SUMMARY— A, gas‐liquid chromatographic method coupled with an electron capture detector has been developed for analyzing chlorinated phenoxyacetic acid residues in canned fruits. The technique involves converting the acid to its methyl ester with diazomethane, chromatography on a 5% silicone grease SE‐30 column at 210°C, and subsequent detection of the compound by an electron capture detector. As low as 0.02 ppm of the residue could be detected. The method is superior to the calorimetric method because parachlorophenoxyacetic acid (PCPA), 2,4‐D, and 2,4,5‐T can be separated and quantitatively determined simultaneously. However, separate standard curves are needed for each, because they differ in chlorine content and in sensitivity toward the electron capture detector. Levels of 2,4‐D and 2,4,5‐T residues in canned apricots, and of PCPA in canned grapes are reported.