scholarly journals Isolation and Characterization of Polysaccharides from the Ascidian Styela clava

Polymers ◽  
2021 ◽  
Vol 14 (1) ◽  
pp. 16
Author(s):  
Jesus Valcarcel ◽  
José Antonio Vázquez ◽  
Uxía R. Varela ◽  
Rui L. Reis ◽  
Ramon Novoa-Carballal
Keyword(s):  
Gel Permeation Chromatography ◽  
Weight Fraction ◽  
Crystalline Cellulose ◽  
X Ray Diffraction ◽  
Styela Clava ◽  
Sea Squirt ◽  
Aspect Ratios ◽  
Light Scattering Detection ◽  
Isolation And Characterization

Styela clava is an edible sea squirt farmed in Korea that has gradually invaded other seas, negatively impacting the ecology and economy of coastal areas. Extracts from S. clava have shown wide bioactivities, and ascidians have the unique capability among animals of biosynthesizing cellulose. Thus, S. clava is a relevant candidate for valorization. Herein, we aimed at surveying and characterizing polysaccharides in both tunic and flesh of this ascidian. To this end, we enzymatically hydrolyzed both tissues, recovering crystalline cellulose from the tunic with high aspect ratios, based on results from microscopy, X-ray diffraction, and infrared spectroscopy analyses. Alkaline hydroalcoholic precipitation was applied to isolate the polysaccharide fraction that was characterized by gel permeation chromatography (with light scattering detection) and NMR. These techniques allowed the identification of glycogen in the flesh with an estimated Mw of 7 MDa. Tunic polysaccharides consisted of two fractions of different Mw. Application of Diffusion-Ordered NMR allowed spectroscopically separating the low-molecular-weight fraction to analyze the major component of an estimated Mw of 40–66 kDa. We identified six different sugar residues, although its complexity prevented the determination of the complete structure and connectivities of the residues. The two more abundant residues were N-acetylated and possibly components of the glycosaminoglycan-like (GAG-like) family, showing the remaining similarities to sulfated galactans. Therefore, Styela clava appears as a source of nanocrystalline cellulose and GAG-like polysaccharides.

Assessment of the X-ray diffraction–absorption method for quantitative analysis of largely amorphous pharmaceutical composites

2003 ◽  
Vol 36 (1) ◽  
pp. 74-79 ◽  
Author(s):  
P. Bergese ◽  
I. Colombo ◽  
D. Gervasoni ◽  
Laura E. Depero
Keyword(s):  
Weight Fraction ◽  
Toxic Waste ◽  
X Ray Diffraction ◽  
Amorphous Halo ◽  
Scanning Calorimetry ◽  
X Ray ◽  
The Matrix ◽  
Diffraction Patterns ◽  
Challenging Question

Determination of the residual weight fraction of a crystalline drug in a largely amorphous pharmaceutical composite is still a challenging question. None of the quantitative X-ray diffraction (QXRD) methods found in the literature is suitable for these inclusion systems. The composite's diffraction patterns present a structured amorphous halo (arising from the amorphous matrix and drug molecular clusters) in which the crystalline drug peaks rise up. Moreover, the matrix traps a non-negligible quantity of water (which cannot be directly detected by X-ray diffraction) and the crystal structure of the drug may be unknown. In this work, a development of the QXRD analysis based on the diffraction–absorption technique is presented. The method is standardless, avoids the interpretation of the amorphous halo and the knowledge of the crystal structures of the phases, and takes into account the absorbed water. Results are in excellent agreement with those obtained by differential scanning calorimetry (DSC). The general features of the technique open its application to other classes of largely amorphous composite materials, like glass systems generated in the stabilization/solidification of toxic waste.

scholarly journals Isolation and Characterization of 1,3-Bis(vinylbenzyl)thymine: Copolymerization with Vinylbenzyl Thymine Ammonium Chloride

2017 ◽  
Vol 2017 ◽  
pp. 1-10
Author(s):  
Ngoc Chau H. Vy ◽  
Nina Bin Chen ◽  
Debora M. Martino ◽  
John C. Warner ◽  
Nancy Lee
Keyword(s):  
Gel Permeation Chromatography ◽  
Cross Linking ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Aromatic Stacking ◽  
Molecular Weight Distributions ◽  
Isolation And Characterization ◽  
Added Benefit ◽  
Vinylbenzyl Thymine

A novel bioinspired molecule, 1,3-bis(vinylbenzyl)thymine (bisVBT), was isolated as a by-product during the synthesis of 1-(4-vinylbenzyl)thymine (VBT) and analyzed with various techniques: NMR, IR, and Single-Crystal X-ray Diffraction. In addition to embodying all the desired characteristics of VBT (i.e., having the ability to undergo a 2π+2π photodimerization reaction upon UV irradiation, a derivatization site, hydrogen bonding sites, and aromatic stacking ability) the bisVBT monomer has the added benefit of having two vinyl groups for cross-polymerization. Copolymerizing the bisVBT monomer with the charged monomer vinylbenzyl triethylammonium (VBA) chloride, different copolymers/terpolymers/cross-linked network were obtained, as it was shown by the absence of the vinyl resonance in the NMR spectra. Thermal Gravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) showed an indication of materials with low degree of cross-linking. A Gel Permeation Chromatography (GPC) method was improved to better characterize the molecular weight distributions of the cationic structures. Preliminary qualitative cross-linking studies were performed on bisVBT-VBA copolymers, and a comparison with VBT-VBA copolymers is presented.

Determination of the Relative Amounts of α-carbamazepine and β-carbamazepine in a Mixture by Powder X-Ray Diffractometry

1990 ◽  
Vol 5 (3) ◽  
pp. 155-159 ◽  
Author(s):  
Raj Suryanarayanan
Keyword(s):  
Weight Fraction ◽  
Preparation Technique ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
X Ray ◽  
Sample Preparation Technique ◽  
Integrated Intensity ◽  
Diffraction Patterns ◽  
Good Agreement

AbstractA powder X-ray diffraction technique has been developed to quantify the relative amounts of α-carbamazepine (A) and β-carbamazepine (B) when they occur as a mixture. The theoretical basis of this technique was developed in 1948 by Alexander and Klug (Anal. Chem., 20:886-889). The powder X-ray diffraction patterns of A and B revealed that the line with d-spacing of 10.1 Å was unique to A. The ratio of the integrated intensity of the 10.1 Å line in a mixture of A and B, to the intensity of the 10.1 Å line in a sample consisting of only A, was calculated as a function of weight fraction of A in the mixture. These ratios were also experimentally determined, and there was a good agreement between the theoretical and experimental intensity ratios. The particle size of the samples, the sample preparation technique and the experimental conditions were controlled so as to eliminate the major sources of error in powder X-ray diffractometry. In order to minimize preferred orientation of the particles, a sample holder was specially fabricated.

Functionality Distribution of Hydroxyl-Terminated Polybutadienes by Gel Permeation Chromatography. I. Method and Calibration Procedure

1976 ◽  
Vol 49 (5) ◽  
pp. 1238-1249
Author(s):  
J. N. Anderson ◽  
S. K. Baczek ◽  
H. E. Adams ◽  
L. E. Vescelius
Keyword(s):  
Molecular Weight ◽  
Near Infrared ◽  
Gel Permeation Chromatography ◽  
Weight Fraction ◽  
Calibration Procedure ◽  
Double Bonds ◽  
Molecular Weight Distributions ◽  
Fractionation Procedure ◽  
Gel Permeation

Abstract In recent years, considerable attention has been focused on the structural characterization of functionally terminated hydrocarbon prepolymers used in propellant binders and other applications. The molecular weight averages and molecular weight distributions of hydroxyl-and carboxyl-terminated poly butadienes have been determined by gel permeation chromatography (GPC). The functionality distribution of these prepolymers has also been previously studied by column fractionation and a procedure combining GPC and column fractionation of the polymer by stepwise elution from silica gel. The carboxyl or hydroxyl equivalent weights of the fractions were determined by infrared or near-infrared spectroscopy. The fractionation procedure is quite laborious, and multiple peaks were observed in the elution profile, making it difficult to decide how the fractions were to be grouped for subsequent analysis. Previously, a technique for determining the distribution of unsaturation in copolymers containing a small number of double bonds as a function of GPC elution volume was developed. The technique utilized a GPC equipped with uv photometer and differential refractometer detectors to determine the ratio of the weight fraction of olefinic bonds to the weight fraction of polymer by GPC analysis of the polymer after derivatization of the double bonds with 2,4-dinitrobenzenesulfenyl chloride. It was suggested that the technique should be applicable for the determination of the distribution of other functional groups with the choice of suitable reagents for derivatization. The purpose of this investigation was to attempt to extend our previous study to simultaneously determine the molecular weight averages, molecular weight distribution, hydroxyl equivalent weight, functionality averages, and functionality distribution of hydroxyl-terminated polybutadienes by a GPC technique.

Sem and X-Ray Analysis of Renal and Biliary Calculi

1976 ◽  
Vol 34 ◽  
pp. 306-307
Author(s):  
R. J. Narconis ◽  
G. L. Johnson
Keyword(s):  
Chemical Constituents ◽  
Natural State ◽  
X Ray Diffraction ◽  
Chemical Methods ◽  
X Ray ◽  
Additional Dimension ◽  
Biliary Calculi ◽  
Calculus Formation ◽  
Scanning Electron

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.

Symmetry breaking in convergent-beam diffraction

1989 ◽  
Vol 47 ◽  
pp. 480-481
Author(s):  
D.J. Eaglesham
Keyword(s):  
Symmetry Breaking ◽  
Point Group ◽  
X Ray Diffraction ◽  
Multiple Diffraction ◽  
Space Groups ◽  
Atomic Displacements ◽  
Small Probe ◽  
Phase Sensitive ◽  
Convergent Beam

Convergent Beam Electron Diffraction is now almost routinely used in the determination of the point- and space-groups of crystalline samples. In addition to its small-probe capability, CBED is also postulated to be more sensitive than X-ray diffraction in determining crystal symmetries. Multiple diffraction is phase-sensitive, so that the distinction between centro- and non-centro-symmetric space groups should be trivial in CBED: in addition, the stronger scattering of electrons may give a general increase in sensitivity to small atomic displacements. However, the sensitivity of CBED symmetry to the crystal point group has rarely been quantified, and CBED is also subject to symmetry-breaking due to local strains and inhomogeneities. The purpose of this paper is to classify the various types of symmetry-breaking, present calculations of the sensitivity, and illustrate symmetry-breaking by surface strains.CBED symmetry determinations usually proceed by determining the diffraction group along various zone axes, and hence finding the point group. The diffraction group can be found using either the intensity distribution in the discs

Sign in / Sign up

Export Citation Format

Share Document