We describe here a simple sample pretreatment method, SPE combined with DLLME, for the sensitive determination of carbamates in fruit and vegetable samples. The new approach has numerous advantages such as simplicity of operation, ultra preconcentration factor, low detection limit and relatively short analysis time compared with other conventional sample-preparation methods. This combined method improved the selectivity and sensitivity of SPE and DLLME. The performance of this procedure in the extraction of carbamates from different matrices was excellent. Accordingly, this method possesses great potential in the analysis of ultra trace compounds in real samples. Acknowledgements This work was supported by Education Department of Hubei Province (grant no. T201101), the National
Nature Science Foundation of China (grant no. 20975030,
20835004), the Natural Science Foundation of Hubei province of
China (grant no. 2009CDB364), and the Specialist Fund of Hubei
University (020091130-ky2006004). The authors would like to
thank their colleagues for their valuable technical assistance.