Abstract: GC-MS was applied to the determination of residual amounts of 53 pesticides in bean sprout with online gel permeation chromatography and solid-phase extraction. The bean sprout sample was extracted with the mixture of acetic acid-acetonitrile (1+99),and purified with solid-phase extraction column. Online gel permeation chromatography and GC was used for separation and the selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 53 pesticides were kept in the same range of 0.01-1.0 mg·L-1,with detection limits in the range of 0.1-6.0 μg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 20,50,100 μg·kg-1,giving values of recovery and RSD′s (n=6) in the ranges of 72.3%-104% and 1.6%-6.6%,respectively.