Focusing of alkali earth metals in ligand step gradient

A capillary electroseparation technique for focusing and selective pre-concentration of metal chelates with subsequent on-line isotachophoresis (ITP) analysis was developed and verified. The ions of alkali earth metals (Mg, Ca, Sr, and Ba) were pre-concentrated from the mixture and analyzed. The focusing of the metals was carried out in a ligand step gradient, which was created by the addition of a convenient ligand agent to the regular stationary pH step gradient. The analytical procedure consisted of three steps. During the first step, the metal ions were electrokinetically continuously dosed into the column where they were selectively trapped on the stationary ligand step gradient in the form of unmoving zones of chelate complexes with effectively zero charge. After a detectable amount of analyte was accumulated, the dosing was stopped. The accumulated zones were mobilized to the analytical column, where they were analyzed by the ITP method with conductivity or photometric detection. The proper electrolyte systems for dosing, mobilizing, and analyzing in isoelectric focusing (IEF), moving boundary electrophoresis (MBE), and ITP modes were consequently developed and put into practice. The trapping selectivity can be regulated by the choice of pH and convenient complexing agents. A mixture of alkali earth metals were used as model analytes. Using a 3000 s dosing time, the proposed method improved the detection limit by 5–29 times in comparison to analysis by ITP with classical injection.