0000000000522514
AUTHOR
J.r. Torres-lapasió
Micellar liquid chromatographic separation of amino acids using pre- and post-column o -phthalaldehyde/ N -acetylcysteine derivatization
Abstract The isocratic analysis of primary proteic amino acids using a C18 column, micellar mobile phases of sodium dodecyl sulphate (SDS) and 1-propanol at varying pH, and pre- and post-column formation of the o-phthalaldehyde (OPA)/N-acetyl- l -cysteine (NAC) isoindoles, is examined. An interpretive optimization strategy was applied to find the best separation conditions. For this purpose, empirical polynomial models were used to describe the elution behavior of the isoindoles and free amino acids, using as separation factors the concentrations of surfactant and modifier (two-factor problem), or these two factors and the pH of the mobile phase (three-factor problem). The separation of the…
Secondary Chemical Equilibria in Reversed-Phase Liquid Chromatography
The addition of reagents to an RPLC mobile phase enables the separation of ionizable compounds, inorganic anions, and metal ions using conventional instrumentation, silica-based materials, and hydro-organic mixtures, thanks to a variety of secondary equilibria. This gives rise to several chromatographic modes, whose main features are outlined in this chapter. The effect of the mobile phase pH on the retention of ionizable compounds is described, together with the recommended experimental practice. The mechanism of adsorption of amphiphilic anions or cations on the stationary phase to attract analytes with opposite charge or suppress the silanol activity is discussed. Different reagents, suc…
Complementary mobile-phase optimisation for resolution enhancement in high-performance liquid chromatography.
An optimisation methodology in high-performance liquid chromatography (HPLC) is presented for the selection of two or more mobile phases having an optimal complementary resolution. The complementary mobile phases (CMPs) are selected in such a way that each one resolves optimally only some compounds in the mixture, while the remainder, resolved by the other mobile phase(s), can overlap among them. The methodology is based on the computation of a peak purity measurement for each solute, using an asymmetrical peak model for peak simulation. Two global resolution criteria (product of elementary resolutions and worst elementary resolution) and two methods for solving the problem (a systematic ex…
Evaluation of several global resolution functions for liquid chromatography
Abstract An interpretative approach, that makes use of the overlapped fraction of each chromatographic peak as elementary resolution criterion, was applied to the separation of mixtures of compounds. The elementary resolution measurements for all peaks in the chromatogram were reduced to a single numerical value using several functions: normalised by the mean resolution product, unnormalised product, geometrical mean of the unnormalised product, and worst elementary resolution value. The descriptive capability of these reduction functions was evaluated through the observation of global resolution diagrams and the change in the shape of the chromatograms in the selected factor space. michrom…
Determination of fatty alcohol ethoxylates by derivatisation with maleic anhydride followed by liquid chromatography with UV-vis detection.
The esterification of fatty alcohol ethoxylates (FAEs) by melting with maleic anhydride has been studied in the presence of urea. The reaction rate and yield of non-ethoxylated and ethoxylated alcohols increase largely when grinded urea is suspended in the reaction medium, a 100% yield being achieved at 80 degrees C in 15 min. The procedure is tolerant to the presence of large amounts of water. The UV-vis response factors of the derivatives of individual FAE oligomers vary little with the number of carbon atoms in the alkyl chain, n, and the number of ethylene oxide units, m. Derivatised samples of industrial FAE mixtures, cleaning products and river and sea waters were chromatographed on a…