High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means of a central composite design (CCD) approach, and the analysis method was fully validated. Six major cannabinoids [tetrahydrocannabinolic acid (THCA), tetrahydrocannabinol (THC), cannabidiol (CBD), tetrahydrocannabivarin (THCV), cannabigerol (CBG), and cannabinol (CBN)] were quantified (RSD < 10%), and seven more cannabinoids were identified and verified by means of a liquid chromatograph coupled to a quadrupole-time-of-flight (Q-ToF) detector. Finally, based on the distribution of the analyzed cannabinoids in 30 Cannabis sativa L. plant varieties and the principal component analysis (PCA) of the resulting data, a clear difference was observed between outdoor and indoor grown plants, which was attributed to a higher concentration of THC, CBN, and CBD in outdoor grown plants.

The optimisation of focused ultrasound extraction and supercritical fluid extraction of volatile oils and cannabinoids from marihuana has been accomplished by experimental design approach. On the one hand, the focused ultrasound extraction method of volatile compounds and cannabinoids was studied based on the optimisation of cyclohexane and isopropanol solvent mixtures, and the instrumental variables. The optimal working conditions were finally fixed at isopropanol/cyclohexane 1:1 mixture, cycles (3 s(-1)), amplitude (80%) and sonication time (5 min). On the other hand, the supercritical fluid extraction method was optimised in order to obtain a deterpenation of the plant and a subsequent cannabinoid extraction. For this purpose, pressure, temperature, flow and co-solvent percentage were optimised and the optimal working conditions were set at 100 bar, 35°C, 1 mL/min, no co-solvent for the terpenes and 20% of ethanol for the cannabinoids. Based on the retention time locking GC-MS analysis of the supercritical fluid extracts the classification of the samples according to the type of plant, the growing area and season was attained. Finally, three monoterpenes and three cannabinoids were quantified in the ranges of 0.006-6.2 μg/g and 0.96-324 mg/g, respectively.

There is an increasing need of developing methods for fast recognition and identification of new psychoactive substances (NPS). The chemical identification of these new substances produced with the intention of mimicking the effects of controlled drugs is a challenge for forensic and Customs laboratories. In this study, we aim to test the potential of Raman spectroscopy for the identification and classification of seized Customs samples into three NPS families. The performance of two excitation wavelength lasers (785 and 1064 nm) in a benchtop Raman instrument was compared in a set of seized samples that included cathinone, fentanyl, and synthetic cannabinoid derivatives or analogues. The 1064 nm wavelength laser had significant advantages for identifying NPS samples overcoming the intense fluorescence induced when using 785 nm lasers in some substances. Principal component analysis was employed to create a model that successfully discriminates the three NPS families. In order to provide Customs officers with a fast and nondestructive in‐field testing method, the same approach used with the benchtop Raman spectrometer was applied using three handheld Raman instruments. The developed identification and classification model allows the discrimination of fentanyl, cathinone, and synthetic cannabinoid analogues or derivatives providing an efficient tool for the rapid identification of three NPS families. The approach presented in this study can facilitate rapid decision‐making that could be of high relevance especially in the frame of the fentanyl crisis.

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