Search results for "Analytical"
showing 10 items of 9586 documents
Simultaneous determination of C1−C8 n-alkyl acetates and corresponding mono-, di- and trichloroacetates on glass capillary columns with programmed te…
1982
Gas chromatography of mixtures of aliphaticn-alkyl acetates (CH3−COOR), chloroacetates (CHCl2−COOR), dichloroacetates (CHCl2−COOR) and trichloroacetates (CCl3−COOR), where the alcohol chain length (R) varied between 1 and 8, has been studied on SE-30, Carbowax 20M and OV-351 glass capillary columns with programmed temperatures from 50°C at 2, 4, 6, 8 and 10°C/min. Compounds in the homologous series are eluted in the direct order from methyl ton-octyl acetate. The isomeric chloro esters are eluted on SE-30 according to their boiling points in the order: mono-, di- and trichloro isomer, whereas on polar columns di- and trichloro esters are eluted in the reverse order. The complete separation …
Influence of the presence of surfactants and humic acid in waters on the indophenol-type reaction method for ammonium determination.
2005
Abstract This work has evaluated the influence of humic acid and/or surfactants in the quantification of ammonium in waters with the indophenol-type reaction method. Thymol has been employed with the colorimetric method for sample ammonium concentrations between 0.25 and 1 mg L −1 . In addition, SPE/diffuse reflectance method has been used for quantification of ammonium at low concentrations (between 0.025 and 0.25 mg L −1 ). Matrix effect owing to humic substances were observed with the colorimetric method when the concentration was equal or higher than 25 mg L −1 . Lower concentrations of humic compounds produced matrix effects with the more sensitive SPE/diffuse reflectance method. Gener…
Enzyme-assisted extraction of proteins from Citrus fruits and prediction of their cultivar using protein profiles obtained by capillary gel electroph…
2017
Abstract The suitability of protein profiles established by capillary gel electrophoresis (CGE) as a tool to discriminate between 11 cultivars of Citrus (orange and tangerine) peel and pulp was evaluated in this work. Before CGE analysis, different extraction buffers (which included enzyme-assisted treatments) were compared. The best results were achieved using 5% ( v/v ) Celluclast ® 1.5 L and 5% ( v/v ) Palatase ® 20,000 L buffers for Citrus peel and pulp protein extracts, respectively. The resulting protein profiles obtained were used to construct linear discriminant analysis (LDA) models able to distinguish Citrus peel and pulp samples according to their cultivar. In both cases, all sam…
Analytical study of proteinaceous binding media in works of art by gas chromatography using alkyl chloroformates as derivatising agents.
2001
In this work, we present the results obtained in an analytical study of the different types of proteinaceous binding media most commonly used in paintings, using GC-FID as the technique of analysis and GC-MS as a confirmatory technique. The application of this methodology requires prior hydrolysis of the proteins in the binding media to obtain free amino acids and then volatile derivatives, in this case by reaction with chloroformates due to advantages of speed, safety and the aqueous medium in which the reaction occurs. The method proposed for the proteinaceous binding media study is to calculate the proportions of the different amino acids with respect to alanine. This method provided goo…
Selective protein removal and desalting using microchip CE.
2006
Abstract This paper describes the on-line sample pretreatment and analysis of proteins and peptides with a poly(methylmethacrylate) (PMMA) microfluidic device (IonChip™). This chip consists of two hyphenated electrophoresis channels with integrated conductivity detectors. The first channel can be used for sample preconcentration and sample clean-up, while in the second channel the selected compounds are separated. Isotachophoresis (ITP) combined with zone electrophoresis (CZE) was used to preconcentrate a myoglobin sample by a factor of about 65 before injection into the second dimension and to desalt a mixture of six proteins with 100 mM NaCl. However, ITP–CZE could not be used for the rem…
Chromatographic Determination of Thiols After Pre‐column Derivatization witho‐Phthalaldehyde and Isoleucine
2004
Abstract The reaction of primary amines with excess o‐phthalaldehyde (OPA) and thiol yields unique isoindole derivatives that are readily separated by reversed‐phase liquid chromatography. In a previous work, a spectrophotometric procedure was proposed for the assay of N‐acetylcysteine by derivatization with OPA and isoleucine at pH 9.5, with satisfactory results. The chromatographic determination of this and other low molecular‐weight thiols, after isoindole formation with isoleucine, using mobile phases of acetonitrile–water at pH 3 and spectrophotometric detection, is now examined. From the assayed thiols (thioglycolic acid, 3‐mercaptopropionic acid, tiopronin, N‐acetylcysteine, N‐acetyl…
Size‐Exclusion Chromatography in Single and Mixed Eluents: Effects of Sorption of Solvent and Polymer Solutes on Novel TSK‐Gel Super AW Columns
2005
Abstract The novel TSK Gel Super AW column packing is based on a polymeric gel with residual hydrophobic and hydrophilic groups on the gel surface. These groups can act as active sites making the chromatographic support compatible both with polar and apolar eluents. This interesting property allows the elution of systems of very different polarities but also induces binary polymer–gel, polymer–solvent, and solvent–gel enthalpic interactions that lead to a mixture of separation mechanisms: repulsion, partition, or adsorption besides the main size‐exclusion chromatography (SEC) mechanism. For this reason, the elution behaviour of many and diverse polymer/solvent systems has been studied in th…
Influence of the pH on the behavior of an imprinted polymeric stationary phase--supporting evidence for a binding site model.
2001
The equilibrium isotherms of the two enantiomers of phenylalanine anilide (PA) were measured by conventional frontal analysis at three different pH on a thermally-treated imprinted stationary phase selective for the L enantiomer. The first of these pH (buffer pH=3.0, pH(app)=4.0) is well below the apparent pKa (6.4) of the two solutes, the second (buffer pH=5.8, pH(app)=7.0) slightly below this pKa, and the third (buffer pH=7.0, pH(app)=8.3) well above it. The experimental data were fitted to several isotherm models. The best estimates of the parameters of these models are reported and discussed. The corresponding isotherms are compared with the experimental ones. The contributions of the e…
Influence of Thermal Annealing on the Thermodynamic and Mass-Transfer Kinetic Properties of d- and l-Phenylalanine Anilide on Imprinted Polymeric Sta…
1999
An investigation of the material, chromatographic, thermodynamic, and kinetic properties of thermally treated (i.e., annealed) polymeric stationary phases imprinted with l-phenylalanine anilide (l-PA) was carried out. The imprinting procedure of the solid phase used in this study was the same as for the untreated imprinted stationary phase studied previously. However, after polymerization, these new stationary phases were treated at elevated temperatures (50, 120, 140, and 160 °C) for 24 h. The treatment at 120 and 140 °C led to a larger decrease in the retention of l-PA than that of d-PA. The polymer treated at 160 °C could no longer resolve the d,l-PA racemate. The heat treatments were ac…
Sensory and Chemical Analysis of Fractions Obtained by Gel Permeation of Water-Soluble Comte Cheese Extracts
1995
The pure water extraction of Comte cheese solubles and their chromatographic separation facilitate sensory analysis experiments with the fractions directly collected from the column. Two extracts, one obtained after ultrafiltration, the other after chromatography on Sephadex G25, have been separated on Toyopearl HW-40S. The sensory evaluation of the obtained fractions shows in the two cases that some fractions have interesting flavors. However, physicochemical analysis shows that organoleptic characteristics are linked more to the presence of amino acids and salts than to the presence of peptides. Apart from monosodium glutamate, most of the amino acids are present in the fractions at conce…