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Metals perform many functions inside organisms to sustain life.These metals are generally present in very small amounts,requiring high sensitivity determinations.To diagnose a congenital metal metabolic disorder,in particular,it is necessary to differentiate between free metals and those combined with proteins.We introduce an LC-ICP/MS method using a new size exclusion chromatography (SEC) mode column to fulfill that specific requirement.We have developed a new SEC micro column (I.D.: 0.3-1 mm) to ensure high-sensitivity determination.Using ICP/MS analysis with this new column,we were able to determine,with high sensitivity,trace amounts of metals in organisms.We explain methods for determining selenoamino acids (derivatives of essential amino acids) and Cu-metallothionein that relates to a congenital metabolic disorder.