In this paper，alkylphenols（APs） were separated by micellar electrokinetic chromatography(MEKC) and reversed electrode polarity stacking mode（REPSM） was developed for the on-line sample stacking of these compounds.MEKC coupled with REPSM increased 20-285 times of the sensitivity for osBP，TBBPA，BPA，OP and NP compared to the conventional MEKC.The separation conditions in the MEKC method were studied，and many factors affecting the sample stacking process were investigated in detail.Additionally，sample injection as large as 41.37 kPa×60 s was applied in REPSM-MEKC.The linear relationship and reproducibility were also examined.Under the optimum conditions，the detection limits（S/N=3） of APs were in the range of 0.027-0.64 μmol/L.The method has been successfully applied in the detection of APs in food-packing bags with recoveries of 86.0%-103%.