Separation of organoselenium compounds and their electrochemical detection

Ochsenkuhn-Petropoulou, Maria Th.; Tsopelas, Fotios N.
July 2004
Analytical & Bioanalytical Chemistry;Jul2004, Vol. 379 Issue 5/6, p770
Academic Journal
A simplified procedure based on ion-exchange separation of selenourea (Se-U) and selenocystamine (Se-CM), which have very close half-wave potential when they are simultaneously analyzed by voltammetric techniques, has been developed and optimized. Thus, selenocystamine remains in the cation exchanger Purolite C 100 H, whereas selenourea is found in the effluent and is determined by square wave cathodic stripping voltammetry using Na2CO3as electrolyte. Selenocystamine is then eluted from the cation exchanger using 4 M HCl and analyzed by square wave cathodic stripping voltammetry in the HCl solution. For each voltammetric determination the corresponding parameters were investigated and optimized; the obtained detection limits were 0.3 ng Se mL-1 for Se-CM and 2 ng Se mL-1 for Se-U. A flow sheet for the separation of inorganic (Se(IV) and Se(VI)) and organoselenium compounds (Se-U, Se-CM, (CH3)2Se2, and (CH3)2Se) developed for their electrochemical detection is presented and it was successfully applied to a certified reference material, an environmental soil sample, and a urine sample.


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