0000000000006245
AUTHOR
R. D. Caballero
Peak deconvolution in one-dimensional chromatography using a two-way data approach.
A deconvolution methodology for overlapped chromatographic signals is proposed. Several single-wavelength chromatograms of binary mixtures, obtained in different runs at diverse concentration ratios of the individual components, were simultaneously processed (multi-batch approach), after being arranged as two-way data. The chromatograms were modelled as linear combinations of forced peak profiles according to a polynomially modified Gaussian equation. The fitting was performed with a previously reported hybrid genetic algorithm with local search, leaving all model parameters free. The approach yielded more accurate solutions than those found when each experimental chromatogram was fitted in…
RAPID LIQUID CHROMATOGRAPHIC DETERMINATION OF TETRACYCLINES IN ANIMAL FEEDS USING A SURFACTANT SOLUTION AS MOBILE PHASE
ABSTRACT A chromatographic procedure was developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), doxycycline (DC) and minocycline (MINO) in animal feeds. Clear analyte-rich extracts were obtained using a 1 : 1 acetonitrile/water mixture buffered at pH 3. The extracts were injected into a conventional unprotected C18 chromatographic column and eluted with a mobile phase of 0.05 M sodium dodecyl sulfate/5% 1-butanol/0.01 M oxalic acid at pH 3. Good resolution was achieved for the five compounds, whereas OTC and TC coeluted with an optimized aqueous-organic mobile phase of methanol/acetonitrile/0.01 M oxalic acid at pH 3. Mean recoveries from spike…
Micellar liquid chromatography: suitable technique for screening analysis.
The screening capability of micellar liquid chromatography (MLC) is discussed using the reported chromatographic data of several sets of compounds (amino acids, beta-blockers, diuretics, phenethylamines, phenols, polynuclear aromatic hydrocarbons, steroids and sulfonamides) and new results (sulfonamides and steroids). The chromatographic data are treated with an interpretive optimisation resolution procedure to obtain the best separation conditions. Usually, the pH and the concentration of surfactant (sodium dodecyl sulfate, SDS, or cetyltrimethylammonium bromide) for the optimal mobile phase were 2.5-3 and0.12 M, respectively. The nature and concentration of organic solvent depended on the…
MICELLAR CHROMATOGRAPHIC PROCEDURE WITH DIRECT INJECTION FOR THE DETERMINATION OF SULFONAMIDES IN MILK AND HONEY SAMPLES
The capability of liquid chromatography with micellar mobile phases of sodium dodecyl sulfate (SDS), of allowing the direct injection of biological fluids into reversed-phase columns, was applied to the determination of sulfonamides in milk and honey samples. The chromatographic behavior of a group of 15 sulfonamides was studied at pH 3.0 where the drugs showed a greater separation space. Acetonitrile was added to the mobile phase to decrease the retention of the most hydrophobic drugs and increase the efficiencies, which yielded a higher resolution. The samples were diluted with 0.10 M SDS to facilitate the solubilization of the matrix compounds and release the protein-bound drugs. The pro…
SINGLE-PEAK RESOLUTION CRITERIA FOR OPTIMIZATION OF MOBILE PHASE COMPOSITION IN LIQUID CHROMATOGRAPHY
Three criteria that evaluate the single peak resolution (peak purity) in chromatography, the free height fraction, free area fraction, and valley ratio, are examined. The main advantages of these criteria against other criteria based on peak pair separation, are that the measurements are not affected by the identity of neighboring peaks and are normalized, which make them very intuitive. The methodology is illustrated through the isocratic separation of mixtures of several sulphonamides (sulphacetamide, sulphadiazine, sulphadimethoxine, sulphaguanidine, sulphamerazine, sulphamethazine, sulphamethoxazole, sulphamethizole, sulphamonomethoxine, sulphanilamide, sulphapyridine, sulphaquinoxaline…
Parabolic-Lorentzian modified Gaussian model for describing and deconvolving chromatographic peaks.
Abstract A new mathematical model for characterising skewed chromatographic peaks, which improves the previously reported polynomially modified Gaussian (PMG) model, is proposed. The model is a Gaussian based equation whose variance is a combined parabolic-Lorentzian function. The parabola accounts for the non-Gaussian shaped peak, whereas the Lorentzian function cancels the variance growth out of the elution region, which gives rise to a problematic baseline increase in the PMG model. The proposed parabolic-Lorentzian modified Gaussian (PLMG) model makes a correct description of peaks showing a wide range of asymmetry with positive and/or negative skewness. The new model is shown to give b…
HYDRO-ORGANIC AND MICELLAR-ORGANIC REVERSED-PHASE LIQUID CHROMATOGRAPHIC PROCEDURES FOR THE EVALUATION OF SULPHONAMIDES IN PHARMACEUTICALS
Two reversed-phase liquid chromatographic procedures were developed for the analysis of ten pharmaceutical formulations used in medicine and veterinary, which contained one of the following sulphonamides: sulphacetamide, sulphadiazine, sulphaguanidine, sulphamethazine, sulphamethizole, sulphamethoxazole, or sulphathiazole. In both chromatographic modes, the same C18 column was utilized and the mobile phase contained a low amount of acetonitrile and citric buffer at pH 3.0. In one of the procedures, the surfactant sodium dodecyl sul phate was added to the mobile phase. The presence of micelles allowed a decrease in the amount of organic solvent from 11% to 6%, and facilitated sample dissolut…