Mitoxantrone, a new anti-cancer agent, was successfully prepared for Lipiodol emulsion. The mixture of Mitoxantrone and non-ionic contrast medium, Omnipaque 300, was combined with Lipiodol at the ratio of 1:2. When the ratio of Mitoxantrone and Lipiodol was 1:4, microscopic study revealed stabilized water in oil emulsion, which could release the anti-cancer agent slowly. We applied it for a case of hepatocellular carcinoma with good result. Intra-arterial infusion of this emulsion might be considered effective for treatment of hepatocellular carcinoma.