Abstract: An HPLC-MS/MS method using carbaryl as the internal standard substance was established for qualitative detection and quantitative determination of carbofuran and its main metabolite benzofuranol in bio-samples to study their postmortem distribution in rats. The rats were poisoned dead by intragastric administration of carbofuran suspension at the concentration of 1. 8 mg/mL, which was 4 times of the LD₅₀(44 mg/kg). Then the rats were dissected at 0, 12, 24, 48, 72 and 96 hours after death to collect the their specimen(heart, liver, spleen, lung, kidney, brain, muscle, stomach, blood)and the carbofuran concentration were determined using HPLC-MS/MS method. The results showed that at 0 h after death, the carbofuran was distributed in rats was as follows: stomach> lung or liver> kidney or spleen> muscle> heart or heart blood or brain and transferred from stomach, lung and heart blood to liver, kidney and muscle over time, while the benzofuranol was distributed as follows: stomach> heart blood> liver or kidney> spleen or muscle or lung or brain > heart, and the concentration of benzofuranol in heart blood, heart, liver, spleen, and kidney had significant increase(P< 0. 05)over time. The postmortem concentration change of carbofuran and benzofuranol could be attributed to the degradation of carbofuran and the trans-tissues diffusion of carbofuran and benzofuranol. The postmortem distribution manner of carbofuran and benzofuranol and their HPLC-MS/MS analysis method could be applied to the forensic identification and help taking samples for toxicology analysis.