DETERMINATION OF 5 SELENIUM-COMPOUNDS IN URINE BY LIQUID-CHROMATOGRAPHY WITH FOCUSED MICROWAVE-ASSISTED DIGESTION AND HYDRIDE GENERATION-ATOMIC ABSORPTION SPECTROMETRIC DETECTION

A method is proposed for the determination of trimethylselenonium ion, selenomethionine, selenocystine, selenite and selenate in urine, foll owing clean-up with C-18 cartridges. The on-line system developed cons ists of an anion-exchange chromatographic column for species separatio n, a focused microwave oven for the oxidation of organic Se species in the presence of 3% K2S2O8 and 3% NaOH solution and reduction of selen ate to selenite in 10 mol l(-1) HCl, a hydride generation system for t he conversion of selenite to selenium hydride and finally an atomic ab sorption spectrometer detector. Optimum chromatographic conditions wer e obtained in a Hamilton PRP-X100 column, using 100 mmol l(-1) phospha te buffer (pH=6.8) as the mobile phase. Detection limits were between 3 and 8 mu g l(-1). The relative standard deviation was <7% at 100 mu g l(-1) Se. The short-term stability test of the studied Se species in urine shows after 5 h of storage about 30% and 60% losses of selenite and SeCys, respectively. After taking pills containing Se about 60% o f the Se ingested is excreted in the first 12 h. Se(VI) ingested is pa rtially excreted as Se(VI) and partially transformed and excreted as a species that behaves as SeCys. SeMet is metabolised and excreted as s pecies that behave as Se(VI) and SeCys. (C) 1998 Elsevier Science B.V. All rights reserved.