Abstract: Samples of flour were extracted with mixed solvent of acetic acid-n-hexane (20+80). After centrifugation, supernatant was concentrated to 2 mL at 50 ℃ by rotary evaporator and made up to 8 mL with mobile phase, which was used for HPLC analysis. CN-chromatographic column was used as stationary phase and mixed solutions of n-hexane, acetonitrile and butylene oxide (97+1+2) was used as mobile phase. DAD-detection was made at 214 nm. Values of detection limits (3S/N) of the 5 organotin compounds found were in the range of 0.14-0.31 mg·L-1. On the base of blank sample of flour, test for recovery was made by standard addition method, values of recovery found were in the range of 82%-95%.