Search results for "MASS SPECTROMETRY"
showing 10 items of 2544 documents
Field desorption mass spectrometric characterization of thiol conjugates related to the oxidative metabolism of the anticancer drug 4′-(9-acridinylam…
1983
Conjugation products with glutathione (GSH) and other endogenous thiol derivatives related to the oxidative metabolism of the anticancer drug, 4′-(9-acridinlyamino) methanesulfon-m-anisidide (m-AMSA) were synthesized and characterized by field desorption mass spectrometry. The primary microsomal oxidation product of m-AMSA, m-AQDI, was prepared by MnO2 oxidation of the parent drug and reacted with equimolar GSH, cysteine, N-acetylcysteine and N-acetylcysteine methyl ester to form m-AMSA-(5′)-thiol conjugates linkedat the aniline ring, as major products. Field desorption mass spectra of the conjugates provided abundant [MH]plus; ions, and characteristic fragment ions by cleavage at the thioe…
Identification of conjugation and cleavage products in the thiolytic metabolism of the anticancer drug 4'-(9-acridinylamino)methanesulfon-m-anisidide.
1981
Conjugation and cleavage products in the thiolytic metabolism of the anticancer drug 4′ -(9-acridinyl amino)methanesulfon-m-anisidide were identified primarily by high-pressure liquid chromatography in combination with field desorption mass spectrometry. The spontaneous metabolic pathway of the drug, as related to its susceptibility to nucleophilic attack by endogenous thiols at the 9-carbon atom of the acridine moiety, has been studied. Among the metabolite fraction of 4′-(9-acridinylamino)methanesulfon-m-anisidide excreted in rat bile after administration of a therapeutic dose, a conjugate was identified as the 9-acridinyl thioether of glutathione. This conjugation product and the corresp…
Design and synthesis of new trehalose-conjugated pentapeptides as inhibitors of Aβ(1-42) fibrillogenesis and toxicity
2009
Aggregation of the amyloid A? peptide and its accumulation into insoluble deposits (plaques) are believed to be the main cause of neuronal dysfunction associated with Alzheimer's disease (AD); small molecules that can interfere with the A? amyloid fibril formation are therefore of interest for a potential therapeutic strategy. Three new trehalose-conjugated peptides of the well known ?-sheet breaker peptide iA?5p,were synthesized. The disaccharide was covalently attached to different sites of the LPFFD peptide chain, i.e. at the N-terminus, C-terminus or at the Asp side chain. CD spectroscopy in different solvents was used to assess changes in the peptide conformation of these compounds. Th…
Apparent content curves: description and analytical applications. Resolution of binary mixtures
1992
The apparent content curves and their analytical applications are described. Basing on these curves a mathematical method, which permits the identification of the interfering component present in a binary mixture as well as the determination of the contents of both constituents, is proposed. The existence of considerable interaction coefficients is not an impediment for its application. Besides, the analyte contents in the mixture can be obtained without the use of standard interference solutions. The proposed procedure is applied to the analysis of mixtures of dyes with overlapping absorption spectra.
Determination of trichothecenes and zearalenones in grain cereal, flour and bread by liquid chromatography tandem mass spectrometry
2012
Although analytical methods have been already reported for legislated mycotoxins as trichothecenes and zearalenone (ZON) separately, we describe the optimization of a simple and rapid multimycotoxin method for the determination of a total of 12 mycotoxins simultaneously, nine trichothecenes (NIV, DON, FUS-X, DAS, 15-AcDON, 3-AcDON, NEO, HT-2, T-2 T2), and zearalenone and its metabolites (ZON, a-ZOL, b-ZOL), of different origin (wheat, oat, barley and spelt) and in three different products where these substance can be present (grain, flour and bread) reach the food chain and cause toxic effect either in humans or animals. The extraction procedure was based on a mixture of acetonitrile/water …
Extraction and Sample Preparation
2015
As everyone knows, the role played by extraction and sample preparation in the analytical sciences cannot be overemphasized. Despite tremendous advances in chromatography, detection, and other aspects of analysis, extraction and sample preparation remain a preanalysis ritual of critical importance. It has been estimated that around 50% to 70% possibly even more of the time and effort that goes into an analytical process comprises extraction and sample preparation. Sample preparation procedure can vary in the degree of selectivity, speed, and convenience, depending on the approach and conditions used, as well as on the geometric configurations of the extraction phase and conditions. Proper d…
Synergistic combination of polyamide-coated paper-based sorptive phase for the extraction of antibiotics in saliva.
2021
Abstract The development of analytical methods that allow the simultaneous determination of a wide range of analytes with different properties is one of the focuses of attention in Analytical Chemistry. This work describes a proof-of-concept of the synergistic extraction of a planar paper-based sorptive phase modified with a polyamide such as nylon. This as-prepared sorptive phase enables the extraction of six penicillin-derived antibiotics of different polarity from human saliva samples in the same analysis, since the analytes either interact with the paper or with the nylon. The synthesis of the sorptive phase is simple as it only requires dipping the paper into an organic solution of the…
Analysis of four parabens and bisphenols A, F, S in urine, using dilute and shoot and liquid chromatography coupled to mass spectrometry
2018
Abstract A new strategy for the analysis of 4 parabens (methylparaben, ethyl paraben, propyl paraben and butyl paraben) and 3 bisphenols (A, F and S) in human urine has been developed. Dilute and shoot and liquid chromatography coupled to mass spectrometry (LC-MS/MS) determination was employed. Procedural matched calibration, certified materials and spiked samples were used for validation. The obtained recoveries varied between 85 and 104% with a precision lower than 20% for all analytes. The LOQ was 0.20 ng mL for all analytes. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for MS detection. The proposed method was successfully applied f…
Diffusion technique for the generation of gaseous halogen standards
2009
Abstract Halogens are known to play an important role in the tropospheric ozone-depletion chemistry and are of special interest because of their influence on the atmospheric oxidation capacity. In this paper, we investigate the application of a capillary diffusion technique for the generation of gaseous halogen standards like Br 2 , IBr, ICl and I 2 . The influence of capillary dimension (i.e. length and inner diameter), ambient pressure and headspace volume of the diffusion vessel on the test gas output has been evaluated. The experimental output rates are determined from the mass loss of the analyte vessel on a regular schedule and compared with their respective theoretical predictions. W…
Amphetamine-type stimulants analysis in oral fluid based on molecularly imprinting extraction
2018
Abstract A methamphetamine-based molecularly imprinted polymer (MIP) has been prepared by bulk polymerization to recognize new psychoactive substances (NPS) of the amphetamine, cathinones and 2C families in oral fluid samples, being the first precedent of a synthetized MIP for the extraction and preconcentration 32 NPS including amphetamine type substances and synthetic cathinones from oral fluids. Pre-polymerization complex and resulting materials were appropriately characterized by infrared spectroscopy, scanning electron microscopy, and nitrogen adsorption-desorption isotherms. Appropriateness of the material for the specific recognition of the target analytes was also evaluated through …