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The tetrahydrocannabinol (THC) was obtained from Cannabis sativa L. plant material using supercritical fluid extraction (SFE) and solid phase extraction (SPE). SFE was utilized at different pressures (15–33 MPa), temperatures (40–80 °C) and ethanol (EtOH) as co-solvent (0–5%). The effect of extraction parameters on response variables (yield and THC content in raw extract) was evaluated. Keeping both temperature and co-solvent concentration constant at 60 °C and 2% respectively, the highest THC content in raw extracts reaches 37.85% at 33 MPa and 36.18% at 15MPa. One extract with high THC content was selected and submitted for purification-isolation by SPE. One final fraction with a 90.1% of THC was obtained using a single SPE step. This fraction was analyzed by GC, RP-HPLC and NMR to verify the THC purity. A sequential SFE-SPE process allows to obtain high purity THC from the cannabis plant, which is suitable as quality control material or analytical standard.
4. Conclusions
A sequential SFE-SPE process was explored to obtain THC with high purity from Cannabis Sativa L plant material. The effect of SFE parameters on extraction yield and THC content in the raw extract were analyzed; ethanol as co-solvent showed the main effect on both response variables, while pressure influenced the THC content. A better extraction yield was obtained at higher levels of pressure, temperature and ethanol percentage; however, these extraction conditions provided
a lower THC content. The highest THC recoveries were achieved using low ethanol percentages (2%), and an additional increase in pressure from 15 to 33 MPa improved THC extraction, but this reduced the extraction selectivity. SFE provided two extracts with the highest THC content, numbers 9 and 11 with 37.85 and 36.18% of THC, respectively. Extract number 11 was selected for the purification-isolation step due to less complexity. One single SPE step on extract number 11 allowed the extraction of THC at 90.1% purity, which was checked by chromatographic and spectroscopic analyses. On the basis of our results we conclude that from 100 g of Cannabis Sativa L plan material subjected to a sequential SFE-SPE process it is possible to obtain 13.97 g of THC enriched extract and 3.55 g of high purity THC. This is a promising candidate for an “in-house standard”, or to continue the purification
until a reference standard is obtained. We have shown the usefulness of combining SFE with SPE to obtain a raw clean extract. The foregoing allows us to have possibly a standard material type in-house THC, obtained at low cost and with fully affordable resources.
A sequential SFE-SPE process was explored to obtain THC with high purity from Cannabis Sativa L plant material. The effect of SFE parameters on extraction yield and THC content in the raw extract were analyzed; ethanol as co-solvent showed the main effect on both response variables, while pressure influenced the THC content. A better extraction yield was obtained at higher levels of pressure, temperature and ethanol percentage; however, these extraction conditions provided
a lower THC content. The highest THC recoveries were achieved using low ethanol percentages (2%), and an additional increase in pressure from 15 to 33 MPa improved THC extraction, but this reduced the extraction selectivity. SFE provided two extracts with the highest THC content, numbers 9 and 11 with 37.85 and 36.18% of THC, respectively. Extract number 11 was selected for the purification-isolation step due to less complexity. One single SPE step on extract number 11 allowed the extraction of THC at 90.1% purity, which was checked by chromatographic and spectroscopic analyses. On the basis of our results we conclude that from 100 g of Cannabis Sativa L plan material subjected to a sequential SFE-SPE process it is possible to obtain 13.97 g of THC enriched extract and 3.55 g of high purity THC. This is a promising candidate for an “in-house standard”, or to continue the purification
until a reference standard is obtained. We have shown the usefulness of combining SFE with SPE to obtain a raw clean extract. The foregoing allows us to have possibly a standard material type in-house THC, obtained at low cost and with fully affordable resources.
Continue at: https://www.researchgate.net/publication/330720744_Extraction_isolation_and_purification_of_tetrahydrocannabinol_from_the_Cannabis_sativa_L_plant_using_supercritical_fluid_extraction_and_solid_phase_extraction
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