Abstract: Gas chromatography was applied to the determination of monochloroacetic acid in drinks. The sample was extracted with methyl tert-butyl ether, and the extract was derivatized with methanol. DB-1701 quartz capillary chromatographic column was used for separation; and electron capture detector was used for determination with 1,2-dibromopropane as internal standard. Values of correlation coefficient in 3 ranges of low, middle and high concentration found were more than 0.996 0. Values of lower limit of determination (10S/N) found were less than 10.0 μg·kg-1. Using blank sample of drinks as matrixes, recovery was tested at 3 different concentration levels and values of recovery found were in the range from 72.4% to 107% with RSD′s (n=6) in the range from 0.39% to 9.0%.