A method was developed for the determination of sodium monofluoroacetate in human blood by ion chromatography. The analysis was performed on a Dionex Ion Pac AS11 column (250 mm x 4 mm i.d.) with an AG11 guard column (50 mm x 4 mm i.d.). A conductivity detector, an SRS suppressor and a 25 microL sample loop were used. The eluent was 2.0 mmol/L Na2B4O7 with a flow rate of 1.0 mL/min. A blood sample of 0.2 mL was pipetted into a test tube followed by adding 1.0 mL of pure water. And then acetonitrile was used to dilute it to 3.0 mL. After the protein was settled down from the blood sample, the supernatant layer was filtered through a 0.45 microm filter before injected into the ion chromatographic system. Good linear relationship between the peak area and the concentration of sodium monofluoroacetate was found with correlation coefficient (r2) of 0.9978 within the range from 0.10 to 10.0 mg/L. The detection limit for blood was 2.5 mg/L. This method also can be used for the determination of sodium monofluoroacetate in food samples.