To explore the most sensitive and useful method for simultaneous determination of 8 carbamate pesticides in livestock productions, the mixture of 8 carbonates was determined by HPLC with scanning fluorescence detector. For mobile phase water, acetonitrile and methanol program gradient showed more applicable sensitivity than water and acetonitrile program gradient used ExW 339 nm and EmW 445 nm for fluorescence detector. On using carbamate columns, the retention time was within 4 to 20 minutes. And this made it possible to separate and detect simultaneously. therefore we could analyze it exactly and efficiently and reduce time. The preparation process of MSPD method showed that the high recovery rate was more than 88.5% in most of the carbamate pesticides. Therefore we could say that it was an efficient and fast method analyzing out of lots of samples.