Determination of lead, cadmium, zinc, copper, and iron in foods by atomic absorption spectrometry after microwave digestion: NMKL Collaborative Study.

A method for determination of lead, cadmium, zinc, copper, and iron by atomic absorption spectrometry (AAS) after microwave digestion was subjected to a collaborative study in which 16 laboratories participated [including users of inductively coupled plasma (ICP) and ICP-mass spectrometry (MS)]. The types of samples included in the study were minced fish, wheat bran, milk powder, bovine and pig liver, mushroom, 2 simulated diets, and bovine muscle; the last 4 were certified reference materials. These were analyzed as single (4 samples), double blind (1 sample), or split level (2 samples) samples. Before the collaborative study, a pretrial was conducted in which 4 ready-made solutions and one fish tissue sample were analyzed for Pb and Cu. The reproducibility relative standard deviation (RSD R ) values, for results above the detection limit, ranged from 59% at 0.155 mglkg to 16% at 1.62 mglkg for Pb, from 28% at 0.0124 mg/kg to 11 % at 0.482 mglkg for Cd, from 9.3% at 35.3 mg/kg to 1.7% at 147 mglkg for Zn, from 39% at 0.241 mglkg to 3.0% at 63.4 mglkg for Cu, and from 17% at 7.4 mglkg to 5.9% at 303 mglkg for Fe. The RSD R values agreed well with the norms described by the International Union of Pure and Applied Chemistry. As a complement to the AAS determinations, a number of laboratories analyzed the samples either by ICP or by ICP-MS. The results of these analyses agreed well with the AAS results. On the basis of the results of the collaborative study, the method was adopted Official First Action by AOAC INTERNATIONAL.