Search results for "Analytical"
showing 10 items of 9586 documents
Hybrid methacrylate monolithic columns containing magnetic nanoparticles for capillary electrochromatography
2015
Abstract Vinylized iron oxide magnetic nanoparticles (VMNPs) were incorporated into polymethacrylate monolithic columns to develop novel stationary phases with enhanced separation performance. The VMNPs were dispersed in a polymerization mixture containing gycidyl methacrylate and ethylene glycol dimethacrylate as monomers, cyclohexanol and 1-dodecanol as porogens and azobisisobutyronitrile as initiator. The stability of the VMNPs in the polymerization mixture was investigated at several VMNP contents. Using short UV-polymerization times, polymeric beds with homogenously dispersed VMNPs were obtained. The novel stationary phases were characterized by scanning electron microscopy. The chroma…
Capillary electrochromatography analysis of hormonal cyclic and linear peptides.
2001
The retention behavior of linear and cyclic peptides has been studied by capillary electrochromatography (CEC) with a variety of different n-alkyl silica reversed-phase sorbents and also with mixed-mode phases containing both strong cation-exchange (sulfonic acid) and n-alkyl groups bonded onto the silica surface, using eluents ranging from pH 2.0 to pH 5.0. Depending upon the amino acid sequence, electrochromatographic retention of the peptides was strongly affected by the composition of the eluent, its pH value, and the choice of sorbent packed into the capillaries. The dominant separation processes operating with these charged analytes could be modulated inter alia by the content of orga…
Study of peak shape and efficiency in butyl acrylate-based monolithic columns for capillary electrochromatography.
2009
Abstract The study and modelling peak shape of in capillary electrochromatography (CEC), obtained using butyl acrylate (BA)-based monolithic columns, is described in this article. A modified-Gaussian model, which is a function of conventional experimental parameters: retention time (tR), peak height (H0) and standard deviation (σ0) at the peak maximum, and left (A) and right (B) halfwidths, was used to describe the peaks of thiourea and several polyaromatic hydrocarbons compounds, which were eluted under several applied voltages. A mean relative error below 2% in the prediction of peak shape is obtained. Based on peak parameters, an easy and reliable estimation of global chromatographic per…
Methacrylate monolithic columns functionalized with epinephrine for capillary electrochromatography applications.
2013
Epinephrine-bonded polymeric monoliths for capillary electrochromatography (CEC) were developed by nucleophilic substitution reaction of epoxide groups of poly(glycidyl-methacrylate-co-ethylenedimethacrylate) (poly(GMA-co-EDMA)) monoliths using epinephrine as nucleophilic reagent. The ring opening reaction under dynamic conditions was optimized. Successful chemical modification of the monolith surface was ascertained by in situ Raman spectroscopy characterization. In addition, the amount of epinephrine groups that was bound to the monolith surface was evaluated by oxidation of the catechol groups with Ce(IV), followed by spectrophotometric measurement of unreacted Ce(IV). About 9% of all th…
‘Intrinsic’ profiles and capillary waves at interfaces between coexisting phases in polymer blends
2001
Abstract Lateral fluctuations in the local position of the center of the interface between coexisting phases in unmixed polymer blends lead to a broadening of interfacial widths; comparing self-consistent field predictions for the ‘intrinsic’ profile to simulations (or experiments), this ‘capillary wave’ broadening needs consideration. This problem has been studied by extensive Monte Carlo simulations of the bond fluctuation model for symmetrical polymer mixtures, both for free interfaces (between bulk phases) and for confined interfaces (in thin films between parallel walls). While the capillary wave predictions at large length scales are confirmed, the extraction of the ‘intrinsic’ profil…
Analysis of carbamate pesticides and their metabolites in water by solid phase extraction and liquid chromatography: A review
2001
Carbamates are an important, broad class of pesticides that are used extensively as insecticides, fungicides, and herbicides. Sensitive, economical, fast, and environmental friendly procedures are constantly developed to investigate their residues in water samples. The state of the art in methods based on solid phase extraction (SPE) and liquid chromatographic determination are examined here. SPE is presently the most extended method for preconcentration of carbamate pesticide residues and their transformation products from water samples. Advantages and limitations of alkyl bonded-silica, and polymeric sorbents, carbon, and mixed-phases in off-line and on-line procedures are discussed. Beca…
Synthesis of active principles from the leaves of Moringa oleifera using S-pent-4-enyl thioglycosides
1998
Abstract α - l -Rhamnosides of 4-hydroxy-benzyl compounds with nitrile, carbamate, and thiocarbamate groups occurring in Moringa oleifera leaf extracts and the α - l -rhamnoside of anisaldehyde derivatives were synthesised. Electrophilic activation of S -pent-4-enyl thiorhamnosides was applied for the construction of glycosidic linkages.
Evaluation of the Fate of Aldicarb and Its Metabolites in Oranges
1995
Abstract The accumulation, persistence and fate of systemic pesticide aldicarb was melencholy evaluated in orange crops. The concentration of this pesticide and its two toxic metabolites, aldicarb sulfoxide and aldicarb sulfone was determined in leaves, rind and pulp of three orange varieties (Satsuma, Navelina and Clemetina de Nules) and in the top soil of the orange groves. The groves were located in two different places in the Valencia Community (Spain). The analysis showed that the aldicarb concentration was lower than those of aldicarb sulfoxide and aldicarb sulfone. In all cases, the residues persisted at least 160 days in vegetable samples and between 157 and 227 days in soil samples…
A fast method for determining low-molecular-mass aliphatic carboxylic acids by high-performance liquid chromatography–atmospheric pressure chemical i…
2006
A fast quantitative high-performance liquid chromatographic separation method with atmospheric pressure chemical ionization mass spectrometric detection (HPLC-APCI-MS) was developed for the determination of low-molecular-mass aliphatic mono- and dicarboxylic acids typically present in different industrial process waters. A mixture of glycolic, lactic, a-glucoisosaccharinic, oxalic, maleic, fumaric, succinic, malic, glutaric, methylsuccinic, and adipic acids was separated using an RP chromatographic system. Adipic acid was used as an internal standard to calculate correlation coefficients for the acids studied. The chromatographic analysis of these acids was primarily carried out by means of…
Quantitative determination of the main aliphatic carboxylic acids in wood kraft black liquors by high-performance liquid chromatography-mass spectrom…
2006
The versatile characterization of organic material and especially of the significant aliphatic hydroxy acids in black liquor is of great importance, for example, in monitoring the progress of the kraft pulping process. This paper describes a simple high-performance liquid chromatographic separation method with atmospheric-pressure chemical ionization mass spectrometry (HPLC-APCI-MS) which was developed for the rapid quantitative analysis of these acids, mainly formed as the alkaline degradation products of feedstock carbohydrates. The fraction of carbohydrate degradation products is mainly composed of hydroxy monocarboxylic and volatile acids (formic and acetic acids) along with lesser amou…