A polarographic method for the determination of as little as 1 µg. of gold in blood and serum samples is described. The relative error is 2.1%. After the sample is dry ashed at 550°, the gold is extracted into ether as the chloride, to separate it from interfering copper and iron. A polarogram of the gold sample is obtained in 2 M potassium hydroxide. The method should be applicable to the determination of gold in other biological samples containing interfering elements.