Abstract:Dispersive liquid-liquid microextraction （DLLME）coupled with ultra performance liquid chromatography-high resolution quadrupole time of flight mass spectrometer（UPLC-TOF-MS）method was established for the determination of five carbamate pesticides in fresh juice.Samples were purified by primary secondary amine（PSA）sorbent，then extraction with methanol as dispersant and chloroform as extractant and finally the organic phase was detected by ultra performance liquid chromatography - high resolution quadrupole time of flight mass spectrometer （UPLC-TOF-MS） after centrifugation.Data were acquisited with electrospray ionization（ESI）and atmospheric pressure chemical ionization（APCI）composite sources and positive ion mode.The calibration curves of five analytes showed good linearity within the concentrations of 2.0 μg/L-200 μg/L（r＞0.999 0）.The average recoveries ranged from 84.5%to 97.8%，the limits of detection and quantification were 0.02 μg/kg-0.05 μg/kg and 0.05 μg/kg-0.15 μg/kg respectively，while the relative standard deviations（RSDs）were 1.28%-6.88%.