METHOD FOR EXTRACTION OF CANNABINOIDS AND SYNTHESIS OF THC TO CBN
A method is disclosed to extract and purify cannabinoids from hemp biomass followed by isolation of various components including THC. The hemp-derived THC is reacted with a halogen, leading to the oxidation of THC to CBN. The removal of halogen is improved via selective solvent exchange. CBN is isolated from the reaction mixture by use of orthogonal chromatography techniques. The CBN is optionally recombined with the remaining purified cannabinoids to create a CBN enriched broad-spectrum extract.
1 . A method of isolating, modifying, and recombining components of industrial hemp to produce a cannabinoid extract free of THC and rich with other cannabinoids comprising the steps of:
extracting hemp with an alcohol to produce a crude cannabinoid composition;
heating the crude cannabinoid composition to decarboxylate cannabinoids;
distillation of the cannabinoids to remove low boiling point impurities and provide a first pass distillate;
distillation of said first pass distillate to remove high boiling point impurities and provide a cannabinoid distillate;
performing chromatography to isolate said cannabinoid distillate into a THC in solvent fraction and a broad-spectrum extract in solvent fraction; and
drying said broad spectrum extract in solvent fraction to provide a broad-spectrum cannabinoid mixture free of THC.
2 . The method of claim 1 further comprising the steps of:
drying said THC in solvent fraction to produce a THC extract;
dissolving said THC extract in a solvent;
reacting said THC extract with a halogen to oxidize to CBN;
quenching said halogen in an aliphatic solvent; and
purifying CBN by orthogonal chromatography to yield purified CBN.
3 . The method of claim 2 further comprising the steps of:
combining a broad-spectrum cannabinoid mixture free of THC.
combining said broad spectrum cannabinoid mixture free of THC and said
purified CBN to produce a CBN enriched broad spectrum extract.
4 . The method of claim 3 , wherein said solvent is toluene.
5 . The method of claim 4 , wherein said halogen is iodine.
6 . The method of claim 5 , wherein the reaction mixture is solvent exchanged from toluene to an alkane after the reaction is complete to decrease soluble iodine.
7 . The method of claim 6 , wherein said alkane is heptane.
8 . The method of claim 1 , wherein said chromatography comprises centrifugal partition chromatography (CPC) performed on a stationary phase of water and methanol with heptane mobile phase.
9 . The method of claim 2 , wherein said orthogonal chromatography comprises a normal phase chromatography performed on a silica gel stationary phase with heptane-ethyl acetate mobile phase.
10 . The method of claim 9 , wherein said orthogonal chromatography step further comprises a reversed phase chromatography performed on C18 silica gel with methanol-water mobile phase.
11 . The method of claim 10 wherein said reversed phase chromatography is performed after said normal phase chromatography.