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A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence (POCL) detection and column switching has been developed for simultaneous determination of 3,4-methylenedioxymethamphetamine (MDMA) and related compounds, for example 3,4-methylenedioxyamphetamine, methamphetamine, and amphetamine, in hair. After digestion of the hair with 1 mol L−1 sodium hydroxide the compounds were extracted with n-heptane and derivatized with 4-( N, N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole. A mixture of hydrogen peroxide and bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate in acetonitrile was used as post-column CL reagent. Calibration plots showed linearity was good ( r = 0.999); detection limits were 0.02–0.16 ng mg−1 hair at a signal-to-noise ratio of 3. The precision of the method, as RSD ( n = 5), in intra-day and inter-day assays was better than 5.0 and 6.9%, respectively. The proposed method was sufficiently sensitive to detect low ng mg−1 levels of MDMA and related compounds in hair, and could be used for quantification of the compounds in hair samples from patients treated in a chemical dependency unit. [ABSTRACT FROM AUTHOR]