Isotope ratios of molybdenum determined by thermal ionization mass spectrometry for stable isotope studies of molybdenum metabolism in humans.

Methods were developed to separate and purify Mo from biological samples and to measure isotopic ratios in 1 microgram of Mo. A magnetic sector, thermal ionization mass spectrometer was used with simultaneous collection of five isotopes. Isotopic ratios were corrected for mass fractionation by iterative normalization using the 96/98 ratio. Ion beam intensity was enhanced by using a double-filament configuration, loading samples onto evaporation filaments with silica gel and boric acid. A triple-isotope-dilution approach was used, so the method could be applied to two-tracer studies of Mo metabolism in human subjects. 94Mo was added to samples prior to purification to quantify the total Mo content of samples and to determine the amounts of enriched 97Mo and 100Mo appearing in urine and fecal samples of study participants. The three ratios, 94/98, 97/98, and 100/98, were determined with within-run precision of from 0.06 to 0.10% (RSD). Precision of the ratios between replicates was from 0.05 to 0.08%.