Search results for "Derivatization"
showing 10 items of 215 documents
High-performance liquid chromatographic separation of modified and native melittin following transglutaminase-mediated derivatization with a dansyl f…
1991
Abstract The 26-amino acid linear, amphiphilic peptide melittin was enzymatically modified with the fluorescent probe monodansylcadaverine using guinea pig liver transglutaminase and a fluorescent derivative of stoichiometry 1:1 was obtained. Reversed-phase and size-exclusion high-performance liquid chromatographic modes were tested in order to resolve the labelled peptide and native species. The influence of several operational variables was analysed and the elution conditions were optimized so that a satisfactory resolution could be achieved in both instances in a rapid, easy manner. Both chromatographic modes offer the possibility of accurate monitoring of the time course of the enzyme-m…
Analysis of primary aliphatic short-chain monoamines by LC in water samples
2003
Abstract Several derivatization procedures with o-phthaldialdehyde-N-acetylcysteine (OPA-NAC) were compared for a rapid analysis of primary aliphatic short-chain monoamines in water samples by HPLC using a LiChorospher analytical separation column (100RP18 125 mm ×4 mm i.d., 5 μm). Both the solution and the solid-support assisted off-line derivatization on C18 SPE cartridges were inadequate options because of beginning degradation processes of the instable isoindol derivatives during their transfer to the analytical column. This problem was precluded with the on-column or solid-support assisted on-line derivatization. In the last mentioned procedure, the derivatization took place in a Hype…
Synthesis, characterization and foaming of PHEA-PLLA, a new graft copolymer for biomedical engineering
2014
Abstract In this study a chemical grafting procedure was set up in order to link high molecular weight poly L-lactic acid (PLLA) chains to the hydrophilic α,β-poly(N-2-hydroxyethyl)-DL-aspartamide (PHEA) backbone. A graft copolymer named PHEA-g-PLLA (or simply PHEA–PLLA) was obtained bearing a degree of derivatization of 1.0 mol.% of PLLA as grafted chain. This new hybrid derivative offers both the opportune crystallinity necessary for the production of scaffolds trough a thermally induced phase separation (TIPS) technique and the proper chemical reactivity to perform further functionalizations with bio-effectors and drugs. PHEA–PLLA porous scaffolds for tissue engineering applications were…
Direct infusion mass spectrometry as a fingerprint of protein-binding media used in works of art
2005
A direct infusion mass spectrometry method for the characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Amino acids are released by acid hydrolysis and dissolved in a mixture of acidic water and ethanol. This mixture is directly infused into a mass spectrometer without any derivatization. The mass spectrometer is operated in positive ion electrospray mode (ESI-MS) to yield [M+H]+ ions for the amino acids. Relative amounts of each amino acid are calculated for each protein (beef and porcine gelatines, albumin, casein and egg). The analyzed proteins were satisfactorily distinguished. The method is…
Determination of ammonia and primary amine compounds and Kjeldahl nitrogen in water samples with a modified Roth's fluorimetric method.
2005
Abstract A method for the simultaneous determination of primary amino groups and ammonium ion has been proposed. The method is based in solution derivatization with o-Phthaldialdehyde/N-acetyl-cisteine (OPA/NAC) and fluorescence measurement of the formed isoindols. Analytical characteristics and description of the developed procedure have been provided. The calibration graphs for ammonium (up to 1.44 mg L−1 of N) and methylamine as primary amino model compound (up to 0.282 mg L−1 of N), were obtained. Bivariate and multivariate calibration models have been tested. The limits of detection were 0.07 mg L−1 of N and 0.004 mg L−1 of N for ammonium and amine, respectively. The procedure was firs…
Styryl-lactones from the stem bark of Goniothalamus arvensis
1999
The fractionation of the methanolic extract of Goniothalamus arvensis (Annonaceae) stem bark led to the isolation of two novel styryl-lactones, arvensin and (+)-2-epi-altholactone. The structures of these compounds, which belong to the furano-pyrone group, were established on the basis of mass spectrometry, one- and two-dimensional nuclear magnetic resonance experiments, as well as simple chemical derivatization. The relative and absolute configurations of the compounds are discussed. Copyright © 1999 John Wiley & Sons, Ltd.
Immunoassays for trifloxystrobin analysis. Part I. Rational design of regioisomeric haptens and production of monoclonal antibodies
2014
Trifloxystrobin is one of the main active principles belonging to the strobilurin family of crop protection compounds. In this article, the synthesis of a battery of regioisomeric functionalized derivatives of trifloxystrobin is described. The same aliphatic linear carboxylated chain was introduced as spacer arm in all of the synthesized haptens, but it was located at different positions of the parent molecule. N,N′-Disuccinimidyl carbonate was employed for hapten activation, so the resulting N-hydroxysuccinimyl ester could be readily purified and efficiently coupled to proteins. After immunization and hybridoma generation, a collection of 20 mouse monoclonal antibodies from different immun…
Characterization of acrylic resins used for restoration of artworks by pyrolysis-silylation-gas chromatography/mass spectrometry with hexamethyldisil…
2006
A procedure based on the technique of the pyrolysis-GC/MS has been applied, in this work, in order to determine the composition of synthetic acrylic resins employed in artworks. The method is based on the on line derivatization of these resins using hexamethyldisilazane (HMDS). Results obtained have been compared with those others from direct pyrolysis and in situ thermally assisted hydrolysis and methylation with tetramethylammonium hydroxide (TMAH). Sensitivity using HMDS as derivatising reagent is found similar to that from direct pyrolysis and methylation with TMAH. Better resolution of the most representative peaks has been also obtained. Additionally, this method reduces the formation…
Analytical characterization of diterpenoid resins present in pictorial varnishes using pyrolysis–gas chromatography–mass spectrometry with on line tr…
2005
Abstract A procedure based on the technique of the pyrolysis–gas chromatography–mass spectrometry (Py–GC–MS) has been applied, in this work, in order to determine the composition of diterpenoid resin employed in art works. The method is based on the on line derivatization of these resins using hexamethyldisilazane (HMDS). Results obtained were compared with those previously reported in literature from Venice turpentine, Strasbourg turpentine, colophony, sandarac and Manila copal using this same method and with those others from in situ thermally assisted hydrolysis and methylation with tetramethylammonium hydroxide (TMAH). Canada balsam, copper resinate and Copaiba balsam have been also ana…
New Biodegradable Hydrogels Based on Inulin and α,β-Polyaspartylhydrazide Designed for Colonic Drug Delivery: In Vitro Release of Glutathione and Oxy…
2010
Succinic derivatives of inulin (INU-SA) with two different degrees of derivatization (20% and 30%, mol/mol) were cross-linked with α,β-polyaspartylhydrazide (PAHy) to obtain INUPAHy hydrogels. Cross-linking was performed using N-ethyl-N-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC) and N-hydroxysulfosuccinimide (NHSS) as coupling agents and by varying the reaction time (4 h, 8 h and 24 h). All samples prepared were characterized by FT-IR analysis and swelling measurements in different media. In vitro assays, performed in the presence of inulinase, demonstrated the degradability of the prepared hydrogels. Cell compatibility was evaluated using Caco-2 cells through both direct and …