Directly suspended droplet liquid–liquid–liquid micro extraction (DSDME) has been used to determine residues of ecstasy (3,4-methylenedioxy-N-methylamphetamine) in hair samples. In this technique a free suspended droplet of an aqueous solvent is delivered to the top-center position of an immiscible organic solvent floating on the top of an aqueous sample while being agitated by a stirring bar placed on the bottom of the sample cell. In the present work, ecstasy was extracted from hair samples by LLLME and analyzed by UV-Vis Spectroscopy. Factors such as organic solvent, extraction and back extraction times, stirring rate and the pH of acceptor and donor phases were optimized. Enrichment factor and detection limit (LOD, n = 3) were 147.4 and 0.0057 ng.ml-1. The linearity ranged from 0.010 to 15 g.ml-1 with a %RSD of 1.63 (n = 3). All experiments were carried out at room temperature (25 ± 0.5 ºC).
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