Sensitive determination of methylenedioxylated amphetamines by liquid chromatography

Different strategies for the liquid chromatographic determination of methyl enedioxylated amphetamines were evaluated: separation and detection of unde rivatized analytes by (i) UV or (ii) fluorescence, (iii) derivatization wit h 3,5-dinitrobenzoyl chloride followed by separation and UV detection of th e derivatives formed and (iv) derivatization with 9-fluorenylmethyl chlorof ormate (FMOC) and subsequent separation and fluorimetric detection of the d erivatives. The compounds tested were 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylampheta mine (MDE). On the basis of these studies, a new procedure for the chromato graphic determination of MDA, MDMA and MDE is proposed, based on derivatiza tion with FMOC. The described procedure allows the quantification of the te sted compounds with adequate linearity, reproducibility and accuracy in the concentration interval 0.5-20.0 mug mL(-1). The limits of detection were 0 .01 mug mL(-1) for MDA and 0.025 mug mL(-1) for MDMA and MDE. The utility o f the described assay was tested by determining methylenedioxylated ampheta mines in plasma and urine.