Salvinorin A, a psychoactive hallucinogen, and related compounds, were analyzed in plants, water, and urine using liquid-liquid extraction (LLE), solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography-time of flight mass spectrometry (GC×GC-ToFMS). A semi-qualitative study of the extraction of Salvinorin A and analogs from Salvia divinorum plants by LLE showed ppb levels of Salvinorin A and several analogs in the leaves and stems of S. divinorum plants, much lower than expected. Quantitative analysis of Salvinorin A spiked into water and urine showed much better figures of merit for SPME than LLE, with limit of detection of about 5 ng/mL, linear range from 8 to 500 ng/mL and precision about ±10% for the SPME-based analyses using external standard quantitation. GC×GC-ToFMS was especially effective in separating the peaks of interest from matrix and chromatographic interferences.
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