Abstract:A method was developed for the separation and measurement of trivalent chromium and hexavalent chromium in health food. Though the study of pretreatment process， It was found that nitric acid， high tempera－ ture and high pressure could make the hexavalent chromium to trivalent chromium， which impacted the mea－ surement of the sample. It was found that the sample which was preprocessed with 10 % HCl and hot water could be effectively released chromium， and could prevent the conversion of hexavalent chromium to trivalent chromium. The separation of trivalent chromium and hexavalent chromium was achieved well on strong anion ex－ change resin， the recovery rate of trivalent chromium achieved 96.2 % and the recovery rate of trivalent chromi－ um achieved as low as 0.6 %. In the other hand， the chromium in health food of chromium yeast tablets was trivalent chromium.