Preparation, Characterization and Hemostatic Properties of Chitosan Caffeates

2019 ◽  
Vol 814 ◽  
pp. 365-371
Author(s):  
Si Tong Lu ◽  
Dong Ying Zhang ◽  
Zhang Hu ◽  
Si Dong Li ◽  
Pu Wang Li
Keyword(s):  
Caffeic Acid ◽  
Freeze Drying ◽  
Water Solubility ◽  
Crystal Form ◽  
Positive Control ◽  
Mass Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Yunnan Baiyao ◽  
Better Than

In this paper, chitosan and caffeic acid were used as starting materials to prepare chitosan caffeates by reflux-heating and freeze-drying. The structures of chitosan caffeates were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and potentiometric titration. At the same time, the physical properties of chitosan caffeates were tested and the hemostatic properties were evaluated. The results showed that four chitosan caffeates with different mass ratios of chitosan and caffeic acid (1:1, 1:2, 1:4, 1:6) had been successfully prepared, which enhanced the water solubility. FTIR analysis demonstrated that caffeic acid had been successfully grafted onto chitosan chains. XRD showed that the crystal form of chitosan changed to some extent and the chain had some regularity in some directions, but its crystallinity reduced. Chitosan caffeates, particularly mass ratio of 1:1, showed excellent hemostatic properties and even better than chitosan and the positive control (Yunnan Baiyao), which were expected to be developed as an effective biomaterial for hemostasis.

scholarly journals Identification, Optimization and Preliminary X-ray Diffraction of a New Crystal Form of the N-terminal Domain of the HIV-1 CA Protein

2007 ◽  
Vol 6 (1) ◽  
Author(s):  
Ryan Van Woerkom ◽  
Andrew Dixon ◽  
Rob Oslund ◽  
Bruce Howard
Keyword(s):  
Crystal Form ◽  
X Ray Diffraction ◽  
X Ray ◽  
Terminal Domain ◽  
Single Protein ◽  
Intersubunit Interactions ◽  
Optimized Conditions ◽  
Mature Virus ◽  
Hiv 1 ◽  
Better Than

In an effort to better understand the detailed intersubunit interactions of the N-terminal Domain of the CA (capsid) protein from HIV-1 within the conical core of the mature virus, we have identified a novel crystal form of this domain and have optimized conditions to grow single protein crystals suitable for x-ray analysis. These high quality crystals diffract to better than 1.8 Å resolution on a rotating anode generator.

Preparation of partially end-capped amino-terminated hyperbranched polymer and dyeing properties enhancement to polyurethane membrane

2017 ◽  
Vol 88 (20) ◽  
pp. 2319-2328
Author(s):  
Longfang Ren ◽  
Jin Geng ◽  
Na Wang ◽  
Zidong Guo
Keyword(s):  
Water Solubility ◽  
Raw Materials ◽  
Mass Ratio ◽  
Drying Method ◽  
X Ray Diffraction ◽  
Hydrogen Bond Interaction ◽  
Dyeing Properties ◽  
X Ray ◽  
Blend Membranes ◽  
Polyurethane Membrane

In this study, a series of products with different water solubility, which were named as partial end-capped amino-terminated hyperbranched polymers (HBPs) 1–6, were obtained by changing the mass ratio of raw materials. The structure was characterized by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR). The polyurethane was respectively mixed with partial end-capped amino-terminated HBPs to prepare different blend membranes by the drying method. The results showed that the water solubility of partial end-capped amino-terminated HBPs had obvious effects on the dyeing properties of blend membranes. When the mass ratio of amino-terminated HBP and single-blocked isophorone diisocyanate was 3:2, the performance of prepared partial end-capped amino-terminated HBP 4 was the best. The structures of blend membranes were characterized by FTIR spectroscopy, X-ray diffraction and scanning electron microscopy (SEM). When the mass fraction of partial end-capped amino-terminated HBP 4 was 2%, dye uptake improved from 12% to 85%. The dry-rub fastness and wet-rub fastness reached 4.5 and 3, respectively. The K/S values indicated that the surface chroma also deepened. The results indicated that partial end-capped amino-terminated HBP and polyurethane had hydrogen-bond interaction and certain phase separation.

scholarly journals Born out of Fire and Ice: Polymorph Studies of the Antiviral Famciclovir

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Variable Temperature ◽  
Chemical Properties ◽  
Crystal Form ◽  
X Ray Diffraction ◽  
Crystal Forms ◽  
X Ray ◽  
Physical Chemical ◽  
Diffraction Patterns ◽  
Crystalline Forms

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.

Influence of High Current Pulsed Electron Beam Irradiation on Ni-P Electroless Plating

2011 ◽  
Vol 299-300 ◽  
pp. 77-81
Author(s):  
Yang Xu ◽  
Sheng Zhi Hao ◽  
Xiang Dong Zhang ◽  
Min Cai Li ◽  
Chuang Dong
Keyword(s):  
Electroless Plating ◽  
Electron Beam Irradiation ◽  
Xrd Analysis ◽  
High Current ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pulsed Electron Beam ◽  
6063 Aluminum Alloy ◽  
Pre Treatment ◽  
Better Than

The surface irradiation of 6063 aluminum alloy by high current pulsed electron was conducted with the aim of replacing the complicated pre-treatment in the processes of electroless plating. To explore the microstructure changes, optical metallography, SEM (scanning electron microscope), XRD (X-ray diffraction) analyses were carried out, and the sliding tests were used for the detection of wear resistance. It was concluded that the HCPEB irradiation could replace the pre-treatment of aluminum substrate as required in conventional electroless plating with a decreased surface roughness of Ni-P alloy plating layer. The plates exhibited an amorphous microstructure as demonstrated by XRD analysis. The plates, produced with the routine of HCPEB irradiation, activation and electroless plating possess, also exhibited good quality, even better than that of conventional electroless plating technique.

Structure and properties of polypropylene/organic rectorite nanocomposites

Clay Minerals ◽  
2009 ◽  
Vol 44 (1) ◽  
pp. 35-50 ◽  
Author(s):  
Yun Huang ◽  
Xiaoyan Ma ◽  
Guozheng Liang ◽  
Hongxia Yan
Keyword(s):  
Loss Modulus ◽  
Polarized Light ◽  
Clay Content ◽  
Crystal Form ◽  
Ammonium Bromide ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Monoclinic Crystal ◽  
X Ray

AbstractMelt blending using a twin-screw extruder was used to prepare composites of polypropylene (PP)/organic rectorite (PR). The organic rectorite (OREC) was modified with dodecyl benzyl dimethyl ammonium bromide (1227). Wide-angle X-ray diffraction (WAXD) and transmission electron microscopy were used to investigate the dispersion of OREC in the composites. The d spacings of OREC in PR composites was greater than in OREC itself. The dispersion of OREC particles in the PP polymer matrix was fine and uniform when the clay content was small (2 wt.%). The rheology was characterized using a capillary rheometer. The processing behaviour of the PR system improved as the amount of OREC added increased. Non-isothermal crystallization kinetics were analysed using differential scanning calorimetry. It was shown that the addition of OREC had a heterogeneous nucleation effect on PP, and can accelerate the crystallization. However, only when fine dispersion was achieved, and at lower rates of temperature decrease, was the crystallinity greater. Wide-angle X-ray diffraction and polarized light microscopy were used to observe the crystalline form and crystallite size. The PP in the PR composites exhibited an a-monoclinic crystal form, as in pure PP, and in both cases a spherulite structure was observed. However, the smaller spherulite size in the PR systems indicated that addition of OREC can reduce the crystal size significantly, which might improve the ‘toughness’ of the PP. The mechanical properties (tensile and impact strength) improved when the amount of OREC added was appropriate. Dynamic mechanical analysis showed that the storage modulus (E′) and loss modulus (E″) of the nanocomposites were somewhat greater than those of pure PP when an appropriate amount of OREC was added. Finally, thermogravimetric analysis showed that the PR systems exhibited a greater thermal stability than was seen with pure PP.

scholarly journals Purification, crystallization and preliminary X-ray diffraction analysis of a hydroxycinnamoyl-CoA shikimate/quinate hydroxycinnamoyltransferase (HCT) fromCoffea canephorainvolved in chlorogenic acid biosynthesis

2012 ◽  
Vol 68 (7) ◽  
pp. 824-828 ◽  
Author(s):  
Laura A. Lallemand ◽  
James G. McCarthy ◽  
Sean McSweeney ◽  
Andrew A. McCarthy
Keyword(s):  
Structural Data ◽  
Coffea Canephora ◽  
Molecular Replacement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Key Enzyme ◽  
Substrate Specifities ◽  
Drop Technique ◽  
Better Than

Chlorogenic acids (CGAs) are a group of soluble phenolic compounds that are produced by a variety of plants, includingCoffea canephora(robusta coffee). The last step in CGA biosynthesis is generally catalysed by a specific hydroxycinnamoyl-CoA quinate hydroxycinnamoyltransferase (HQT), but it can also be catalysed by the more widely distributed hydroxycinnamoyl-CoA shikimate/quinate hydroxycinnamoyltransferase (HCT). Here, the cloning and overexpression of HCT fromC. canephorainEscherichia colias well as its purification and crystallization are presented. Crystals were obtained by the sitting-drop technique at 293 K and X-ray diffraction data were collected on the microfocus beamline ID23-2 at the ESRF. The HCT crystals diffracted to better than 3.0 Å resolution, belonged to space groupP42212 with unit-cell parametersa=b= 116.1,c= 158.9 Å and contained two molecules in the asymmetric unit. The structure was solved by molecular replacement and is currently under refinement. Such structural data are needed to decipher the molecular basis of the substrate specifities of this key enzyme, which belongs to the large plant acyl-CoA-dependent BAHD acyltransferase superfamily.

Study on the Preparation and Performance of Carboxymethyl Chitosan Calcium and Carboxymethyl Chitosan Zinc Composite Materials

2016 ◽  
Vol 852 ◽  
pp. 1319-1324 ◽  
Author(s):  
Jing Li ◽  
Chang Ping Wei ◽  
Feng Ming Wang ◽  
Li Dan Dong ◽  
Shuang Sun ◽  
...  
Keyword(s):  
Chloride Solution ◽  
Water Solubility ◽  
Chloroacetic Acid ◽  
Sem Analysis ◽  
Carboxymethyl Chitosan ◽  
X Ray Diffraction ◽  
Test Study ◽  
Alkaline Conditions ◽  
And Performance ◽  
Better Than

In this paper,under alkaline conditions,with chloroacetic acid to modify chitosan,obtained carboxymethyl chitosan. At pH<7 conditions,the obtained carboxymethy chitosan respectively were reacted with calcium chloride solution,zinc chloride solution,after fully reacted,obtained carboxymethyl chitosan calcium and carboxymethyl chitosan zinc .Through infrared spectrum,X-ray diffraction and scanning electron microscopy (sem) analysis means,the structure of the products were characterized.Through the cutting of mice tail hemostasia test ,study the performance of the product.The results showed that the water solubility of carboxymethyl chitosan is better than that of chitosan and with excellent performance,and the performance of carboxymethyl chitosan calcium and carboxymethyl chitosan zinc was better than that of carboxymethyl chitosan.

Salts of purine alkaloids caffeine and theobromine with 2,6-dihydroxybenzoic acid as coformer: structural, theoretical, thermal and spectroscopic studies

2021 ◽  
Vol 77 (11) ◽  
Author(s):  
Mateusz Gołdyn ◽  
Anna Komasa ◽  
Mateusz Pawlaczyk ◽  
Aneta Lewandowska ◽  
Elżbieta Bartoszak-Adamska
Keyword(s):  
Hydrogen Bonds ◽  
Water Solubility ◽  
Theoretical Calculations ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Dihydroxybenzoic Acid ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Purine Alkaloids ◽  
Vis Spectroscopy

The study of various forms of pharmaceutical substances with specific physicochemical properties suitable for putting them on the market is one of the elements of research in the pharmaceutical industry. A large proportion of active pharmaceutical ingredients (APIs) occur in the salt form. The use of an acidic coformer with a given structure and a suitable pK a value towards purine alkaloids containing a basic imidazole N atom can lead to salt formation. In this work, 2,6-dihydroxybenzoic acid (26DHBA) was used for cocrystallization of theobromine (TBR) and caffeine (CAF). Two novel salts, namely, theobrominium 2,6-dihydroxybenzoate, C7H9N4O2 +·C7H5O4 − (I), and caffeinium 2,6-dihydroxybenzoate, C8H11N4O2 +·C7H5O4 − (II), were synthesized. Both salts were obtained independently by slow evaporation from solution, by neat grinding and also by microwave-assisted slurry cocrystallization. Powder X-ray diffraction measurements proved the formation of the new substances. Single-crystal X-ray diffraction studies confirmed proton transfer between the given alkaloid and 26DHBA, and the formation of N—H...O hydrogen bonds in both I and II. Unlike the caffeine cations in II, the theobromine cations in I are paired by noncovalent N—H...O=C interactions and a cyclic array is observed. As expected, the two hydroxy groups in the 26DHBA anion in both salts are involved in two intramolecular O—H...O hydrogen bonds. C—H...O and π–π interactions further stabilize the crystal structures of both compounds. Steady-state UV–Vis spectroscopy showed changes in the water solubility of xanthines after ionizable complex formation. The obtained salts I and II were also characterized by theoretical calculations, Fourier-transform IR spectroscopy (FT–IR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and elemental analysis.

scholarly journals MSMEG_6292, a Mycobacterium smegmatis RNA polymerase secondary channel-binding protein: purification, crystallization and X-ray diffraction analysis

2018 ◽  
Vol 74 (9) ◽  
pp. 543-548
Author(s):  
Abyson Joseph ◽  
Valakunja Nagaraja ◽  
Ramanathan Natesh
Keyword(s):  
Rna Polymerase ◽  
Mycobacterium Smegmatis ◽  
Transcriptional Activity ◽  
Molecular Replacement ◽  
X Ray Diffraction ◽  
Secondary Channel ◽  
X Ray ◽  
Cell Parameters ◽  
Crystallization Method ◽  
Better Than

The transcriptional activity of RNA polymerase (RNAP) is controlled by a diverse set of regulatory factors. A subset of these regulators modulate the activity of RNAP through its secondary channel. Gre factors reactivate stalled elongation complexes by enhancing the intrinsic cleavage activity of RNAP. In the present study, the protein MSMEG_6292, a Gre-factor homologue from Mycobacterium smegmatis, was expressed heterologously in Escherichia coli and purified using standard chromatographic techniques. The hanging-drop vapour-diffusion crystallization method yielded diffraction-quality crystals. The crystals belonged to the trigonal space group P3121 (or its enantiomorph P3221), with unit-cell parameters a = b = 83.15, c = 107.07 Å, α = β = 90, γ = 120°. The crystals diffracted to better than 3.0 Å resolution. Molecular-replacement attempts did not yield any phasing models; hence, platinum derivatization was carried out with K2PtCl4 and derivative data were collected to 3.4 Å resolution.

The structures of benzimidazole derivatives and their potential as tuberculostatics

2018 ◽  
Vol 74 (12) ◽  
pp. 1684-1691
Author(s):  
Marek L. Główka ◽  
Sylwia Kałużyńska ◽  
Malwina Krause ◽  
Katarzyna Gobis ◽  
Henryk Foks ◽  
...  
Keyword(s):  
Multidrug Resistant ◽  
Benzimidazole Derivatives ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Resistant Varieties ◽  
Different Types ◽  
Mdr Tb ◽  
Aromatic Systems ◽  
Better Than

Tuberculosis still remains a very important problem, especially its multidrug resistant varieties (MDR-TB). Among the potential tuberculostatics, there are two benzimidazole derivatives, namely 5,6-dimethyl-2-phenylethylbenzo[d]imidazole (1) and (E)-5,6-dimethyl-2-styryl-1H-benzo[d]imidazole (2) which showed significant tuberculostatic activities, better than those of Pyrazinamide and Isoniazyd. Also, the cytotoxicity of 1 appeared promising. The compounds were studied (with the use of X-ray diffraction) in the form of the hemihydrate of 1, C17H18N2·0.5H2O (1a), the methanol hemisolvate of 2, C17H16N2·0.5CH3OH (2a), and the acid oxalate salt of 2, namely (E)-5,6-dimethyl-2-styryl-1H-benzo[d]imidazolium hydrogen oxalate, C17H17N2 +·C2HO4 − (2b). All three structures reveal a similar extended conformation, despite the flexible linker between the two aromatic systems and the different types of strong intermolecular hydrogen bonds. The molecules of 2a are practically planar due to the double bond in the linker, which enables conjugation along the whole molecule, while the molecules of 1a exhibit the possibility of parallel orientations of their aromatic systems, despite the aliphatic (ethyl) linker.

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