A capillary electrokinetic chromatography technique is described that employs neutral cyclodextrins (CDs) as a primary phase, transported with electroosmotic flow, and charged CDs as an electrophoretically mediated secondary phase. Neutral, hydrophobic solutes are separated on the basis of their differential distribution between these CD phases. The technique resembles micellar electrokinetic capillary chromatography (MECC) with regard to instrumentation and the fundamental relationships for resolution and capacity factor, which are influenced by the existence of a finite elution window. Conversely, the CD technique offers unique and beneficial characteristics when compared to MECC. Efficiency, selectivity, and system retention are evaluated on the basis of separations of polyaromatic hydrocarbons (PAHs). mciency is comparable to that of MECC (> lo5 platedm). The specificity associated with solute-CD inclusion complexation provides elution orders for PAHs that do not follow the hydrophobicity trends of MECC. Moreover, since the CD phases are largely noninteractive, complex CD systems can be used to enhance selectivity. Capacity factors can be altered in a convenient and predictable fashion simply by changing the CD phase ratio. The technique is rather robust with regard to the use of running buffers containing organic solvents; the effects or organic modifier and pH on system retention are demonstrated.
Polycyclic aromatic hydrocarbons (PAH) and a fullerene mixture (C60/C70) were separated with capillary columns (50 microns ID) packed with a reversed-phase packing (octadecylsilica, 3 microns diameter) using electrokinetic pumping. Nonaqueous (acetonitrile modified with methylene chloride or tetrahydrofuran, THF) mobile phases were used for these experiments. The effects of mobile phase composition on such factors as electroosmotic flow, plate height, and capacity factor (k') are reported. The less polar solvents methylene chloride and THF produced predictable reductions in k' when used to modify an acetonitrile mobile phase. Large amounts of the less polar modifiers (50% v/v) also resulted in a fourfold decrease in flow rate. This meant that even with a decrease in k', the retention time increased. Nonaqueous capillary electrokinetic chromatographic (CEC) separations gave efficiencies as high as 160,000 plates/m. Use of nonaqueous mobile phases provided small currents which in turn diminished the role of heating effects on efficiency. The nonaqueous system also provided greater solubility for the hydrophobic solutes. A Van Deemter plot for an acetonitrile mobile phase was obtained that exhibited expected trends in plate height with flow rate and k'. Solvent rinses with water and THF are shown to have only small effects on retention and flow rate.
The crude ethanol extract from the leaves of Dendropanax arboreus (Araliaceae) from Monteverde, Costa Rica, exhibits cytotoxic activity against Hep-G2, A-431, H-4IIE, and L-1210 tumor cell lines, but is not toxic against normal hepatocytes. The active component has been isolated by activity-directed separation and identified by 1H- and 13C-NMR spectroscopy as the acetylenic compound cis-1,9,16-heptadecatriene-4,6-diyne-3,8-diol.
Since its advent, capillary electrophoresis (CE) has been used to solve many chemical separation problems. Isolation and identification of components in samples ranging from human cells to shale oil have been achieved using CE.A wide variety of applications of CE have appeared in the literature. Many of these applications are presented in this article so as to demonstrate the power and versatility of CE. Separations of ionizable species including numerous small anions, proteins, and biopolymers are presented. Packed capillary and affinity CE methods are also discussed. Examples of the selectivity and resolving power of additives such as micelles and cyclodextrins are provided. Finally, the "future" of CE, including a examples of "CE on a chip," is discussed.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.