Search results for "Derivatization"
showing 10 items of 215 documents
Determination of the cultivar and aging of Sicilian olive oils using HPLC-MS and linear discriminant analysis
2010
A large number of certified samples (84) of Sicilian olive oils arising from the eight cultivars most represented in Sicily (Biancolilla, Cerasuola, Moresca, Nocellara del Belice, Nocellara Etnea, Oglialora Messinese, Brandofino and Tonda Iblea) have been collected and analyzed by HPLC/MS using an atmospheric pressure chemical ionization (APCI) source. The sample preparation is very simple; in fact, the oil samples are diluted without any chemical derivatization. A following statistical data treatment by general discriminant analysis (GDA) allows the determination of the olive oil cultivar. Furthermore, changes in the composition of glyceridic components of the olive oils lead to easy discr…
Antiproliferative activity against leukemia cells of sesquiterpene lactones from the Turkish endemic plant Centaurea drabifolia subsp. detonsa
2017
The apolar organic extract obtained from aerial parts of Centaurea drabifolia Sibth. & Sm. subsp. detonsa (Bornm.) Wagenitz, growing wild in Turkey, was investigated for the first time for its secondary metabolite composition. Seven sesquiterpene lactones belonging to the guaiane class (1-7), including the new compound 4, along with a fatty acid lactone derivative (8), were isolated. The structures of these compounds were established by spectroscopic analysis, including 2D NMR spectroscopic techniques, with the stereostructure of the new guaiane 4 determined with the help of MTPA derivatization. Cytotoxic activities of compounds 1-7 were evaluated against two cancer cell lines, namely acute…
Gas chromatography-mass spectrometry characterization of the varnish and glue of an ancient 18th century double bass.
2007
A GC–MS investigation is conducted on the double bass “Panormus”, property of Conservatorio di Musica “Vincenzo Bellini” in Palermo. The most important components of the varnish (fatty acids) and of the glue (proteinaceous amino acids), with which the musical instrument was treated in the past, are determined. The analyses are carried out by prior derivatization of fatty acids by acidic methanol and of amino acids by acidic methanol and trifluoroacetic anhydride (TFAA). Analytes identification is achieved by direct comparison with several reference materials and the use of a digitized library.
Ethyl Pyrogallarene and Pyrogallarene: Synthesis, Structural Analysis and Derivatization
2004
In the acid-catalyzed synthesis of ethyl pyrogall[4]arene, a novel hexamer, ethyl pyrogall[6] arene, is obtained as a readily isolable minor product. Pyrogall[6]arene can be isolated from the reaction mixture in three different ways yielding the hexamer in different forms and stabilities. Crystallization from DMSO and then recrystallization from acetone gives a stable crystalline solid, recrystallization directly from acetone yields an unstable white powder, while direct recrystallization from THF gives a stable white powder. Both pyrogall[4]arene and pyrogall[6]arene crystallize readily with DMSO filling the voids in the crystal lattice. Co-crystallization studies of the hexamer isolated b…
Extensive Evaluation of a Diffusion Denuder Technique for the Quantification of Atmospheric Stable and Radioactive Molecular Iodine
2010
In this paper we present the evaluation and optimization of a new approach for the quantification of gaseous molecular iodine (I(2)) for laboratory- and field-based studies and its novel application for the measurement of radioactive molecular iodine. alpha-Cyclodextrin (alpha-CD) in combination with (129)I(-) is shown to be an effective denuder coating for the sampling of gaseous I(2) by the formation of an inclusion complex. The entrapped (127)I(2) together with the (129)I(-) spike in the coating is then released and derivatized to 4-iodo-N,N-dimethylaniline (4-I-DMA) for gas chromatography-mass spectrometry (GC-MS) analysis. The (127)I(2) collected can be differentiated from the (129)I(-…
Glycidyl methacrylate derivatization of α,β-poly(N-hydroxyethyl)-dl-aspartamide and α,β-polyasparthydrazide
1997
Abstract α,β-Poly(N-hydroxyethyl)- dl -aspartamide (PHEA) and α,β-polyasparthydrazide (PAHy) are two synthetic macromolecules having many potential applications in the field of biomedical sciences. This paper describes the functionalization of PHEA and PAHy with glycidyl methacrylate (GMA), in order to introduce pendant double bonds in their chains. Derivatized PHEA and PAHy (samples PHG and PAG, respectively) at various GMA content have been obtained and characterized. It has been shown that the derivatization reaction can be controlled by varying some parameters as solvent, catalyst, pH, GMA concentration and reaction time. As expected, PAHy reacted more rapidly and more extensively than …
Characterization of waxes used in pictorial artworks according to their relative amount of fatty acids and hydrocarbons by gas chromatography.
2005
A study attempted to characterize natural waxes used in pictorial works of art was carried out by means of gas chromatography. The analytical treatment requires prior hydrolysis of the waxes to release the fatty acids (FA) (myristic (myr), palmitic (pal), oleic (ole), stearic (ste), araquidic (ara), behenic (beh), lignoceric (lig), cerotic (cer)) from the main esters of the waxes. The formation of volatile derivatives of the fatty acids was carried out by derivatization with ethyl choroformate (ECF). This derivatization reagent was chosen due to the speed, safety and quantitativity of the reaction. The analyzed hydrocarbons were n-eicosane, n-heneicosane, n-docosane, n-tricosane, n-tetracos…
Extraction of dansylated amino acids using the supported liquid membrane technique
1997
Extraction using the supported liquid membrane (SLM) technique demands conditions where the extracted compounds can be made uncharged allowing them to pass through the membrane. For amino acids, being bifunctional, such conditions can not be obtained directly. One way to overcome this problem is to block one of the functionalities by derivatization, utilising the other group for the transport. The SLM extraction of dansylated amino acids was investigated and optimized. It was possible to obtain high extraction efficiencies (>90%) for most amino acids. For amino acids with polar side chains, such high extraction efficiencies were only obtained at low analyte concentrations ( 10 nmol 1-l). Fo…
A detailed MSn study for the molecular identification of a dimer formed from oxidation of pinene
2016
Abstract Dimeric products formed in the oxidation of α- and β-pinene have been frequently observed in laboratory and field studies of biogenic SOA formation. While their existence is undoubted, their exact chemical structures remain unclear. This study uses a combined two step approach aiming on the molecular identification of the most important of the various dimers that have been observed in biogenic secondary organic aerosol formation, a dimer with the molecular weight 358 g mol−1. The first step is the application of a functional group derivatization technique (esterification) to quantify the number of carboxylic acid groups in the target molecule. Based on the detailed interpretation o…
Study of binding media in works of art by gas chromatographic analysis of amino acids and fatty acids derivatized with ethyl chloroformate
1997
The aim of this work is to identify proteinaceous and oil binding media used in paintings from art collections in the Region of Valencia (Spain). This information is extremely useful for conservation and restoration work. The proposed procedure involves protein and glyceride hydrolysis from sub-milligram samples by treatment with hydrochloric acid, followed by neutralization, partition with chloroform and derivatization with ethyl chloroformate (ECF) of both the aqueous and the organic phases. The ECF derivatives of amino acids and azelaic, myristic, palmitic and stearic acids are separated by capillary gas chromatography. Amino acids are mainly found in the aqueous phase and long chain fat…