CN115531442A - Method for simultaneously extracting industrial hemp flower and leaf original distillate and full spectrum oil - Google Patents
Method for simultaneously extracting industrial hemp flower and leaf original distillate and full spectrum oil Download PDFInfo
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- CN115531442A CN115531442A CN202211000474.7A CN202211000474A CN115531442A CN 115531442 A CN115531442 A CN 115531442A CN 202211000474 A CN202211000474 A CN 202211000474A CN 115531442 A CN115531442 A CN 115531442A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/60—Moraceae (Mulberry family), e.g. breadfruit or fig
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a method for simultaneously extracting industrial hemp flower and leaf crude distillate and full spectrum oil, which comprises the following steps: (1) Pretreating industrial hemp flowers and leaves to obtain pretreated industrial hemp flowers and leaves, wherein the size of the pretreated industrial hemp flowers and leaves is 2-10 cm, and the water content is 50-75%; (2) Extracting the pretreated industrial hemp flower and leaf by adopting an out-phase liquid ultramicro process to obtain a light component and a heavy component, wherein the light component is original dew of the industrial hemp flower and leaf; (3) And separating and purifying the heavy components by adopting a high-speed counter-current chromatograph to obtain full spectrum oil, wherein the full spectrum oil is rich in cannabidiol. The extraction method provided by the invention can simultaneously extract the flower and leaf original dew and the full spectrum oil rich in cannabidiol from the industrial hemp flowers and leaves, thereby greatly improving the added value of the industrial hemp flowers and leaves and fully utilizing resources; the extraction process has simple flow, low energy consumption and high extraction efficiency.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to a method for simultaneously extracting industrial hemp flower and leaf juice and full spectrum oil.
Background
Hemp (Cannabis sativa L.) is a traditional economic crop in China, has a long history of cultivation, and is mainly applied to multiple fields of textile, papermaking, food, medicine and the like. Industrial cannabis refers to cannabis plants with a tetrahydrocannabinol content of less than 0.3% in roots, stems, leaves and seeds. The research shows that the industrial hemp plants contain more than 400 chemical substances, wherein more than 60 cannabinol substances are separated, the main phenolic substances comprise Tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), cannabigerol (CBG), cannabichromene (CBC), sub-Cannabidiol (CBDV) and the like, and the former three substances account for 90% of the cannabinol substances. The industrial hemp flower and leaf is rich in various hemp pigment components, wherein CBD is proved to have the functions of blocking the adverse effect of certain polyphenol on the human nervous system, blocking breast cancer metastasis, treating epilepsy, resisting inflammation, rheumatoid arthritis, resisting insomnia and other physiological activities, and has good effect of treating multiple sclerosis. The hemp plant contains hallucinogenic addiction-causing THC, which limits the development of its value in the pharmaceutical field. The industrial hemp full-spectrum oil is extracted from industrial hemp, and its main active ingredient is non-addictive CBD except for containing most cannabinoids including CBN, CBG, CBC, a small amount of THC, etc., terpenes and aromatic compounds. The full spectrum oil is usually viscous, dark in color and has the plant taste of hemp. Due to the medicinal value of CBD and medicinal expectation of CBN, CBC, CBG and CBDV, the full-spectrum oil extracted from the industrial hemp flowers and leaves has wide market prospect.
In addition, industrial hemp flowers and leaves also contain abundant flavones and their glycosides, alkaloids, coumarins, terpenes and sterols, fatty acids, phenanthrenes and other compounds. The effective components have analgesic, intraocular pressure lowering, antitumor, emesis resisting, fear memory weakening, blood pressure resisting, antithrombotic, antibacterial, antiinflammatory, antioxidant and other pharmacological effects, and have high development and utilization values. The flower and leaf original lotion prepared from the industrial hemp flower and leaf can fully utilize other nutrient components except cannabinoids in the industrial hemp flower and leaf, and improve the added value of the industrial hemp flower and leaf.
At present, a method for simultaneously extracting CBD full-spectrum oil and raw juice from industrial cannabis sativa leaves does not exist, so that researches and developments of a method for simultaneously extracting raw juice of the leaves and full-spectrum oil rich in cannabidiol from the industrial cannabis sativa leaves are very necessary, and the additional value of the industrial cannabis sativa is further improved.
Disclosure of Invention
The invention provides a method for simultaneously extracting industrial cannabis sativa leaf crude distillate and cannabidiol, which aims to solve the technical problem that the prior art cannot simultaneously extract the cannabis sativa leaf crude distillate and full spectrum oil from industrial cannabis sativa leaves.
According to an aspect of the present invention, there is provided a method for simultaneously extracting industrial cannabis sativa leaf distillate and whole spectrum oil, comprising the steps of:
(1) Pretreating industrial hemp flowers and leaves to obtain pretreated industrial hemp flowers and leaves, wherein the size of the pretreated industrial hemp flowers and leaves is 2-10 cm, and the water content is 50-75%;
(2) Extracting the pretreated industrial hemp flower and leaf by adopting an out-phase liquid ultramicro process to obtain a light component and a heavy component, wherein the light component is original dew of the industrial hemp flower and leaf, and the heavy component is a crude extract of full-spectrum oil;
(3) And separating and purifying the heavy components by adopting a high-speed counter-current chromatograph to obtain full-spectrum oil, wherein the full-spectrum oil is rich in cannabidiol.
Further, the pre-processing comprises: when the industrial hemp flowers and leaves are fresh flowers and leaves, the pretreatment comprises the following steps: cleaning, removing impurities and cutting into pieces; when the industrial hemp flowers and leaves are dried flowers and leaves, the pretreatment comprises: cleaning, removing impurities, cutting into pieces and soaking.
Further, the heterogeneous liquid state ultramicro process comprises:
stacking the pretreated industrial hemp flowers and leaves as a raw material, heating the lower part of the raw material to a first temperature, cooling the lower part of the raw material to a second temperature so as to form convection between the upper part and the lower part of the raw material and generate vacuum, wherein the first temperature is higher than the second temperature, and the temperature difference between the first temperature and the second temperature is at least 140 ℃;
reducing the overall temperature of the raw materials to a third temperature in a vacuum environment, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed, wherein the third temperature is higher than the second temperature and lower than the first temperature;
and under the vacuum environment, raising the temperature of the raw material to a fourth temperature, keeping the temperature for 10-48 h, and collecting heavy components separated out from the raw material and condensed, wherein the fourth temperature is higher than the third temperature and lower than the first temperature.
Further, the heterogeneous liquid state ultramicro process comprises:
1) Stacking the pretreated industrial hemp flowers and leaves as raw materials, heating the lower part of the raw materials to 160-220 ℃ for 60-120 s, cooling the lower part of the raw materials to 10-20 ℃ to form convection between the upper part and the lower part of the raw materials and generate vacuum;
2) Reducing the integral temperature of the raw materials to 70-90 ℃ in a vacuum environment, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed;
3) Raising the temperature of the raw material to 100-150 ℃ in a vacuum environment, keeping the temperature for 10-48 h, collecting heavy components separated out from the raw material and condensed,
wherein the negative pressure of the vacuum environment is-0.08 to-0.1 MPa.
Further, the industrial hemp flower and leaf essence comprises terpenoids, esters, ketones, organic acids, amino acids, alkaloids and brass.
Further, the separation and purification of the heavy components by using a high-speed counter-current chromatograph comprises the following steps:
s1, mixing n-hexane, methanol and pure water to prepare a solvent, or mixing n-hexane, ethanol and pure water to prepare a solvent, standing the solvent, and taking an upper phase liquid and a lower phase liquid;
s2, taking the upper phase liquid as a stationary phase, dissolving the heavy component by using the stationary phase to obtain a mixed liquid, and pumping the mixed liquid into a high-speed counter-current chromatographic separation device after filtering;
s3, taking the lower phase liquid as a mobile phase, starting the high-speed counter-current chromatographic separation device, pumping the mobile phase to elute relative to the mixed liquid, and collecting eluent;
and S4, concentrating the eluent under reduced pressure to obtain full-spectrum oil.
Further, in step S2, the mass/volume ratio of the recombinant component to the stationary phase is 1: (5-10).
Further, in step S3, the elution rate of the mobile phase is 0.5 to 5mL/min.
Further, in step S3, in step S4, the temperature at the time of concentration under reduced pressure is 60 to 80 ℃.
Further, the cannabidiol content in the whole spectrum oil is 20-70% by mass, and the tetrahydrocannabinol content in the whole spectrum oil is lower than 0.2% by mass.
The invention has the following beneficial effects:
the extraction method provided by the invention can simultaneously extract the flower and leaf original dew and the full spectrum oil rich in cannabidiol from the industrial hemp flowers and leaves, thereby greatly improving the added value of the industrial hemp flowers and leaves and fully utilizing resources; the extraction process has simple flow, low energy consumption and high extraction efficiency.
The industrial cannabis sativa leaf original juice prepared by the extraction method comprises terpenoids, esters, ketones, organic acids, amino acids, alkaloids or brass, has extremely high medicinal value and the like, does not contain tetrahydrocannabinol, and is safe to use.
The cannabidiol content in the full spectrum oil prepared by the extraction method is 20-70% by mass, and the method has the advantages of high cannabidiol yield and high cannabidiol content.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a raw dew of industrial hemp leaves obtained in example 1 of the present invention;
FIG. 2 is a LC-MS chart of the industrial hemp flower leaf raw dew prepared in example 1 of the present invention;
FIG. 3 is a full spectrum oil chart obtained in example 1 of the present invention;
FIG. 4 is a chromatogram of the full spectrum oil of industrial hemp flowers and leaves obtained in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention more clear, the present invention is further described in detail with reference to the following embodiments. It should be understood that the embodiments described in this specification are only for the purpose of explaining the present invention and are not intended to limit the present invention.
For the sake of brevity, only some numerical ranges are explicitly disclosed herein. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and similarly any upper limit may be combined with any other upper limit to form a range not explicitly recited. Also, although not explicitly recited, each point or individual value between endpoints of a range is encompassed within the range. Thus, each point or individual value may, as its lower or upper limit, be combined with any other point or individual value or with other lower or upper limits to form ranges not explicitly recited.
In the description herein, it is to be noted that, unless otherwise specified, "above" and "below" are inclusive, and "a plurality" of "one or more" means two or more.
The embodiment of the application provides a method for simultaneously extracting industrial hemp flower and leaf original dew and full spectrum oil, which comprises the following steps:
(1) Pretreating industrial hemp flowers and leaves to obtain pretreated industrial hemp flowers and leaves, wherein the size of the pretreated industrial hemp flowers and leaves is 2-10 cm, and the water content is 50-75%;
(2) Extracting the pretreated industrial hemp flowers and leaves by adopting a heterogeneous liquid ultramicro process to obtain a light component and a heavy component, wherein the light component is original dew of the industrial hemp flowers and leaves, and the heavy component is a crude extract of full-spectrum oil;
(3) And separating and purifying the heavy components by adopting a high-speed counter-current chromatograph to obtain full spectrum oil, wherein the full spectrum oil is rich in cannabidiol.
Extracting the pretreated industrial hemp flower and leaf by an out-phase liquid ultramicro process, wherein the light component obtained after extraction is industrial hemp flower and leaf crude dew, and the heavy component is a crude extract of full-spectrum oil which is rich in cannabidiol; separating and purifying the heavy components by using a high-speed counter-current chromatograph to obtain full-spectrum oil. The combination of the two can simultaneously extract the flower and leaf original dew and the full spectrum oil rich in cannabidiol from the industrial hemp flowers and leaves, greatly improves the added value of the industrial hemp flowers and leaves and fully utilizes resources; the extraction process has simple flow, low energy consumption and high extraction efficiency.
The extraction method provided by the invention can simultaneously extract the flower and leaf original dew and the full spectrum oil rich in cannabidiol from the industrial hemp flowers and leaves, thereby greatly improving the added value of the industrial hemp flowers and leaves and fully utilizing resources; the extraction process has simple flow, low energy consumption and high extraction efficiency.
In some embodiments, the pre-processing comprises: when the industrial hemp flowers and leaves are fresh flowers and leaves, the pretreatment comprises the following steps: cleaning, removing impurities and cutting into pieces; when the industrial hemp flowers and leaves are dried flowers and leaves, the pretreatment comprises: cleaning, removing impurities, cutting into pieces and soaking. The size of the pretreated industrial hemp flowers and leaves is 2-10 cm, the size is too thin, the loading of raw materials is not facilitated, the leakage situation can occur, and the too thin raw materials are not conducive to the penetration of heat, so that the heating is not uniform, and the extraction is not sufficient; the raw materials are too thick, so that the raw materials are difficult to fill uniformly, the space of a material bin can be wasted, and the use efficiency of equipment is reduced.
In some embodiments, the water content of the pretreated industrial hemp flowers and leaves is 50-75%, the water content is too low, and dry raw materials cannot be in a cell filling state, so that the extraction rate of effective components is reduced; the water content is too high, so that the water content in the extracted original dew is too much, the effective components in the original dew are diluted, and the subsequent concentration process is increased.
In some embodiments, the heterogeneous liquid state ultramicro process comprises:
stacking the pretreated industrial hemp flowers and leaves as a raw material, heating the lower part of the raw material to a first temperature, cooling the lower part of the raw material to a second temperature so as to form convection between the upper part and the lower part of the raw material and generate vacuum, wherein the first temperature is higher than the second temperature, and the temperature difference between the first temperature and the second temperature is at least 140 ℃;
in a vacuum environment, reducing the overall temperature of the raw materials to a third temperature, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed, wherein the third temperature is higher than the second temperature and lower than the first temperature;
and under the vacuum environment, raising the temperature of the raw material to a fourth temperature, keeping the temperature for 10-48 h, and collecting heavy components separated out from the raw material and condensed, wherein the fourth temperature is higher than the third temperature and lower than the first temperature.
According to the embodiment of the application, in the heterogeneous liquid ultramicro process, the high-concentration extraction of the original floral leaf can be realized by adding zero organic solvent or a small amount of ethanol, and the method is environment-friendly and healthy; nutrient substances existing in the large molecular groups can be collected and extracted after being subjected to micromolecule formation, so that the nutrient substances are easy to absorb by a human body and have comprehensive nutrient components; can effectively separate light components and heavy components extracted from the raw materials, so that the extracted flower and leaf original dew does not contain the psychotoxic substance tetrahydrocannabinol.
In some embodiments, the heterogeneous liquid state ultramicro process comprises:
1) Stacking the pretreated industrial hemp flowers and leaves as raw materials, heating the lower part of the raw materials to 160-220 ℃ for 60-120 s, cooling the lower part of the raw materials to 10-20 ℃ to enable the upper part and the lower part of the raw materials to form convection and generate vacuum;
2) In a vacuum environment, reducing the overall temperature of the raw materials to 70-90 ℃, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed;
3) Raising the temperature of the raw material to 100-150 ℃ in a vacuum environment, keeping the temperature for 10-48 h, collecting heavy components separated out from the raw material and condensed,
wherein the negative pressure of the vacuum environment is-0.08 to-0.1 MPa.
In the scheme, different temperature gradients are adopted to respectively extract flowers She Yuanlou and crude extracts rich in cannabidiol in industrial cannabis sativa leaves. At a lower temperature, terpene substances contained in the extracted flower and leaf raw dew are mainly volatile terpenes containing 10-15 carbons, while tetrahydrocannabinol and cannabidiol both contain 21 carbons in molecular structures, have higher boiling points and can be separated out at a higher temperature generally.
According to the embodiment of the application, the flowers She Yuanlou and heavy components in the industrial hemp flowers and leaves are respectively extracted by adopting the different temperature gradients (the first temperature is 160-220 ℃, the third temperature is 70-90 ℃ and the fourth temperature is 100-150 ℃). At a lower temperature, terpene substances contained in the extracted flower and leaf original dew are mainly volatile terpenes containing 10-15 carbons. The molecular structures of tetrahydrocannabinol and cannabidiol both contain 21 carbons, have higher boiling points, and can be separated out at higher temperature.
In the examples of the present application, the industrial hemp flower leaf essence includes terpenoids, esters, ketones, organic acids, amino acids, alkaloids, brass and other easily volatile or water-soluble substances with low boiling points. Furthermore, the industrial cannabis sativa leaf raw distillate does not contain tetrahydrocannabinol.
In an embodiment of the present application, the separating and purifying the heavy component by using a high-speed counter-current chromatograph includes:
s1, mixing n-hexane, methanol and pure water to prepare a solvent, or mixing n-hexane, ethanol and pure water to prepare a solvent, standing the solvent, and taking an upper phase liquid and a lower phase liquid;
s2, taking the upper phase liquid as a stationary phase, dissolving the heavy component by using the stationary phase to obtain a mixed liquid, filtering the mixed liquid, and pumping the mixed liquid into a high-speed counter-current chromatography separation device;
s3, taking the lower phase liquid as a mobile phase, starting the high-speed counter-current chromatographic separation device, pumping the mobile phase to elute relative to the mixed liquid, and collecting eluent;
and S4, concentrating the eluent under reduced pressure to obtain full-spectrum oil.
According to the embodiment of the application, the stationary phase and the mobile phase used in the separation and purification are both liquid, and the stationary phase can be updated after each separation, so that the phenomenon of column efficiency reduction can not occur; the separation effect is very stable, and the solvent can be recycled, thereby reducing the cost.
In the examples of the present application, in step S1, the volume ratio of n-hexane, methanol and pure water is 10:8.5:1.5; the mass ratio of n-hexane, ethanol and pure water is 10:7:3; and (3) standing the mixed solvent for 0.5-2 h to generate layering, and taking an upper phase liquid and a lower phase liquid.
In the examples of the present application, in step S2, the mass/volume ratio of the recombinant fraction to the stationary phase is 1: (5-10).
According to an embodiment of the application, the mass/volume ratio of the recombinant component to the stationary phase is 1: (5-10) all effective components in the heavy component can not be completely dissolved due to the low proportion of …; the volume required to be separated is too large due to too high proportion, the separation amount of subsequent separation is increased, the separation efficiency is reduced, too much separation reagent is consumed, and the separation cost is increased.
In the examples of the present application, the elution rate of the mobile phase in step S3 is 0.5 to 5mL/min.
According to the embodiment of the application, in the step S3, the elution speed of the mobile phase is 0.5 to 5mL/min, which is because the elution speed of the mobile phase is too high, resulting in poor separation effect; the elution speed is too slow, and the time consumed is too long, resulting in low separation efficiency.
In the embodiment of the application, the content of cannabidiol in the whole spectrum oil is 20-70% by mass, and the content of tetrahydrocannabinol in the whole spectrum oil is lower than 0.2% by mass.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrative only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. All parts, percentages, and ratios reported in the following examples are on a weight basis, all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the equipment used in the examples is commercially available, unless otherwise specified.
Example 1
The embodiment provides a method for simultaneously extracting a floral leaf raw distillate and a cannabidiol-rich full-spectrum oil from industrial cannabis sativa leaves, which comprises the following steps:
(1) Preparing raw materials: cleaning freshly picked 2.1kg of industrial hemp flowers and leaves with purified water, removing impurities, cutting into pieces of 8cm, and extracting the fresh flowers and leaves with the water content of 68%;
(2) Extraction treatment: the raw materials are piled up, the lower part of the piled raw materials is rapidly heated to 190 ℃, the upper part of the raw materials is cooled, the temperature of the raw materials is kept at low temperature of 20 ℃, the upper part and the lower part of the raw materials are in convection, and vacuum is generated. The temperature of the raw materials is reduced to 70 ℃ in a vacuum environment of-0.08 MPa, the raw materials are kept for 40h, and 1.4L of light components separated out from the raw materials and condensed are collected, namely the industrial hemp flower and leaf original juice (figure 1), which is clear and transparent from figure 1, does not contain visible impurities such as green leaves and the like, has hemp fragrance when smelling the flower and leaf original juice, and is detected by a full-spectrum metabolism detection technology, so that the flower and leaf original juice contains rich substance components including terpenes, esters, ketones, organic acids, amino acids, alkaloids, flavones and the like, and does not contain tetrahydrocannabinol (Table 1). FIG. 2 is a LC-MS diagram of the industrial hemp flower and leaf distillate, which shows that the components in the flower and leaf distillate are rich and various.
Heating the raw materials to 120 deg.C under-0.08 MPa, maintaining for 48 hr, collecting heavy components separated out from the raw materials and condensed to obtain extract rich in cannabidiol, wherein the content of cannabidiol in the extract is 6.3% by detection.
The detection method comprises the following steps: detecting the extract by High Performance Liquid Chromatography (HPLC), wherein the detection conditions of HPLC are as follows: the mobile phase is acetonitrile and 0.1% acetic acid, and the proportion of acetonitrile and 0.1% acetic acid is 75%:25 percent, isocratic elution with the flow rate of 0.8mL/min; the sample injection amount is 10 mu L; the column temperature was 25 ℃; the detector detection wavelength is 220nm.
(3) Separation and purification: mixing n-hexane, methanol and pure water according to a ratio of 10.5; dissolving the extract rich in cannabidiol with 5 times volume of stationary phase, filtering with 0.45 μm filter membrane, and subjecting to high speed countercurrent chromatography; pumping the stationary phase into a high-speed counter-current chromatography separation device, starting the separation device, pumping the mobile phase at the flow rate of 2mL/min, and starting elution; collecting target eluate, and concentrating under reduced pressure at 60-80 deg.C to obtain cannabidiol-rich full-spectrum oil (figure 3), which is brown viscous and rich in taste of industrial cannabis plant as shown in figure 3. High performance liquid chromatography detection shows that the full spectrum oil contains 75.1% of CBD and 0.13% of THC, and FIG. 4 is a chromatogram of the full spectrum oil, which shows that the full spectrum oil contains various cannabinoids, and has the highest CBD content and very low THC content.
Table 1 full spectrum metabolome assay results in the industrial cannabis sativa leaf stock solution prepared in example 1
Note: the one with the highest relative content in the original flower and leaf lotion is cyclohexanol (relative value 2.54E + 08), while cannabigerol (relative value 1.16E + 05), sub-cannabidiolic acid (relative value 5.15E + 04), sub-cannabichromenic acid (relative value 2.12E + 04), cannabidiolic acid (relative value 9.26E + 04), and delta 9-tetrahydrocannabinol with very low content are detected.
Example 2
A method for simultaneously extracting a floral leaf raw distillate and a full spectrum oil rich in cannabidiol from industrial cannabis sativa leaves comprises the following steps:
(1) Preparing raw materials: removing impurities from 1.6kg industrial hemp dried flower and leaf, cutting into 10cm pieces, soaking in 9L purified water overnight, taking out, air drying to dry surface, and separating out the flower and leaf with water content of 72%;
(2) Extraction treatment: the raw materials are stacked, the lower part of the raw materials is rapidly heated to 205 ℃, the upper part of the raw materials is cooled, the temperature is kept at low 15 ℃, the upper part and the lower part of the raw materials are in convection, and vacuum is generated. Reducing the temperature of the raw materials to 85 ℃ in a vacuum environment of-0.10 MPa, keeping the temperature for 48h, collecting 7.5L of light components separated out and condensed from the raw materials, namely the industrial hemp flower and leaf original juice, and detecting by using a full-spectrum metabolic detection technology to find that the flower and leaf original juice contains rich substance components including terpenes, esters, ketones, organic acids, amino acids, alkaloids, flavones and the like, and does not contain tetrahydrocannabinol. Heating the raw materials to 150 ℃ in a vacuum environment of-0.10 MPa, keeping the temperature for 42h, collecting heavy components separated out from the raw materials and condensed, namely the extract rich in cannabidiol, wherein the content of cannabidiol in the extract is 4.2% by detection.
(3) High-speed countercurrent chromatographic separation: mixing n-hexane, ethanol and pure water according to a ratio of 10; dissolving the extract rich in cannabidiol with 10 times volume of stationary phase, filtering with 0.45 μm filter membrane, and subjecting to high speed countercurrent chromatography; pumping the stationary phase into a high-speed counter-current chromatography separation device, starting the separation device, pumping the mobile phase at the flow rate of 3mL/min, and starting elution; collecting target eluent, concentrating under reduced pressure at 60-80 deg.C to obtain full spectrum oil rich in cannabidiol, and detecting by high performance liquid chromatography to obtain the full spectrum oil with CBD content of 69.1% and THC content of 0.10%.
Example 3
A method for simultaneously extracting a floral leaf raw distillate and a full spectrum oil rich in cannabidiol from industrial cannabis sativa leaves comprises the following steps:
(1) Preparing raw materials: removing impurities from 1.4kg of industrial hemp dried flower and leaf, cutting into 5cm pieces, soaking in 4L of purified water overnight, taking out, air drying until the surface is dry, and extracting the flower and leaf with water content of 58%;
(2) Extraction treatment: extracting the fresh flower leaves by using an out-phase liquid ultramicro raw juice extractor, wherein the extraction temperature is 219 ℃, the extraction time is 42h, collecting 3.7L of condensate in an extraction bin after extraction, namely the industrial hemp flower leaf raw juice, and detecting by using a full-spectrum metabolic detection technology to find that the raw juice contains rich substances, including terpenes, esters, ketones, organic acids, amino acids, alkaloids, flavones and the like, and does not contain tetrahydrocannabinol; meanwhile, the discharge in the discharge bin in the next step is collected, namely the extract rich in cannabidiol, and the content of cannabidiol in the extract is 4.9% through detection.
(3) High-speed countercurrent chromatographic separation: mixing n-hexane, methanol and pure water according to a ratio of 10.5; dissolving the extract rich in cannabidiol with a stationary phase with 8 times volume, filtering with a 0.45 μm filter membrane, and subjecting to high-speed countercurrent chromatography; pumping the stationary phase into a high-speed counter-current chromatography separation device, starting the separation device, pumping the mobile phase at the flow rate of 1.5mL/min, and starting elution; collecting target eluent, concentrating under reduced pressure at 60-80 deg.C to obtain full spectrum oil rich in cannabidiol, and detecting by high performance liquid chromatography to obtain the full spectrum oil with CBD content of 72.5% and THC content of 0.19%.
Comparative example 1
A method for simultaneously extracting a floral leaf raw distillate and a full spectrum oil rich in cannabidiol from industrial cannabis sativa leaves comprises the following steps:
(1) Preparing raw materials: removing impurities from 1.4kg of industrial hemp dried flower and leaf, cutting into 5cm pieces, soaking in 4L of purified water overnight, taking out, air drying until the surface is dry, and extracting the flower and leaf with water content of 58%;
(2) Extraction treatment: rapidly heating the lower part of the dried flower and leaf to 250 deg.C, cooling the upper part of the raw material, and maintaining at 5 deg.C to allow convection between the upper and lower parts of the raw material to generate vacuum. Reducing the temperature of the raw materials to 100 ℃ in a vacuum environment of-0.10 MPa, keeping the temperature for 40h, collecting 7.5L of light components separated out and condensed from the raw materials, wherein the light components are industrial hemp flower and leaf original dew, and after detection by a full-spectrum metabolism detection technology, the flower and leaf original dew contains rich substance components including terpenes, esters, ketones, organic acids, amino acids, alkaloids, flavones and the like, and contains low-concentration tetrahydrocannabinol. Heating the raw materials to 200 deg.C under-0.10 MPa, maintaining for 40 hr, collecting heavy components separated out from the raw materials and condensed to obtain extract rich in cannabidiol, wherein the content of cannabidiol in the extract is 1.8% by detection.
(3) High-speed countercurrent chromatographic separation: mixing n-hexane, ethanol and pure water according to a ratio of 10; dissolving the extract rich in cannabidiol with 8 times of stationary phase, filtering with 0.45 μm filter membrane, and subjecting to high speed countercurrent chromatography; pumping the stationary phase into a high-speed counter-current chromatography separation device, starting the separation device, pumping the mobile phase at the flow rate of 1.5mL/min, and starting elution; collecting target eluent, concentrating under reduced pressure at 60-80 deg.C to obtain full spectrum oil rich in cannabidiol, and detecting with high performance liquid chromatography to obtain full spectrum oil with CBD content of 42.5% and THC content of 0.32%.
In comparative example 1, it is known that, in the extraction process, when the second temperature is too high, part of cannabinoids with high boiling points, including cannabidiol, tetrahydrocannabinol and the like, is simultaneously separated out, so that the low-concentration tetrahydrocannabinol in the floral leaf original water is caused; and the third temperature is too high, which causes serious carbonization of the raw material, and large loss of part of cannabinoids such as cannabidiol and the like, thereby reducing the yield of cannabidiol in heavy components. In the separation process, an improper ratio of the fixed phase to the mobile phase cannot achieve an ideal separation effect, and finally the THC content in the whole-spectrum oil exceeds the standard.
While the present application has been described with reference to preferred embodiments, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the present application, and in particular, features shown in the various embodiments may be combined in any manner as long as there is no structural conflict. The present application is not intended to be limited to the particular embodiments disclosed herein but is to cover all embodiments that may fall within the scope of the appended claims.
Claims (10)
1. A method for simultaneously extracting industrial hemp flower and leaf juice and full spectrum oil is characterized by comprising the following steps:
(1) Pretreating industrial hemp flowers and leaves to obtain pretreated industrial hemp flowers and leaves, wherein the size of the pretreated industrial hemp flowers and leaves is 2-10 cm, and the water content is 50-75%;
(2) Extracting the pretreated industrial hemp flower and leaf by adopting an out-phase liquid ultramicro process to obtain a light component and a heavy component, wherein the light component is original dew of the industrial hemp flower and leaf, and the heavy component is a crude extract of full-spectrum oil;
(3) And separating and purifying the heavy components by adopting a high-speed counter-current chromatograph to obtain full-spectrum oil, wherein the full-spectrum oil is rich in cannabidiol.
2. The method for simultaneous extraction of industrial cannabis sativa leaf distillate and whole spectrum oil as claimed in claim 1, characterized in that the pre-treatment comprises:
when the industrial hemp flowers and leaves are fresh flowers and leaves, the pretreatment comprises the following steps: cleaning, removing impurities and cutting into pieces;
when the industrial hemp flowers and leaves are dried flowers and leaves, the pretreatment comprises: cleaning, removing impurities, cutting into pieces and soaking.
3. The method for simultaneously extracting industrial cannabis sativa leaf distillate and whole spectrum oil as claimed in claim 1, characterized in that the heterogeneous liquid ultramicro process comprises:
stacking the pretreated industrial hemp flowers and leaves as a raw material, heating the lower part of the raw material to a first temperature, cooling the lower part of the raw material to a second temperature so as to form convection between the upper part and the lower part of the raw material and generate vacuum, wherein the first temperature is higher than the second temperature, and the temperature difference between the first temperature and the second temperature is at least 140 ℃;
reducing the overall temperature of the raw materials to a third temperature in a vacuum environment, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed, wherein the third temperature is higher than the second temperature and lower than the first temperature;
and under the vacuum environment, raising the temperature of the raw material to a fourth temperature, keeping the temperature for 10-48 h, and collecting heavy components separated out from the raw material and condensed, wherein the fourth temperature is higher than the third temperature and lower than the first temperature.
4. The method for simultaneously extracting industrial cannabis sativa leaf distillate and whole spectrum oil as claimed in claim 3, characterized in that the heterogeneous liquid ultramicro process comprises:
1) Stacking the pretreated industrial hemp flowers and leaves as raw materials, heating the lower part of the raw materials to 160-220 ℃ for 60-120 s, cooling the lower part of the raw materials to 10-20 ℃ to form convection between the upper part and the lower part of the raw materials and generate vacuum;
2) Reducing the integral temperature of the raw materials to 70-90 ℃ in a vacuum environment, keeping the temperature for 10-48 h, and collecting light components separated out from the raw materials and condensed;
3) Raising the temperature of the raw material to 100-150 ℃ in a vacuum environment, keeping the temperature for 10-48 h, collecting heavy components separated out from the raw material and condensed,
wherein the negative pressure of the vacuum environment is-0.08 to-0.1 MPa.
5. The method for simultaneously extracting industrial cannabis sativa leaf distillate and full spectrum oil according to any one of claims 1-4, characterized in that terpenes, esters, ketones, organic acids, amino acids, alkaloids and brass are included in the industrial cannabis sativa leaf distillate.
6. The method for simultaneously extracting industrial cannabis sativa leaf distillate and full spectrum oil as claimed in claim 1, wherein the separation and purification of the heavy components by high speed counter current chromatography comprises:
s1, mixing n-hexane, methanol and pure water to prepare a solvent, or mixing n-hexane, ethanol and pure water to prepare a solvent, standing the solvent, and taking an upper phase liquid and a lower phase liquid;
s2, taking the upper phase liquid as a stationary phase, dissolving the heavy component by using the stationary phase to obtain a mixed liquid, filtering the mixed liquid, and pumping the mixed liquid into a high-speed counter-current chromatography separation device;
s3, taking the lower phase liquid as a mobile phase, starting the high-speed counter-current chromatographic separation device, pumping the mobile phase to elute relative to the mixed liquid, and collecting eluent;
and S4, concentrating the eluent under reduced pressure to obtain full-spectrum oil.
7. The method for simultaneously extracting industrial cannabis sativa leaf distillate and full spectrum oil according to claim 6, wherein in step S2, the mass/volume ratio of the heavy components to the stationary phase is 1: (5-10).
8. The method for simultaneously extracting industrial cannabis sativa leaf distillate and full spectrum oil as claimed in claim 6, wherein the elution speed of the mobile phase in step S3 is 0.5-5 mL/min.
9. The method for simultaneously extracting industrial hemp flower and leaf juice and full spectrum oil according to claim 6, wherein in step S4, the temperature at the time of vacuum concentration is 60-80 ℃.
10. The method for simultaneously extracting industrial cannabis sativa leaf distillate and whole spectrum oil as claimed in any one of claims 6-9, wherein the weight percentage of cannabidiol in the whole spectrum oil is 20-70%, and the weight percentage of tetrahydrocannabinol in the whole spectrum oil is lower than 0.2%.
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Application publication date: 20221230 |