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Three-phase single drop microextraction (SDME) was in-line coupled to chiral capillary electrophoresis (CE) of weakly basic amine compounds including amphetamine.SDME was used for the matrix isolation and sample preconcentration in order to directly analyze urine samples with the minimal pretreatment of adding NaOH.A small drop of an acidic aqueous acceptor phase covered with a thin layer of octanol was formed at the tip of a capillary by simple manipulation of the liquid handling functions of a commercial CE instrument.