Determination of cannabinoids by gas chromatography–mass spectrometry and large-volume programmed-temperature vaporiser injection using 25 μl of biological fluid

This paper presents a GC–MS confirmation method, based on large-volume programmed-temperature vaporisation (PTV) injection, for the determination of cannabinoids in plasma samples (or whole blood) with deuterium-labelled internal standards using only 25 μl of biological fluid. The analytes, Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH), were enriched by means of solid-phase extraction cartridges containing octadecyl-bonded silica and were, subsequently, methylated. A 20 μl aliquot of an extract in hexane was injected into a PTV in solvent split mode. Method development and the results of the analyses of standard reference material and real samples are presented and discussed. This micro-method is precise and sensitive enough to assess relevant cannabinoid levels in human blood for forensic investigations as well as for clinical applications.