Direct Analysis of Psilocin and Muscimol in Urine Samples Using Single Drop Microextraction Technique In-Line with Capillary Electrophoresis.

Abstract

The fully automated system of single drop microextraction coupled with capillary electrophoresis (SDME-CE) was developed for in-line preconcentration and determination of muscimol (MUS) and psilocin (PSC) from urine samples. Those two analytes are characteristic active metabolites of <i>Amanita</i> and <i>Psilocybe</i> mushrooms, evoking visual and auditory hallucinations. Study analytes were selectively extracted from the donor phase (urine samples, pH 4) into the organic phase (a drop of octanol layer), and re-extracted to the acidic acceptor (background electrolyte, BGE), consisting of 25 mM phosphate buffer (pH 3). The optimized conditions for the extraction procedure of a 200 µL urine sample allowed us to obtain more than a 170-fold enrichment effect. The calibration curves were linear in the range of 0.05-50 mg L^-1, with the correlation coefficients from 0.9911 to 0.9992. The limit of detections was determined by spiking blank urine samples with appropriate standards, i.e., 0.004 mg L^-1 for PSC and 0.016 mg L^-1 for MUS, respectively. The limits of quantification varied from 0.014 mg L^-1 for PSC and 0.045 mg L^-1 for MUS. The developed method practically eliminated the sample clean-up step, which was limited only to simple dilution (1:1, <i>v</i>/<i>v</i>) and pH adjustment.

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