An economical, fast, and simple method for the extraction and liquid chromatographic determination of chloramphenicol (CAP) in milk is described. CAP is extracted by using a recently developed membrane-based method named "diphasic dialysis." CAP is detected and quantitated in the organic solvent used in dialysis without additional cleanup steps by reversed-phase liquid chromatography and UV detection (270 nm). The determination limit of CAP in milk was about 5 micrograms/L, although as little as 1 microgram/L could be detected under optimal working conditions.