Total iodine in nutritional and biological reference materials using neutron activation analysis and inductively coupled plasma mass spectrometry

In a recent collaborative study intended to extend the variety of reference materials certified for iodine, three mineralization methods were developed to quantify the total iodine content of biological and nutritional materials by inductively coupled plasma mass spectrometry (ICP-MS). A mixture of water-soluble tertiary amines was used as the matrix solution for two oxygen combustion methods and for a simple extraction at room temperature. Calibrations with matrix-matched standards, internal calibration, and isotope dilution with ¹²⁹I were used. Good agreement between neutron activation analysis (NAA) and the two combustion methods was observed except for < 0.1 mg kg^–1 iodine concentrations. The amine extraction method gave the most reliable results for the mixed diet, milk powder, and infant formula samples but low recoveries for other biological materials owing to an incomplete extraction and solubilization of iodine. The NAA method, with its freedom from reagent blank, is a useful technique for the independent determination of iodine in biological, environmental and food matrices, especially for verification of iodine results obtained by ICP-MS. Received: 11 February 1998 / Revised: 21 April 1998 / Accepted: 16 June 1998