A separation method is described for rapidly removing zinc from interfering matrix components, such as chloride, from digested biological samples prior to measurement of zinc stable isotopes by ICP-MS. The method employs chelation of the zinc with trifluoroacetylacetone (TFA), extraction of the chelate with hexane, destruction of the chelate and dissolution of the zinc into nitric acid for determintion. Complete separation of the zinc from matrix salts is achieved, and the method does not employ chlorinated hydrocarbon solvents as used in earlier, similar schemes. Cerium from borosilicate glass tubes used in sample digestion was found to be a potential problem when measuring ⁷⁰Zn, owing to the presence of ¹⁴⁰Ce²⁺. This potential problem can be avoided by using quartz digestion tubes and/or correcting for any cerium by monitoring m/z 140. Accuracy was verified by an independent method, and examples of the use of stable isotopes of zinc as metabolic tracers in human metabolism are given. The detection limit for the ID method (3s of blank) was 0.7 µg Zn. An in-house urine pool was found to contain 1.18 ± 0.005 µg g^–1 of Zn (n= 3) by ID and 1.17 ± 0.006 µg g^–1 of Zn (n= 3) by AAS.