The general use of a number of Tc-99m-labelled compounds makes the need for good routine quality control procedures, especially the labelling efficiency measurements. The purpose of these study were to measure the labelling efficiency of Tc-99m-labelled MDP, DTPA, Tin colloid, and Antimony sulfide colloid using miniaturized paper and instant thin layer chromatography. The chromatographic systems include whatman 3 MM paper and acetone, Gelman ITLC-SG and 0.9% sodium chloride. The chromatographic strips are miniaturized (1×10 cm), marked and numbered. Labelling efficiencies of Tc-99m-labelled DTPA and Tin colloid were above 98.0%. Tc-99m- labelled Antimony sulfide colloid was 90.0%. And labelling efficiency of Tc-99m-labelled MDP was 89.0% Coefficient variance of Tc-99m-labelled MDP, DTPA, Tin colloid, and Antimony sulfide colloid were 5.14%, 2.06%, 1.82% and 4.90%, respectively. We found that this miniaturized chromatographic quality control was simple and reliable.