Search results for "analytical"
showing 10 items of 9586 documents
Determination of the Herbicide Fluometuron by Photo‐induced Chemiluminescence in a Continuous‐flow Multicommutation Assembly
2007
Abstract This study was dealing with the chemiluminometric determination of the selective herbicide Fluometuron or 1,1‐dimethyl‐3‐(α,α,α‐trifluoro‐m‐tolyl)urea, (C10H11F3N2O) with a molecular weight 232.29 belongs to the phenyl urea herbicides family. The analytical strategy is based on the continuous‐flow manifold, multicommutation and the analyte pre‐treatment, the photo‐degradation. The optimization of chemical (pH, medium, temperature, and organized media) and hydrodynamic parameters (volume of reagents and flow rate) was performed by univariant and multiparametric simplex procedure respectively. Analytical figures of merit and the effect of foreign substances were studied. The method r…
Enhancement of retention predictions in reversed-phase liquid chromatography using reference compounds
2004
Abstract The use of reference compounds to correct errors associated with the preparation of mobile phase is studied, in order to enhance modelling of retention for optimisation purposes in reversed-phase liquid chromatography. The method fits individual retention models for a set of reference compounds, which are present in all injections. In second step, mobile-phase composition is corrected for each chromatogram, according to the fitted models of the reference compounds. The enhanced precision provided by the large number of replicates for the reference compounds is partially propagated to the retention models of the analytes. The approach is assayed in the separation of amino acids, aft…
Determination of trimethoprim by the linear absorbances method
1995
The determination of trimethoprim in the presence of dyphylline, proxyphylline, theophylline and caffeine by the linear absorbances method is described. Collinear couples of wavelengths, for the interfering dyphylline-proxyphylline-theophylline-caffeine system (in H2SO4, 0.05 mol/L), are provided in order to allow the determination of the analyte in the presence of these interfering substances.
Theoretical prediction of the native fluorescence of pharmaceuticals
2009
At present, to search fluorescent compounds or to increase the native fluorescence is an active research line specially and not only with analytical purposes. On some analytical areas and from the early times of applications of fluorescence (mid-fifties) the fluorimeter was defined as the suitable detector for determination of pharmaceuticals and subsequently, this detection mode has been widely applied. Therefore, it is mandatory to develop new strategies to discover or to enhance in a simple way the native fluorescence of organic compounds to increase the number of analytes to be determined by direct fluorescence. In the present paper are studied further applications of a new tool suitabl…
Chemometric determination of lipidic parameters in serum using ATR measurements of dry films of solvent extracts
2013
Attenuated total reflectance (ATR) infrared spectroscopy of dried organic extracts of serum samples has been evaluated as a fast method for the determination of triglycerides, cholesterol, high density lipoprotein (HDL) and low density lipoprotein (LDL). After careful selection of solvents based on green parameters, serum samples were extracted using hexane-isopropanol and ethyl acetate-ethanol mixtures. Microscopy studies and comparison with standard spectra were performed in order to investigate whether the proposed methodology is suitable for the quantification of lipids in serum samples. The results of these preliminary studies confirmed that the variations in the IR spectra of sample e…
Optimisation of gradient elution with serially-coupled columns. Part I: single linear gradients.
2014
A mixture of compounds often cannot be resolved with a single chromatographic column, but the analysis can be successful using columns of different nature, serially combined through zero-dead volume junctions. In previous work (JCA 1281 (2013) 94), we developed an isocratic approach that optimised simultaneously the mobile phase composition, stationary phase nature and column length. In this work, we take the challenge of implementing optimal linear gradients for serial columns to decrease the analysis time for compounds covering a wide polarity range. For this purpose, five ACE columns of different selectivity (three C18 columns of different characteristics, a cyano and a phenyl column) we…
Capillary electrokinetic fractionation mass spectrometry (CEkF/MS): Technology setup and application to metabolite fractionation from complex samples…
2014
Capillary electrokinetic fractionation (CEkF) is investigated as a new, simple, and robust approach for semipreparative and analytical sample analysis based on pKa -dependant pH-driven electrophoretic mobility. CEkF was optimized with contactless conductivity detection and conducted with 10 kV reverse voltage for 10 min, then coupled on/at-line to ESI/MS. We propose a semi-empirical model with 14 representative compounds based on the correlation between sample/medium pH regulating the partial charge, the electrokinetic loading of the capillary and intensity (I) of analytes. According to the model, an empirical function (I = f (pH)) could be derived to calculate the acid dissociation constan…
Preconcentration of aluminium by micellar-enhanced ultrafiltration
1993
Abstract Traces of aluminium were preconcentrated in water samples by forming a complex with lumogallion, and successfully accumulated in the micellar phase obtained from cationic or non-ionic surfactants and filtered through 10 000 molecular weight cut-off ultrafiltration membranes. Studies indicated that, at pH 5.9, with 1 X 10 −3 M lumogallion and 2 X 10 −2 M cetyltrimethylamonium bromide, quantitative retention of aluminium present at μg ml −1 concentration levels was achieved. A micellar-enhanced fluorimetric procedure was employed to analyse the permeate solutions, whereas nitrous oxide-acetylene flame atomic emission spectrometry was used to determine aluminium in the retentate. The …
H-Point Curve Isolation Method for Coupled Liquid Chromatography and UV−Visible Spectrophotometry
2000
The H-point curve isolation method (HPCIM) for the detection of unknown interferences in chromatography is proposed. The method allows one to estimate the UV-vis spectra of interfering species in a sample as well as to test the purity of the chromatographic peaks. Besides the detection of the unknown interferences in a sample, this method allows one to calculate the concentration of an analyte in the presence of unknown compounds. To illustrate the reliability of the proposed method, samples of diuretics and amphetamines have been analyzed by normal- and reversed-phase high-performance chromatography.
A chemometric study of the simultaneous determination of calcium and magnesium in natural waters
1999
A method for the simultaneous spectrophotometric determination of calcium and magnesium in mineral waters with an FIA system is tested. The method is based on the reaction between the analytes and arsenazo(III) at pH 8.5. The calculations of the amounts of both analytes in the samples are carried out with the H-point standard addition method (HPSAM) for ternary mixtures, and with a partial least squares (PLS) model after a proper variable selection. The results obtained for the determination of calcium were comparable using both methods. The employment of the HPSAM brings to our attention the influence of the calcium concentration in the sample to the development of the reaction between mag…