A GC/ECD method was developed for the determination of glucosides.The target compound（phenyl β D glucopyranoside） was derivatized with N methyl bis（trifluoroacetamide）（MBTFA）.The derivatization temperature and time were optimized.The result indicated that the best derivatization conditions were achieved at 60 ℃ for 50 min.Fluorine was introduced to the product molecule after derivatization to provide the fundamental element for the detection of GC/ECD.Linear study was conducted by using phenyl β D glucopyranoside as a typical compound,and a correlation coefficient（r2） of 0.999 6 was obtained in the range of 0.05-200 mg?L-1.Six glucosides could be accurately identified by GC/ECD after MBTFA derivatization.Repeatability experiment showed that this derivatization combined with GC/ECD determination had a good performance,the relative standard deviation for the corresponding peak area was lower than 3% in 72 h.This method was also compared with the GC-MS method,and the limit of detection of GC/ECD method was greatly lowered.The proposed method is applicable in the determination of trace amount of glucosides in real sample.