Search results for "Deriva"
showing 10 items of 1423 documents
Derivatization techniques for automated chromatographic analysis of amphetamine usingo-phthaldialdehyde: A comparative study
2000
The potential of different chromatographic systems for automated, on-line analysis of amphetamine in biological fluids is illustrated. The various systems integrate analyte purification and enrichment, separation, derivatization in different derivatization modes witho-phthaldialdehyde (OPA) and N-acetyl-L-cysteine (NAC), and fluorimetric detection. The reliability of the systems has been tested by analysing urine and plasma samples containing amphetamine in the 0.1–20.0 μg mL−1 range. Pre, on and post-column derivatization strategies are compared in terms of their instrumental requirements, selectivity, sensitivity, linearity and reproducibility.
Determination of sulphonamides in human urine by azo dye precolumn derivatization and micellar liquid chromatography
1995
Abstract A high-performance liquid chromatographic method for the determination of sulphonamides in urine is reported. The drugs (sulphadiazine, sulphaguanidine, sulphamethizole, sulphamethoxazole, and sulphathiazole) were diazotized with nitrite and coupled with N-(1-naphthyl)ethylenediamine dihydrochloride in a sodium dodecyl sulphate (SDS) micellar medium. Separation of the sulphonamide azo dyes was performed on a C18 column with a 0.05 M SDS-2.4% pentanol mobile phase, which permitted the direct injection of the urine samples. The limits of detection were in the 0.1–0.3 μg/ml range.
Derivative Fourier transform infrared spectrometric determination of ethanol in alcoholic beverages
1994
Abstract A derivative Fourier transform infrared (FT-TR) spectrometric procedure was developed for the direct determination of ethanol in alcoholic beverages, from beers to spirit samples. The method is based on first-order derivative FT-IR measurements between the peak at 1052 cm −1 and the valley at 1040 cm −1 , which are present in aqueous solutions and alcoholic beverages, by using a micro flow transmittance cell with ZnSe windows and a spacer of 0.029 mm. The method involves the accumulation of ten scans and provides accurate results in the determination of ethanol in alcoholic beverages without requiring any previous chemical treatment of the sample or a previous separation or extract…
Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples
2005
An accurate and sensitive species-specific isotope dilution GC/ICPMS method was developed for the determination of trimethyllead (Me3Pb+) in biological and environmental samples. A trimethyllead spike was synthesized from 206Pb-enriched metallic lead by reaction of lead halide with methyllithium and subsequent formation of trimethyllead iodide. The isotopic composition of the spike solution was determined by GC/ICPMS after derivatization with tetraethylborate, and its concentration was determined by reverse isotope dilution analysis. The species-specific GC/ICP-IDMS method was validated by reference material CRM 605 (urban dust) certified for Me3Pb+. The method was also applied to determine…
Comparative study of the determination of trimethylamine in water and air by combining liquid chromatography and solid-phase microextraction with on-…
2005
This work describes a new approach for the determination of trimethylamine (TMA) in water and air by liquid chromatography (LC). The assay is based on the employment of a solid-phase microextraction (SPME) fiber for sampling and for derivatization of the analyte with the fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC). The fiber, with a Carbowax-templated resin -50mum coating, was first immersed into a solution of the reagent. Once loaded with the reagent, the fiber was immersed into the water samples or exposed to the air samples in order to extract and to derivatize the analyte. Finally, the fiber was placed into a HPLC-SPME interface to desorb and transfer the TMA-FMOC derivat…
Determination of sertraline in rat plasma by HPLC and fluorescence detection and its application toin vivopharmacokinetic studies
2012
A simple, rapid, and sensitive HPLC method based on 9H-fluoren-9-ylmethyl chloroformate derivatization for the quantification of sertraline in rat plasma has been developed, requiring a plasma sample of only 0.1 mL, which was deproteinized and derivatized for 5 min in two single steps. The obtained derivative was stable at room temperature and was determined by HPLC using a fluorescence detector. The analytical column was a C(18) column and the mobile phase was acetonitrile and water (80:20, v/v). Calibration curves were linear in the range of 10-500 ng/mL. The limit of detection was approximately 3 ng/mL, and the lower limit of quantification was established at 10 ng/mL. The bias of the me…
Immunoassays for pyraclostrobin analysis in processed food products using novel monoclonal antibodies and QuEChERS-based extracts
2013
Strobilurins are a family of synthetic natural-derived pesticides widely used for fungi control in many crops. As part of a larger research project, a collection of monoclonal antibodies to one of the most relevant strobilurins, i.e. pyraclostrobin, has been generated using functionalized haptens with the spacer arm located at different sites. The toxophore aliphatic moiety, as observed with other strobilurins, and the planar aromatic two-ring system characteristic of this molecule were revealed as the best tethering sites for high-affinity monoclonal antibody production. A central derivatization position did not generate a good immune response, but such derivatives were useful as heterolog…
Analytic first and second derivatives for the CCSDT-n (n = 1–3) models: a first step towards the efficient calculation of CCSDT properties
2000
Analytic first and second derivatives of the energy are implemented for closed-shell systems described by the CCSDT-n (n=1, 1b, 2 and 3) and CC3 electron correlation models. A detailed discussion of the computational requirements of these calculations is given, along with diagrammatic formulas for all relevant quantities. The method is applied to calculate the nuclear magnetic shielding of H2O, CO and N2O and the structure and properties of propadienylidene.
Diastereoselective Synthesis of Dialkylated Bis(phosphino)ferrocenes: Their Use in Promoting Silver-Mediated Nucleophilic Fluorination of Chloroquino…
2017
International audience; The diastereoselective synthesis of dialkylated ferrocenyl bis(phosphane)s bearing aryl, alkyl, and hetero- or polycyclic substituents on the phosphino groups is reported, together with their characterization in the solid state by X-ray structure analysis and in solution by multinuclear NMR spectroscopy. Introduction of various alkyl groups on the ferrocene backbone, namely, tert-butyl, isopropyl, and trimethylsilyl, has a significant influence on the stereoselectivity of the ensuing lithiation/phosphination reactions. Only the introduction of the tert-butyl groups ensures both a high yield and perfect diastereoselectivity, which leads to the exclusive formation of t…
The pyrrole moiety as a template for COX-1/COX-2 inhibitors
2000
Aroyl- and thiophene-substituted pyrrole derivatives have been synthesized as a new class of COX-1/COX-2 inhibitors. The inhibition of COX-1 was evaluated in a biological system using bovine PMNLs as the enzyme source, whereas LPS-stimulated human monocytes served as the enzyme source for inducible COX-2. The determination of the concentration of arachidonic acid metabolites was performed by HPLC for COX-1 and RIA for COX-2. Variation of the substitution pattern led to a series of active compounds which showed inhibition for COX-1 and COX-2. Structural requirements for the development of COX-1/COX-2 inhibitors are discussed.