Methods of Extraction of Plant Materials and Extracts Obtained Using Supercritical Glycerin

Abstract

A method for extracting bioactive compounds from plant materials using supercritical glycerin and at least one inert co-solvent that lowers the effective supercritical point of the supercritical glycerin to its boiling point, and the extracts obtained from the method.

Claims

1. A system for supercritical glycerin extraction of a composition of matter containing bioactive compounds comprising: a) at least one liquid glycerin reservoir; b) at least one heater connected to the liquid glycerin reservoir for converting the liquid glycerin from the liquid glycerin reservoir into glycerin vapor; c) at least one pressure regulator connected to the heater; d) at least one co-solvent gas reservoir; e) at least one condenser connected to the co-solvent gas reservoir; f) at least one pressure regulator connected to the condenser; g) a proportioning valve that receives the co-solvent gas and the glycerin vapor to form a mixture; h) an at least one additional heater connected to the proportioning valve to heat the mixture to form a supercritical mixture of co-solvent and glycerin; i) at least one extraction chamber containing the composition of matter for supercritical glycerin extraction connected to the additional heater; and j) at least one separator connected to the extraction chamber to separate gas co-solvent from the gas mixture comprising gaseous glycerin and gaseous co-solvent.

2. The system of claim 1, wherein the extraction process is automated.

3. The system of claim 1, wherein a plurality of separators are connected sequentially to the extraction chamber to separate selected bioactive compounds.

4. A method for supercritical extraction of a composition of matter containing bioactive compounds comprising contacting a selected composition of matter which contain bioactive compounds that are soluble in supercritical glycerin, with a supercritical mixture of glycerin and one or more non-reactive inert gas co-solvents with an effective supercritical point temperature below 301° Kelvin to provide optimal concentrations of glycerin in the extract while reducing the supercritical point of the mixture, in an amount effective to maintain the glycerin in supercritical phase for a sufficient time to extract the selected bioactive materials from the selected composition of matter, wherein the one or more inert co-solvents lower the effective supercritical temperature of the supercritical mixture to its boiling point for a time effective to produce a glycerin extract containing the selected bioactive compounds.

5. The method of claim 4 wherein the plant materials are contacted for extraction with a supercritical mixture of glycerin vapor and one or more inert gas co-solvents at temperatures between approximately 550° K and approximately 700° K and at pressures between approximately 250 kPa and approximately 7500 kPa.

6. The method of claim 4 wherein the one or more inert co-solvents are selected from the group consisting of Helium, Neon, Argon, and Krypton, Carbon Dioxide, and Xenon gases.

7. The method of claim 4 wherein the composition of matter consists of plant materials.

8. The method of claim 7 wherein the plant materials are cannabis plants and/or seeds.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The advantages of the invention will become readily apparent to those skilled in the art from the detailed description of implementations of the invention when considered in the light of the accompanying drawings, in which:

[0014] FIG. 1 depicts an implementation of a supercritical fluid extraction apparatus for performing the methods of the invention.

DETAILED DESCRIPTION

[0015] The present invention provides a method of performing SFE of plant materials such as cannabis, containing bioactive compounds, using supercritical glycerin and a co-solvent, resulting in less viscous extracts in glycerin that are readily mixed and packaged by automation in line with the extraction process. The result is a high throughput extraction system.

[0016] In an implementation of the invention, a temperature above 554° Kelvin (290° C.) (the boiling point of glycerin) is used during extraction to prevent the supercritical glycerin from returning to a liquid state. However, temperatures higher than glycerin's boiling point may increase decomposition of desirable thermolabile bioactive products. Thus, in the method of the invention, the effective supercritical temperature point of the mixture of glycerin combined with one or more inert co-solvents is lowered to the boiling point of glycerin, limiting the decomposition rate to reasonable levels. The co-solvent used must be a non-reactive (inert) gas species with an effective supercritical point temperature below 310° Kelvin to provide optimal concentrations of glycerin in the extract, while reducing the supercritical point of the mixture. Suitable inert co-solvents include gases having low critical point temperatures and pressures and in particular gases that are non-reactive at 563° Kelvin that have a critical point temperature below 250° to 300° Kelvin. Suitable gases include Helium, Neon. Argon, and Krypton. Carbon dioxide and Xenon may be used as the co-solvent in higher amounts (based on the molar fraction of glycerin to co-solvent) however, the total glycerin content would constitute a lower percentage of the eluate, lessening efficiency by lowering the throughput of the apparatus used for the extraction.

[0017] In the method of the invention, a selected plant material is prepared, for example, by washing and/or fragmenting the material and is added to the main extraction chamber 10 before the extraction process begins. Referring to the system depicted in FIG. 1, at least one co-solvent gas such as helium, in an amount dependent on the selected extraction batch size, is added to a reservoir 12 and liquid glycerin is added to a separate reservoir 14. Multiple co-solvent gases may be used, in which case additional separate reservoirs may be added. At the initiation of the extraction process, the extractor 10 may be flushed with an inert gas, for example helium, and a mild vacuum is used to remove oxygen and other gaseous contaminates from the extractor 10.

[0018] When the system of FIG. 1 is placed in operation, the helium is released from reservoir 12 into a condenser 16 that condenses the helium to above its critical pressure at 227 kPa, forming supercritical helium. The condenser 16 releases the supercritical helium into a gas pump 18 that further raises the pressure to a pre-determined level for the mixture of supercritical glycerin and helium. In the case of the minimum viable temperature (563 Kelvin) for optimal conservation of glycerin, the pressure is at least or above 4975 kPa in a 35% Helium, 65% glycerin mixture. This ratio is determined using an Equation of State such as the Peng Robinson equation of state (“PR EOS,” Peng, D. Y.; Robinson, D. B. (1976) Industrial and Engineering Chemistry: Fundamentals 15: 59-64.) The liquid glycerin is pumped from reservoir 14 via a liquid pump 20 to regulate the amount of glycerin introduced, dependent on the selected extraction batch size. The liquid pump 20 pumps the glycerin into a pre-heater 22 to raise the liquid glycerin to its vapor temperature so that the gases may be mixed. The vapor glycerin and the supercritical helium move through the individual back pressure regulators 24 and 26 into a proportioning valve 28, where they become a mixture. The proportioning valve 28 serves to ensure the correct preselected amounts of the two gases in the mixture is achieved; in this example, as a 35% Helium, 65% glycerin molar mixture. The proportioning valve 28 outputs to another heater 30, which ensures the two gases in the mixture are brought to the appropriate temperature of 563° K and remain above the 4975 kPa pressure. This supercritical mixture is then fed into the extractor 10 until that same pressure and temperature level is achieved and the supercritical mixture is allowed to mix with the plant material, extracting the compounds. The extractor 10 includes temperature and pressure sensors within its chamber to monitor and regulate the pressure and temperature. The supercritical mixture remains in the extractor 10 at the desired temperature and pressure for a period of time sufficient to extract the bioactive compounds from the specific plant material. The supercritical fluid mixture with the plant material is then expelled from the extractor 10.

[0019] After extraction is completed, the plant material is removed and the supercritical fluid product is cooled down to below 563° Kelvin to bring the glycerin containing the extracted bioactive products back to a liquid form, as the mixture passes through the separators 32, 34, 36 and 38, which recapture the helium to be used again, and remove the now liquid glycerin extract into a separate product container. At least one separator is used, however multiple separators may be used for a fractionation process to separate out specific bioactive compounds in multiple runs on the same batch of plant material using a fractionation column. The extract is then in a concentrated form of liquid glycerin with a viscosity lower than a pure oil, which can then be packaged or diluted further for use.

[0020] Different co-solvents may be used to obtain optimum amounts of desired bioactive products from a selected plant material. Co-solvents with higher supercritical temperatures will require a higher co-solvent to glycerin ratio. This means there will be less glycerin in the end, extracted product, and thus a higher ratio of extracted compounds to glycerin, i.e. a more concentrated solution. The lower the supercritical temperature of the co-solvent(s), the less concentrated the end product.

[0021] The present invention can be practiced other than as specifically illustrated and described herein without departing from its spirit or scope.