Study of enantioseparation of ß-blockers using amylose tris(3-chloro-5-methylphenylcarbamate) as chiral stationary phase under polar-organic, reversed-phase and hydrophilic interaction liquid chromatography conditions.

In this study, we describe the experimental variables influencing enantioseparation of twelve ß-blockers when analyzed under polar-organic, reversed-phase and hydrophilic interaction liquid chromatography conditions on a column with immobilized amylose tris(3-chloro-5-methylphenylcarbamate) as chiral stationary phase. Regarding polar-organic mode, two component mobile phases consisting of methanol, ethanol or acetonitrile with the addition of basic additives such as diethylamine, triethylamine, mono-ethanolamine, ethylendiamine or trifluoroacetic acid/diethylamine mixture were evaluated. Studies of retention at different temperatures were also performed. In reversed-phase mode, mixtures consisting of methanol or acetonitrile with either aqueous boric acid-borate buffer or sodium hydrogen carbonate-carbonate buffer solutions were compared aiming to study the influence of organic modifier as well as buffer type and pH on resolution. In addition, a systematic evaluation of the retention factors of ß-blockers enantiomers in hydro-organic eluents containing acetonitrile in presence of diethylamine as additive was carried out by increasing progressively the water content, in order to check for retention dependencies indicative of the interplay of both hydrophilic interaction liquid chromatography and reversed-phase modes.

Chiral separation of several pesticides on an immobilized amylose tris(3-chloro-5-methylphenylcarbamate) column under polar-organic conditions. Influence of mobile phase and temperature on enantioselectivity.

In this work, the use of different solvents and temperatures was explored, aiming to evaluate their influence on the enantioseparation of pesticides by HPLC in polar-organic conditions, employing a column containing immobilized amylose tris(3-chloro-5-methylphenyl-carbamate). The chiral separation of seventeen different pesticides widely used as herbicides, fungicides, insecticides and precursors were studied. The mobile phases included methanol, ethanol, iso-propanol, n-propanol and acetonitrile; either pure or containing additives such as diethylamine, trifluoroacetic acid, formic acid, acetic acid or mixtures thereof. We studied the influence of these eluents on chiral separation of those pesticides in terms of retention factor, enantioselectivity, enantioresolution and peak symmetry. Regarding temperature influence, evaluated within the range 5 - 40 °C, nearly all the compounds decreased their retention and selectivity factors with the increase in temperature, although the effect was dependent on the mobile phase solvent. Moreover, estimation of thermodynamic parameters was performed based on linear van´t Hoff plots.