A rapid and efficient chromatographic method was developed to determine the labelling yields and radiochemical purity of99mTc-renal radiopharmaceuticals, including99mTc-glucoheptonate (99mTc-Gh),99mTc-gluconate (99mTc-Gl),99mTc-dimercaptosuccinic acid (99mTc-DMSA), and99mTc-diethylene triamine penta acetic acid (99mTc-DTPA). The chloroform/water partition coefficient was determined. For the separation of radiochemical impurities from99mTc-renal radiopharmaceuticals, the chromatography TLC on silica gel, and the instant thin-layer chromatography (ITLC) were used, applying polar and nonpolar solvents. The quantitative distribution of99mTc-renal preparation was determined by biological analysis on white rats.