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Results for “Spectroscopy, Fourier Transform Infrared”

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PubMed2004

Surface modified ormosil nanoparticles.

Organically modified silanes (ORMOSIL) such as vinyl triethoxysilane readily aggregate in the aqueous cores of reverse micelles where the triethoxysilane moieties are hydrolyzed to form a hydrated silica network and the vinyl groups protruded out from the surface of the nanoparticles toward the hydrophobic side of the micellar interface. These particles are spherical and the size distribution of the particles is relatively narrow, with an average diameter of 87 nm. Surface vinyl silica nanoparticles so formed have been oxidized to surface carboxylic silica nanoparticles, followed by chemical conjugation with polyethyleneglycol amine (PEG amine) through the ethyl-3-(3-dimethylaminopropyl) (EDCI) carbodiimide reaction. The characteristic surface groups have been identified by Fourier transform infrared spectroscopy, while the size and the morphology of the particles have been studied by dynamic light scattering and transmission electron microscopy. It has been found that about 80-85% of the carboxylic groups are PEGylated during the EDCI reaction.

Micelles↗

PubMed2001

Ring-opening polymerization of lactones in the presence of hydroxyapatite.

The ring-opening polymerization of epsilon-caprolactone, delta-valerolactone (VL) and D,L-lactide, respectively, in the presence of different proportions of hydroxyapatite (HA) was catalyzed by stannous (II)octoate (SnOct2) at 130 degrees C and resulted in composites. The lactones were almost completely converted to the polymers within a reaction time of 70 up to 240 min. The number-average molecular weights Mn as determined by size exclusion chromatography decreased with increasing content of HA. The initiating efficiency of HA as calculated from the difference of the polymerization degrees P. obtained with and without HA turned out to be relatively low with ca. 11 to 0.5% for 1 to 80 wt% HA, respectively. For the polymerization of VL, the initiating efficiency of HA was on the average threefold higher. The quantitative proof of non-extractable polymer on HA by means of thermogravimetric analysis, fourier transform infrared spectroscopy with photoacoustic detection and differential scanning calorimetry confirmed the initiating efficiency of HA as mentioned above. This poly(lactone) can be debound from HA by treatment with aqueous HCl. Hence it is assumed to be ionically bound.

Biopolymers↗

PubMed2002

Novel synthesis and characterization of an AB-type carbonate-substituted hydroxyapatite.

A novel synthesis route has been developed to produce a high-purity mixed AB-type carbonate-substituted hydroxyapatite (CHA) with a carbonate content that is comparable to the type and level observed in bone mineral. This method involves the aqueous precipitation in the presence of carbonate ions in solution of a calcium phosphate apatite with a Ca/P molar ratio greater than the stoichiometric value of 1.67 for hydroxyapatite (HA). The resulting calcium-rich carbonate-apatite is sintered/heat-treated in a carbon dioxide atmosphere to produce a single-phase, crystalline carbonate-substituted hydroxyapatite. In contrast to previous methods for producing B- or AB-type carbonate-substituted hydroxyapatites, no sodium or ammonium ions, which would be present in the reaction mixture from the sodium or ammonium carbonates commonly used as a source of carbonate ions, were present in the final product. The chemical and phase compositions of the carbonate-substituted hydroxyapatite was characterized by X-ray fluorescence and X-ray diffraction, respectively, and the level and nature of the carbonate substitution were studied using C-H-N analysis and Fourier transform infrared spectroscopy, respectively. The carbonate substitution improves the densification of hydroxyapatite and reduces the sintering temperature required to achieve near-full density by approximately 200 degrees C compared to stoichiometric HA. Initial studies have shown that these carbonate-substituted hydroxyapatites have improved mechanical and biologic properties compared to stoichiometric hydroxyapatite.

Bone Substitutes↗

PubMed1995

Hydrogen bonding in a non-steroidal anti-inflammatory drug--Naproxen.

Photophysical properties of a non-steroidal anti-inflammatory drug, Naproxen (6-methoxy alpha-methyl-2-naphthalene acetic acid sodium salt), were investigated in solvents of different polarity, hydrogen donor ability and also in cyclodextrins. The results indicate that in all cases the emitting state is the 1L(b) singlet. In alcoholic solvents, an intermolecular hydrogen bond is responsible for the observed photophysical behaviour of the probe whereas in non-protic solvents (polar and weakly polar) an intramolecular hydrogen bond type is postulated to rationalize the data found. In water, the non-radiative rate constant has a value similar to those found in aqueous solutions of alpha- and beta-cyclodextrins where the probe form complexes. The behaviour in water is explained by a water-structure enforced hydrophobic effect. The spectroscopic results are interpreted on the basis of a multiple-parameter model that considers specific solute-solvent interactions. These were also observed in the ground state and detected by Fourier transform infrared spectroscopy. Molecular mechanics (MM) and molecular orbital (AM1) calculations also support the existence of two conformations (rotamers) in Naproxen with non-equivalent intramolecular hydrogen bond-like formation.

Anti-Inflammatory Agents, Non-Steroidal↗

PubMed1995

Organic analysis of hydrogen cyanide polymers: prebiotic and extraterrestrial chemistry.

Hydrogen cyanide polymerizes readily to a black solid from which a yellow-brown powder can be extracted by water and further hydrolyzed to alpha-amino acids. These macromolecules could be major components of the dark matter observed on many bodies in the outer solar system, including comets and asteroids. Primitive Earth might therefore have been covered with HCN polymers through bolide bombardment or be terrestrial synthesis. Several instrumental methods were used for the separation and identification of these intriguing polymeric materials, including photoacoustic Fourier transform infrared spectroscopy, supercritical fluid extraction chromatography and pyrolysis mass spectrometry. Our integrated analytical approach revealed fragmentation patterns and chemical functionalities consistent with the presence of polymeric peptide precursors both in HCN polymers and in the Murchison meteorite.

Astronomy↗

PubMed2000

Plant fructans stabilize phosphatidylcholine liposomes during freeze-drying.

Fructans have been implicated as protective agents in the drought and freezing tolerance of many plant species. A direct proof of their ability to stabilize biological structures under stress conditions, however, is still lacking. Here we show that inulins (linear fructose polymers) isolated from chicory roots and dahlia tubers stabilize egg phosphatidylcholine large unilamellar vesicles during freeze-drying, while another polysaccharide, hydroxyethyl starch, was completely ineffective. Liposome stability was assessed after rehydration by measuring retention of the soluble fluorescent dye carboxyfluorescein and bilayer fusion. Inulin was an especially effective stabilizer in combination with glucose. Analysis by HPLC showed that the commercial inulin preparations used in our study contained no low molecular mass sugars that could be responsible for the observed stabilizing effect of the fructans. Fourier transform infrared spectroscopy showed a reduction of the gel to liquid-crystalline phase transition temperature of dry egg PtdCho by more than 20 degrees C in the presence of inulin. A direct interaction of inulin with the phospholipid in the dry state was also indicated by dramatic differences in the phosphate asymmetric stretch region of the infrared spectrum between samples with and without the polysaccharide.

Cichorium intybus↗

PubMed2001

A new method for the generation of patterned protein films by encapsulation in arrays of thermally evaporated lipids.

In this article we demonstrate a versatile method for the generation of patterned protein films by encapsulation in arrays of the lipids, octadecylamine (ODA, cationic), and arachidic acid (AA, anionic). A simple 2 x 2 array of ODA and AA was vacuum deposited on different substrates using appropriate masks. Thereafter, the enzymes pepsin and fungal protease as well as the heme-proteins cytochrome c and hemoglobin were encapsulated in the different elements of the array by sequential immersion (combined with judicious masking) of the array elements in the different protein solutions. The proteins are incorporated into the lipid elements by electrostatic interaction between charged amino acid residues on the protein surface and charged functional groups in the lipid matrix. This procedure leads to spatially distinct regions of the different proteins on one substrate and shows promise for single-chip multianalyte immunoassay/multiplex, high-throughput biosensor and catalysis applications. Fourier transform infrared spectroscopy (FTIR) was used to monitor the incorporation of the proteins in the different elements of the array as well as to ascertain whether intermixing of the proteins in a particular array element had occurred. The heme-protein composite regions were further characterized using UV-VIS spectroscopy.

Amines↗

PubMed1995

Lyophilization-induced reversible changes in the secondary structure of proteins.

Changes in the secondary structure of some dozen different proteins upon lyophilization of their aqueous solutions have been investigated by means of Fourier-transform infrared spectroscopy in the amide III band region. Dehydration markedly (but reversibly) alters the secondary structure of all the proteins studied, as revealed by both the quantitative analysis of the second derivative spectra and the Gaussian curve fitting of the original infrared spectra. Lyophilization substantially increases the beta-sheet content and lowers the alpha-helix content of all proteins. In all but one case, proteins become more ordered upon lyophilization.

Amides↗

PubMed2004

[Isolation and identification of alkaloids from Armeniaca mume Sieb].

OBJECTIVE: To study the alkaloids from Armeniaca mume Sieb. METHODS: The alkaloids were extracted with chloroform from 80% alcoholic extract and concentrated. Then they were transferred into aqueous solution and absorbed by macroporous cation exchange resin. The concentrated total eluent was extracted with chloroform. The alkaloids were purified by recrystallization with petroleum ether and sublimation. Then they were determined by Fourier Transform Infrared spectroscopy, Mass spectrometry and Nuclear magnetic resonance etc methods. RESULT: Two alkaloids were separated and their structures were elucidated as 2,2,6,6-tetramethyl-4-piperidone and tert-butylurea on the basis of spectral evidence. CONCLUSION: They are new alkaloids from A. mume.

Alkaloids↗

PubMed2006

Synthesis and characterization of PCL-b-PEO-b-PCL-based nanostructured and porous hydrogels.

Hydrogels with nanoscale structure were synthesized using amphiphilic poly(epsilon-caprolactone)-poly(ethylene oxide)-poly(epsilon-caprolactone) (PCL-b-PEO-b-PCL) triblock copolymers. Small-angle X-ray scattering (SAXS) studies show that the block copolymers form 30-40 nm structures in aqueous solution and that these patterns are retained, with some increase in length scale, following electron beam cross-linking. Lamellar nanostructures were observed by SAXS and atomic force microscopy (AFM), with SAXS indicating cylindrical structure as the block lengths become more different in length. It is demonstrated through Fourier transform infrared spectroscopy (FTIR), mass loss, and differential scanning calorimetry (DSC) that the PCL can be completely removed by hydrolysis in NaOH(aq) to form porous PEO hydrogels. These hydrogels retain active functional groups following PCL removal that serve as sites for further chemical modification.

Calorimetry, Differential Scanning↗

PubMed1993

Infrared spectral analysis of extractables from poly(etherurethane urea) (PEUU) elastomers.

Poly(etherurethane urea) (PEUU) elastomers when employed as biomedical devices may be susceptible to extraction upon implantation. Four PEUU elastomers containing a single PEUU formulation, but varying in terms of their additives, were subjected to an in vitro extraction procedure. The additives in the PEUUs were Methacrol 2138 F at 5 wt% and Santowhite powder at 1 wt% levels. Only 1-2 wt% of the PEUUs was extractable with methanol. Fourier transform infrared spectroscopy (FT-IR) furnished qualitative and quantitative information on the extractables. The extractables consisted of a PEUU component that on the average was richer in soft segment than the bulk PEUU, and the two additives, Methacrol 2138 F and Santowhite powder.

Biocompatible Materials↗

PubMed2005

[Analysis of Chinese drug beimu and its fake species with clustering analysis and FTIR spectra].

OBJECTIVE: To identify Chinese drug Beimu from its fake species. METHOD: IR spectra was obtained by Fourier Transform Infrared Spectroscopy (FTIR) and clustering analysis was adopted for authentication. RESULT: There were significant differences between Beimu and its fake species. CONCLUSION: The established method was quick, sensitive and accurate. It could be used for the differentiation of different species of Beimu materials and their fake species.

China↗

PubMed2005

Preparation and characterization of uniform nanosized cephradine by combination of reactive precipitation and liquid anti-solvent precipitation under high gravity environment.

In this work, a novel direct method, which was combined with reactive precipitation and liquid anti-solvent precipitation under high gravity environment, had been developed to prepare nanosized cephradine with narrow particle size distribution. Compared with commercial crude cephradine, the prepared cephradine showed a significant decrease in particle size, a significant increase in the specific surface area and shorter dissolving time when used for injection. The characteristic particle size was between 200-400 nm. The specific surface area increased from 2.95 to 10.87 m2/g after micronization. When the amount of L-arginin decreased from 0.25 to 0.18 g, the mixture of nanosized cephradine and L-arginine could still dissolve in 1 min. The X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) analysis indicated that the physical characteristics and molecular states remained unchanged after the recrystallization process. This method had potential application in industrial fields because of its low cost, efficient processing and the ease of scaling-up.

Cephalosporins↗

PubMed2003

Tau filaments from human brain and from in vitro assembly of recombinant protein show cross-beta structure.

Abnormal filaments consisting of hyperphosphorylated microtubule-associated protein tau form in the brains of patients with Alzheimer's disease, Down's syndrome, and various dementing tauopathies. In Alzheimer's disease and Down's syndrome, the filaments have two characteristic morphologies referred to as paired helical and straight filaments, whereas in tauopathies, there is a wider range of morphologies. There has been controversy in the literature concerning the internal molecular fine structure of these filaments, with arguments for and against the cross-beta structure demonstrated in many other amyloid fibers. The difficulty is to produce from brain pure preparations of filaments for analysis. One approach to avoid the need for a pure preparation is to use selected area electron diffraction from small groups of filaments of defined morphology. Alternatively, it is possible to assemble filaments in vitro from expressed tau protein to produce a homogeneous specimen suitable for analysis by electron diffraction, x-ray diffraction, and Fourier transform infrared spectroscopy. Using both these approaches, we show here that native filaments from brain and filaments assembled in vitro from expressed tau protein have a clear cross-beta structure.

Alzheimer Disease↗

PubMed2004

Spectroscopic determination of the degree of esterification of pectic substances from kenaf.

Pectins were isolated from bark, wood and pith of four kenaf (Hibiscus cannabinus L.) varieties. The degree of esterification of isolated pectins was studied using Fourier transform infrared spectroscopy. It was determined as being between 57 and 90% and there were no notable differences between kenaf varieties. The higher value of the degree of esterification was presented in wood pectins (86-90%), the interim in pith (75-83%) and the lower in bark (57-64%).

Hibiscus↗

PubMed2003

Synthesis of p, p'-divinylazobenzene.

OBJECTIVE: To synthesize p, p'-divinylazobenzene (DVAB). METHOD: Wittig reagent was initially synthesized using P-nitrobenzyl bromide and triphenylphosphine, followed by reaction with formaldehyde to produce p-nitro styrene, which was then deoxidized by Zn/NaOH for the final product of DVAB. RESULTS: Fourier transform infrared spectroscopy, nuclear magnetic resonance and element analysis were employed to identify the structure of DVAB, and the lambda(max) as determined by ultraviolet spectroscopy occurred at 357 nm. CONCLUSIONS: The synthesis procedure of DVAB was therefore optimized with high yield.

Azo Compounds↗

PubMed1994

Calcium phosphate formation on sol-gel-derived bioactive glasses in vitro.

When soluble salts are used in the sol-gel processing of bioactive glasses, the resulting materials are not homogeneous. To produce homogeneous gel-glasses, a sol-gel method using all alkoxide precursors was developed. In this work the in vitro bioactivity of the new all-alkoxide gel-glasses is investigated. Three compositions in the system, CaO-P2O5-SiO2, were studied. Solid samples were soaked in Tris buffer and simulated body fluid (SBF), and the rate of formation of hydroxy carbonate apatite (HCA) on the surface of the glasses was measured by Fourier transform infrared spectroscopy. The solutions were analyzed before and after reaction by inductively coupled plasma. All compositions studied formed a hydroxy carbonate apatite (HCA) layer within 8 h in both test solutions. The HCA layer grew rapidly when SBF was used.

Apatites↗

PubMed2005

Synthesis of dawsonite: a method to treat the etching waste streams of the aluminium anodising industry.

Synthesis of dawsonite was studied as a way to deal with the etching waste streams of the aluminium anodising industry in order to reduce the emissions to the environment and also to recover useful and marketable mineral resource materials. The process of synthesis was carried out using two different waste streams arising from the etching section of an anodising process when a cascade rinsing system is employed, the spent etching bath solution (132 g/l of Al and 151 g/l of Na), and the first stage effluent from the cascade rinsing system (67 g/l of Al and 71 g/l of Na). The synthesis of dawsonite was studied as a function of NaHCO3/Al molar ratio (1-10), crystallization temperature (30-150 degrees C), and reaction time (2-48 h) using supersaturated NaHCO3 solutions. A NaHCO3/Al molar ratio of 3 was optimal to obtain dawsonite as a single phase, and a reaction time of 24 h and high crystallization temperature (150 degrees C) to improve its crystallinity. The mineral characterisation was performed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and differential thermal analysis (DTA), all of which indicated characteristics typical of the desired compound. Almost 100% of the aluminium initially present in the etching waste streams was recovered in the form of dawsonite when the appropriate conditions for its synthesis were used.

Aluminum Compounds↗