A gas chromatographic method using an electron capture detector (GC-ECD) was developed for the determination of residual dalapon, esterified with methanol in sulfuric acid, in sugarcane. Dalapon in plant matrix was initially extracted with sulfuric acid solution, followed by partition extraction with diethyl ether in the presence of NaCl and esterification with 10% H2SO4 methanolic for GC-ECD analysis. Recovery of dalapon (0.05~0.20 ppm) spiked in sugarcane samples was carried out to obtain an average recovery of 89.7~109.4% with a coefficient of variation (CV) of 1.0~9.3% and a method detection limit (MDL) of 0.01 ppm. Peak of dalapon methyl ester was further identified by a GC-MS spectrum. The developed procedure was simple and the reagents used were slightly toxic, thus suitable for the accurate quantification of dalapon residues in crops.