Jr. Turnlund et al., ISOTOPE RATIOS OF MOLYBDENUM DETERMINED BY THERMAL IONIZATION MASS-SPECTROMETRY FOR STABLE-ISOTOPE STUDIES OF MOLYBDENUM METABOLISM IN HUMANS, Analytical chemistry, 65(13), 1993, pp. 1717-1722
Methods were developed to separate and purify Mo from biological sampl
es and to measure isotopic ratios in 1 mug of Mo. A magnetic sector, t
hermal ionization mass spectrometer was used with simultaneous collect
ion of five isotopes. Isotopic ratios were corrected for mass fraction
ation by iterative normalization using the 96/98 ratio. Ion beam inten
sity was enhanced by using a double-filament configuration, loading sa
mples onto evaporation filaments with silica gel and boric acid. A tri
ple-isotope-dilution approach was used, so the method could be applied
to two-tracer studies of Mo metabolism in human subjects. Mo-94 was a
dded to samples prior to purification to quantify the total Mo content
of samples and to determine the amounts of enriched Mo-97 and Mo-100
appearing in urine and fecal samples of study participants. The three
ratios, 94/98, 97/98, and 100/98, were determined with within-run prec
ision of from 0.06 to 0.10% (RSD). Precision of the ratios between rep
licates was from 0.05 to 0.08%.