A high-performance liquid chromatography technique has been presented to measure the [(201)Tl]TlCl(3) impurity in [(201)Tl]TlCl radiopharmaceutical for precise determination of radiochemical purity. Diethylene tetraamine pentaacetic acid (DTPA) has been used for complete complexation of [(201)Tl]Tl(III). [(201)Tl]Tl(III)-DTPA was analyzed in the presence of [(201)Tl]Tl(I) using a cation exchange HPLC column.