Abstract: A method based on microextraction flask-high performance liquid chromatography was used for determination of carbamate insecticides in apple vinegar.Carbamate insecticides were separated on C18 column(5μm,250 × 4.6mm i.d.) using methanol∶ acetonitrile∶ water=40∶ 17∶ 43 as mobile phase and determined by UV detector at 210 nm.The flow rate of mobile phase was 1.0 mL/min.Isooctane was used as extractant.In this paper the regression equations of carbaryl,pirimicarb,ioprocarb and fenobucarb were determined in the samples with good linearity in the range of 16~1000 ng/mL,the correlation coefficients was more than 0.9968.The average recoveries were 86.33%,101.22%,100.17% and 112.32% respectively.The relative standard deviations were less than 5.26%.