DETERMINATION OF TELLURIUM IN URINE BY ISOTOPE-DILUTION GAS-CHROMATOGRAPHY MASS-SPECTROMETRY USING (4-FLUOROPHENYL)MAGNESIUM BROMIDE AS A DERIVATIZING AGENT AND A COMPARISON WITH ELECTROTHERMAL ATOMIC-ABSORPTION SPECTROMETRY

The antitumor drug AS-101 [ammoniumtrichloro(dioxoethylene-O,O')tellurate(IV)] is the first tellurium-containing compound that has been identified as possessing immunomodulating properties and minimal toxicity. We have developed a stable isotope dilution gas chromatography/mass spectrometry method using Te-120 as an internal standard and (4-fluorophenyl)magnesium bromide as a derivatizing agent for Te determination in urine. The urine samples were digested using HNO3 + H2O2 prior to derivatization with lithium bis-(trifluoroethyl)dithiocarbamate at a pH of 3. The trifluoro-diethyldithiocarbamate of tellurium was reacted with the Grignard reagent in anhydrous diethyl ether to obtain Te(FC6H4)(2) for GC/MS analysis. All isotope ratio measurements were made by selected ion monitoring with a Finnigan MAT 8230 organic mass spectrometer using a 10-m fused silica capillary column. Overall percision values for the five major Te isotopes relative to Te-130 were 0.6-3.1% when 10-ng samples of chelated Te were analyzed. No appreciable memory or carry-over effect was observed when two synthetic mixtures differing in Te-120:Te-130 ratios by a factor of 50 were sequentially analyzed. The isotope dilution GC/MS method was validated by determining Te in urine samples and comparing the values with electrothermal atomic absorption spectrometry. Te concentrations were determined in the 100-500 mu g/L range with CVs of 1-4%.