A rapid and simple method for the simultaneous detection and quantitation of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA) and methylenedioxyethylamphetamine (MDEA) in human serum was developed and fully validated. Serum samples were extracted with cyclohexane, derivatised with perfluorooctanoyl chloride without prior evaporation of the solvent and analysed with gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM). For quantitation, deuterated analogues were used as the internal standards. The limit of detection (LOD) and lower limit of quantitation (LLOQ), bias and within-day and between-day precision were determined. LODs calculated as the average of the six calibration curves were below 5 ng/mL for all of the measured compounds; LLOQs obtained in the same manner were below 20 ng/mL, with the exception of MDA (24.1 ng/mL). The coefficients of variation were below 7% within series, 10% or less between series and the bias was below 8% for all compounds. The calibration curves were linear between the lower limits of quantitation and 800 ng/mL.

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A rapid and selective cleanup procedure based on immunoadsorption is described for the simultaneous extraction of diazepam and its free or glucuronidated metabolites nordiazepam, temazepam, and oxazepam from urine. The method can also be used for the extraction of lorazepam and lorazepam-glucuronide. Because the samples do not have to be hydrolyzed before extraction, valuable information is preserved. With the exception of lorazepam-glucuronide, recoveries between 86 and 100% were obtained at spiking levels up to 200 ng of benzodiazepine or glucuronide per milliliter of urine. Using methanol/water (90:10, v/v) as an eluent, the immunoadsorber could be used at least 20 times. High-performance liquid chromatograms of urine samples from patients receiving low therapeutic dosages of diazepam or lorazepam are shown to demonstrate the high purity of the extracts.