Search results for "Deriva"
showing 10 items of 1423 documents
Total Synthesis of (±)-Oxalicumone C and Chiral Resolution and Elucidation of Its Absolute Configuration
2014
The racemic total synthesis, the chiral resolution, and the elucidation of the absolute configuration of the natural product oxalicumone C were investigated. The goal was achieved by a synthetic strategy beginning with the synthesis of a 5-hydroxy-7-methylchromone precursor. Further modification possibilities were achieved by introduction of a vinyl moiety into the chromone, which was based on a selective iodination step in the 3-position. Further transformations furnished the racemic natural product. To determinate the absolute configuration of naturally occurring oxalicumone C, both enantiomers were separated by chiral HPLC. Comparison of the calculated and experimental vibrational circul…
Synthese von 2-Acyloxy- und 2-Alkyloxy-3-ketoglycalen und ihren Bromaddukten
1983
Die an den Hydroxygruppen acetyl-, pivaloyl- und methylgeschutzten 2-Hydroxy-3-ketoglycale 5a, 5b bzw. 11 werden durch Oxidation der entsprechenden 1-O-Acylglucopyranosen 3a, 3b bzw. 9 an der freien 3-Hydroxygruppe mit Dimethylsulfoxid/Acetanhydrid oder Chlorsulfonylisocyanat hergestellt und charakterisiert. Nur beim Acetylderivat 3a verlaufen die Oxidation und die Eliminierung des 1-Acetyloxysubstituenten in einem Schritt. Beim Pivaloylderivat 3b und beim Methylderivat 9 mus die Eliminierung aus der 3-Ulose 4 bzw. 10 mit Diazabicycloundecen (DBU) vervollstandigt werden. – Die geschutzten Hex-1-enopyran-3-ulosen 5a, 5b und 11 addieren Brom stereoselektiv unter Bildung der D-ribo-konfigurier…
Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.
2009
Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise f…
Chiral determination of amphetamine and related compounds using chloroformates for derivatization and high-performance liquid chromatography
1999
The enantiomeric determination of amphetamine and various amphetamine-type compounds by liquid chromatography after chiral derivatization with 9-fluorenylmethyl chloroformate-L-proline (FMOC-L-Pro) is reported. The results obtained were compared with those achieved after achiral derivatization with 9-fluorenylmethyl chloroformate and subsequent separation of the derivatives on a beta-cyclodextrin chiral stationary phase. Conditions for the derivatization of amphetamines with FMOC-L-Pro were investigated, including the effect of the derivatization reagent concentration, pH and reaction time, using amphetamine, ephedrine and pseudoephedrine as model compounds. On the basis of these studies, p…
Photochemical Derivatization and Fluorimetric Determination of Promethazine in a FIA Assembly
1992
Abstract The flow injection fluorimetric determination of promethazine is carried out by on-line photoderivatization. The PTFE tubing is helically coiled around the lamp. An analytical procedure is proposed by using aqueous solution as carrier stream: the calibration graph is linear over the range 0.05 - 20 ppm. The influence of foreign compounds is studied and the method is applied to promethazine determination in pharmaceutical formulations.
Characterization of bile acids and fatty acids from ox bile in oil paintings by gas chromatography?mass spectrometry*1
2004
Characterization of ox bile, traditionally used in painting, is of interest in the fields of archaeometry and conservation and restoration of works of art. Bile acids, fatty acids (F), and cholesterol found in ox bile have been identified using a derivatization method that combines the formation of ethyl esters from the carboxylic groups and the trimethylsilyl ethers from hydroxyl groups. This method of analysis is consistent with these others proposed by the authors to analyze drying oils, proteins, and diterpenic resins usually used as binders and varnishes by the painters. Bile acids from binary samples such as animal glue/ox bile, casein/ox bile and Arabic gum/ox bile have been successf…
On the Derivatization of Drugs Using 1-Nitroso-2-naphthol, 4-aminoantipyrine and 2,6-Dihaloquinone Chlorimides
1992
Coupling of 1-nitroso-2-naphthol (1N2N), 4-aminoantipyrine (4-AAP), 2,6-dichloroquinone chlorimide (DCQC) and 2,6-dibromoquinone chlorimide (DBQC) with several bioactive substances, including adren...
Simple high-performance liquid chromatographic assay for polyamines and their monoacetyl derivatives.
1993
A rapid reversed-phase high-performance liquid chromatographic method, using pre-column derivatization with benzoyl chloride and ultraviolet detection at 254 nm, was developed for the simultaneous measurement of polyamines and their monoacetyl derivatives. Calibration curves were linear for concentrations from 1.25 to 25 nmol/ml. The method was employed to assay these compounds in chick embryo retina explants using organic solvent extraction and 1,7-diaminoheptane as an internal standard. This simple and sensitive method can be applied to routine determinations of these compounds in various biological samples.
Spectrofluorimetric determination of emetine by flow injection using barium peroxide and UV derivatization
1993
Abstract The flow-injection spectrofluorimetric determination of emetine was carried out by photoderivatization in the presence of barium peroxide, in a flow-injection assembly in which the PTFE tubing in the injection valve is helically coiled around the lamp. The sample solution merges with a barium peroxidephosphoric acid solution and then the resulting mixture is irradiated; pure distilled water is used as a carrier stream. The calibration graph is linear over the range 0.05–50 μ g ml −1 of emetine dihydrochloride. The influence of foreign compounds was studied and the method was applied to the determination of emetine in injection and human urine samples.
A new derivatization procedure for the determination of cephalexin with 1,2-naphthoquinone 4-sulphonate in pharmaceutical and urine samples using sol…
1998
Abstract The present report shows how to derivatize cephalexin with 1,2-naphthoquinone-4-sulphonate (NQS) into solid-phase extraction cartridges (C18) using UV–visible detection. Optimum conditions for this new procedure are: hydrogen carbonate/carbonate buffer pH=10.5, 5 min reaction time at 25°C and NQS concentration of 7.1×10−3 mol l−1. The accuracy and the precision of the method were tested. The procedure was used to measure cephalexin in pharmaceutical and urine samples. The results obtained were contrasted with those reported by UV-spectrophotometric and HPLC methods for pharmaceutical samples and with HPLC method for urine samples. The H-point standard additions method was used to m…