Jj. Thompson, DETERMINATION OF ULTRATRACE LEVELS OF LEAD IN INFANT FORMULA BY ISOTOPE-DILUTION INDUCTIVELY-COUPLED PLASMA-MASS SPECTROMETRY, Journal of AOAC International, 76(6), 1993, pp. 1378-1384
A simple method was developed for the accurate and precise determinati
on of low- and sub-ppb (ng/g) concentrations of lead in infant formula
by isotope dilution inductively coupled plasma mass spectrometry usin
g ultrasonic nebulization. After addition of a known amount of Pb-207,
samples were microwave digested and the ratio Pb-207/Pb-208 was measu
red in the digests. Agreement with certified values for lead in milk p
owder standard reference materials was good, and isotope dilution anal
ysis using Pb-206 yielded identical results for the standard reference
materials. Lead concentrations determined for several infant nutritio
nal products were verified by an independent method. Typically, relati
ve standard deviations of <4% were obtained with this method for lead
concentrations above 2 ppb. The recovery of 2 ng of lead from an aqueo
us standard carried through the microwave digestion was 104 +/- 4%. In
fant formula (containing 0.6 ppb lead) to which 0.4 ng of natural-abun
dance lead had been added, to simulate a formula containing 0.9 ppb le
ad, was analyzed by isotope dilution, and the result was 96 +/- 18% of
the theoretical value. Thus, differences of 0.3 ppb lead could be cle
arly distinguished, and the detection limit was estimated to be 0.1 ng
lead per gram of infant formula. The keys to accuracy for this method
are minimizing contamination and accurately determining the concentra
tion of lead in the isotopically enriched standard.