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A method is described for the fractionation and estimation of iodine-containing constituents in the plasma, by means of preferential precipitation and elution. The plasma of 11 normal subjects and 22 patients suffering from thyrotoxicosis was analysed. Two significant findings emerged, namely, the presence of iodinated tyrosines and a decrease in the level of plasma inorganic iodide in thyrotoxicosis. The factors determining the concentration of plasma inorganic iodide are discussed.