA and dot blot analysis. The findings revealed that the first peptide at a dilution ratio of 1:400 and the second peptide at a dilution ratio of 1:100 had the best results and the best concentration of antigens was introduced at 4 μg/ml. Moreover, 191 sera samples were analyzed by both peptides by using the ELISA method, including fascioliasis sera, other parasitic sera and negative sera. The sensitivity of the peptides 1-ELISA and peptide 2-ELISA for the diagnosis of the various cases was 100%. The specificity of the first peptide was 87.3% and its efficacy was determined to be 93.65%. The specificity and the efficacy of the second peptide were 79% and 89.5%, respectively. The positive predictive values of the first and second peptides were obtained to be 86.27% and 79.27% respectively, and the negative

  16. A new approach to synthesis and application of novel classes of ligands for the affinity capture and characterisation of phosphorylated peptides

    OpenAIRE

    Agron, Mataj

    2017-01-01

    Mass spectrometry has emerged as the technique of choice for the detection of posttranslational modifications of proteins due to its capability in high-throughput, and high sensitive analyses of proteolytic ally derived peptides. The use of enrichment techniques in combination with mass spectrometry has led to the identification of numerous novel phosphorylated peptides from phosphorylated proteins from whole cell lysates. Despite recent advances in the field of mass spectro...

  17. Engineering cell factories for producing building block chemicals for bio-polymer synthesis.

    Science.gov (United States)

    Tsuge, Yota; Kawaguchi, Hideo; Sasaki, Kengo; Kondo, Akihiko

    2016-01-21

    Synthetic polymers are widely used in daily life. Due to increasing environmental concerns related to global warming and the depletion of oil reserves, the development of microbial-based fermentation processes for the production of polymer building block chemicals from renewable resources is desirable to replace current petroleum-based methods. To this end, strains that efficiently produce the target chemicals at high yields and productivity are needed. Recent advances in metabolic engineering have enabled the biosynthesis of polymer compounds at high yield and productivities by governing the carbon flux towards the target chemicals. Using these methods, microbial strains have been engineered to produce monomer chemicals for replacing traditional petroleum-derived aliphatic polymers. These developments also raise the possibility of microbial production of aromatic chemicals for synthesizing high-performance polymers with desirable properties, such as ultraviolet absorbance, high thermal resistance, and mechanical strength. In the present review, we summarize recent progress in metabolic engineering approaches to optimize microbial strains for producing building blocks to synthesize aliphatic and high-performance aromatic polymers.

  18. CHEMICALS

    CERN Multimedia

    Medical Service

    2002-01-01

    It is reminded that all persons who use chemicals must inform CERN's Chemistry Service (TIS-GS-GC) and the CERN Medical Service (TIS-ME). Information concerning their toxicity or other hazards as well as the necessary individual and collective protection measures will be provided by these two services. Users must be in possession of a material safety data sheet (MSDS) for each chemical used. These can be obtained by one of several means : the manufacturer of the chemical (legally obliged to supply an MSDS for each chemical delivered) ; CERN's Chemistry Service of the General Safety Group of TIS ; for chemicals and gases available in the CERN Stores the MSDS has been made available via EDH either in pdf format or else via a link to the supplier's web site. Training courses in chemical safety are available for registration via HR-TD. CERN Medical Service : TIS-ME :73186 or service.medical@cern.ch Chemistry Service : TIS-GS-GC : 78546

  19. A general strategy for synthesis of cyclophane-braced peptide macrocycles via palladium-catalysed intramolecular sp3 C-H arylation

    Science.gov (United States)

    Zhang, Xuekai; Lu, Gang; Sun, Meng; Mahankali, Madhu; Ma, Yanfei; Zhang, Mingming; Hua, Wangde; Hu, Yuting; Wang, Qingbing; Chen, Jinghuo; He, Gang; Qi, Xiangbing; Shen, Weijun; Liu, Peng; Chen, Gong

    2018-05-01

    New methods capable of effecting cyclization, and forming novel three-dimensional structures while maintaining favourable physicochemical properties are needed to facilitate the development of cyclic peptide-based drugs that can engage challenging biological targets, such as protein-protein interactions. Here, we report a highly efficient and generally applicable strategy for constructing new types of peptide macrocycles using palladium-catalysed intramolecular C(sp3)-H arylation reactions. Easily accessible linear peptide precursors of simple and versatile design can be selectively cyclized at the side chains of either aromatic or modified non-aromatic amino acid units to form various cyclophane-braced peptide cycles. This strategy provides a powerful tool to address the long-standing challenge of size- and composition-dependence in peptide macrocyclization, and generates novel peptide macrocycles with uniquely buttressed backbones and distinct loop-type three-dimensional structures. Preliminary cell proliferation screening of the pilot library revealed a potent lead compound with selective cytotoxicity toward proliferative Myc-dependent cancer cell lines.

  20. Magnesium carbide synthesis from methane and magnesium oxide - a potential methodology for natural gas conversion to premium fuels and chemicals

    Energy Technology Data Exchange (ETDEWEB)

    Diaz, A.F.; Modestino, A.J.; Howard, J.B. [Massachusetts Institute of Technology, Cambridge, MA (United States)] [and others

    1995-12-31

    Diversification of the raw materials base for manufacturing premium fuels and chemicals offers U.S. and international consumers economic and strategic benefits. Extensive reserves of natural gas in the world provide a valuable source of clean gaseous fuel and chemical feedstock. Assuming the availability of suitable conversion processes, natural gas offers the prospect of improving flexibility in liquid fuels and chemicals manufacture, and thus, the opportunity to complement, supplement, or displace petroleum-based production as economic and strategic considerations require. The composition of natural gas varies from reservoir to reservoir but the principal hydrocarbon constituent is always methane (CH{sub 4}). With its high hydrogen-to-carbon ratio, methane has the potential to produce hydrogen or hydrogen-rich products. However, methane is a very chemically stable molecule and, thus, is not readily transformed to other molecules or easily reformed to its elements (H{sub 2} and carbon). In many cases, further research is needed to augment selectivity to desired product(s), increase single-pass conversions, or improve economics (e.g. there have been estimates of $50/bbl or more for liquid products) before the full potential of these methodologies can be realized on a commercial scale. With the trade-off between gas conversion and product selectivity, a major challenge common to many of these technologies is to simultaneously achieve high methane single-pass conversions and high selectivity to desired products. Based on the results of the scoping runs, there appears to be strong indications that a breakthrough has finally been achieved in that synthesis of magnesium carbides from MgO and methane in the arc discharge reactor has been demonstrated.