CN110786513A - Method for extracting and purifying hemp full spectrum oil - Google Patents
Method for extracting and purifying hemp full spectrum oil Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention discloses a method for extracting and purifying hemp full-spectrum oil. Which comprises the following steps: 1. drying flowers and leaves in the sun, and coarsely crushing; 2. placing the coarsely crushed flowers and leaves into an oven for dry heat treatment; 3. pulverizing the obtained flower and leaf, and granulating; 4. extracting the obtained hemp grains in a subcritical extraction tank; 5. dissolving the concentrated extract with ethanol, and filtering; 6. concentrating the filtrate, adding silica gel, and stirring; 7. after the material glue is loaded into a pre-column, a reverse chromatographic column is used for separation; 8. concentrating and crystallizing the separated multi-spectrum oil section; 9. filtering the crystallization liquid by using a glass sand funnel, dissolving crystals obtained by filtering by using normal hexane, and extracting obtained filtrate by using normal hexane; 10. and combining the n-hexane dissolving solution and the extract, and concentrating to obtain the hemp full-spectrum oil concentrate. The method has the advantages of simple process, no tetrahydrocannabinol in the prepared hemp full-spectrum oil, low energy consumption, realization of recycling of the organic solvent, environment-friendly extraction and separation process and low toxicity.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine extraction processes, and particularly relates to a method for extracting and purifying full-spectrum oil of cannabis sativa.
Background
Industrial hemp (Stevia rebaudiana Bertoni) is an annual plant of the genus cannabis of the family cannabinaceae, widely distributed around the world. The Cannabis plants in the world are mainly 3 species of wild Cannabis sativa (Cannabis ruderalisisch), Indian Cannabis sativa (Cannabis indica Lam) and cultivated Cannabis sativa (Cannabis sativaL), and many Cannabis varieties and subspecies are generated in the long-term biological evolution process. Cannabis sativa contains Tetrahydrocannabinol (THC), a hallucinogenic secondary metabolite, and is one of the well-known drug-source plants. For convenience of supervision and reasonable use, the varieties of cannabis with THC content of less than 0.3% in cannabis are internationally defined as industrial cannabis which does not have drug utilization value. At present, 27 countries in the world grow industrial cannabis, and 26 industrial cannabis varieties with THC content of less than 0.3% are cultivated. The industrial hemp plants are tall and big, the branches are few, the fiber content is high, and the economic value of the industrial hemp plants relates to a plurality of aspects such as papermaking, spinning, building materials, food, medicine and the like. At present, more than one hundred Cannabinoids (CBs) are isolated from the plant cannabis sativa, mainly including Tetrahydrocannabinol (THC), Cannabidiol (CBD), Cannabinol (CBN), and cannabichromene (CBC), among which THC and CBD are the highest. Tetrahydrocannabinol (THC) has hallucinogenic addiction and limits the development of value in the medicinal field, the industrial hemp full-spectrum oil is extracted from industrial hemp, the main component cannabidiol is the main active component in cannabinoids, and the cannabidiol and the tetrahydrocannabinol have completely different active effects, are non-addictive active components and have no neurotoxicity. Has the function of protecting nerves, has no addiction, and has the functions of resisting epilepsy, spasm, rheumatic arthritis and anxiety, thereby attracting wide attention in the fields of medicine and pharmacology and becoming a research hotspot in recent years. The industrial hemp full-spectrum oil belongs to a fat-soluble mixture, components with hallucinogenic and addictive effects such as THC and the like are removed as much as possible, and a high-purity product is obtained, which is the premise for developing and applying the hemp full-spectrum oil.
Hemp oil has excellent skin affinity as a diluent for the hemp full spectrum oil, allowing rapid absorption of the hemp full spectrum oil, while also having its unique benefits. Hemp seed oil is the highest in all oils of monounsaturated and polyunsaturated fatty acids, with an average of 89%. Is the only water-soluble vegetable oil in the world at present. A polyunsaturated linoleic omega-6 fatty acid in sesame oil at a level of 55.6 g/100 g, a polyunsaturated alpha-linolenic acid mega-3 fatty acid at a level of 17.2 g/100 g. The ratio of the two fatty acids was 3.38, very close to the World Health Organization (WHO) recommended average ratio of 4.0. Hemp seed oil is an edible oil containing both linoleic acid and alpha-linolenic acid, the direct metabolites gamma-linolenic acid (GLA) and arachidic acid (SDA). Rich in unsaturated fatty acid (omega-3, omega-6, omega-9) and various active substances, and the ratio of omega-3, omega-6, omega-9 reaches the international recommended standard (omega-3: omega-6 is less than or equal to 1: 4); the unsaturated fatty acids omega-3, omega-6 and omega-9 have health promotion effects of preventing and adjuvant treating cardiovascular disease and cerebrovascular disease (hypertension, hyperlipemia and hyperglycemia); the hemp seed oil also has the effects of improving the excretion of organisms, removing wastes in the bodies, removing bad fat in the bodies, removing free radicals of cells, increasing the immunity of the organisms, regulating the internal environment of the human bodies, improving the sleep, delaying the aging and the like; meanwhile, the hemp seed oil is the only vegetable oil dissolved in water in the world and is more beneficial to the absorption of a human body.
The full spectrum (or broad spectrum) cannabis oil is a hemp flower leaf extract without further purification and separation, and contains Cannabidiol (CBD), Cannabinol (CBN), cannabichromene (CBC), Cannabigerol (CBG), Cannabidivarin (CBDV), and the like, and sometimes terpenes and aromatic compounds. The full spectrum CBD oils are generally more viscous, darker in color, and have the vegetable taste of china-hemp. Due to the medicinal value of Cannabidiol (CBD) and the medicinal expectations of Cannabinol (CBN), cannabichromene (CBC), Cannabigerol (CBG) and Cannabidivarin (CBDV), the extraction of full spectrum oil from cannabis sativa leaves has a wide market prospect.
Some reports about the hemp full-spectrum oil extraction method exist in the current published information, and the following problems are mainly found in the prior art by comparing and researching the existing process routes:
(1) the most used method in the existing cannabidiol extraction process is a solvent extraction method, one method is that a large amount of organic solvents with high cannabidiol solubility, such as n-hexane, petroleum ether, dichloromethane, chloroform, methanol and the like, are added, although the extraction rate of cannabidiol is improved, the use of the organic solvents can harm the environment, and the solvent residues in the final product cannot be removed completely, so that the safety of the product is also influenced; the other one is ethanol as an extractant, which reduces the toxicity of organic solvents, but has the problems of low extraction rate caused by low solubility of cannabidiol, large solvent recovery loss and high cost.
(2) The supercritical CO2 fluid extraction technology is applied to a cannabidiol extraction process in recent years, and although the supercritical extraction has the advantages of strong extraction capacity, high extraction rate, strong selectivity, good product quality and the like, the supercritical extraction also has the defects of high cost, high energy consumption, difficulty in realizing industrial scale-up production and the like.
Therefore, the method which has low cost and low energy consumption and is beneficial to industrial production needs to be provided at present. According to the principle of similarity and intermiscibility of organic matters, the extraction material and the extracting agent are subjected to molecular diffusion in the soaking process, so that fat-soluble components in the solid material are transferred to the liquid extracting agent, the extracting agent is separated from a target product through the process of reduced pressure evaporation, and the target product is finally obtained. The method has the advantages of no toxicity, harmlessness, environmental protection, no pollution, no hot processing, no damage and oxidation of active ingredients in the extract, high capacity, large-scale industrial production, energy conservation, low operation cost and easy separation of products; the invention not only protects the activity of the hemp full-spectrum oil, but also completely extracts the effective components in the hemp flower and leaf. In order to make full use of the full-spectrum hemp oil, the hemp full-spectrum oil is diluted by the hemp oil, so that the hemp full-spectrum oil is more beneficial to the absorption of a human body, and meanwhile, the hemp oil also has the health-care effects of preventing and assisting in treating cardiovascular and cerebrovascular diseases (hypertension, hyperlipidemia and hyperglycemia), improving the excretion of the human body, removing wastes in the body, removing bad fat in the body, removing cell free radicals and the like, and has the effects of increasing the immunity of the human body, regulating the internal environment of the human body, improving the sleep, delaying the aging and the like.
Disclosure of Invention
In order to completely extract the effective components in the hemp flowers and leaves and fully utilize the effective components, the invention adopts a subcritical fluid technology which is non-toxic, harmless, environment-friendly, pollution-free and non-thermal processing and a method for dissolving hemp multispectral oil by using hemp oil, so that the hemp full-spectrum oil is more beneficial to the absorption of a human body.
In order to achieve the purpose, the invention is realized by the following technical scheme:
1. pretreatment: the collected flower leaves are dried in the sun in situ, the leaf stalks are removed after the drying in the sun, and the crushed leaves are collected and crushed.
2. Dry heat treatment: spreading the coarsely crushed hemp flowers and leaves in a drying tray, and controlling the thickness to be 2-5 cm; the drying box is opened, the drying temperature is set at 100 ℃ and 150 ℃, and the drying time is 2-6 hours.
3. And (3) granulating: pulverizing the dried and heat treated flower and leaf into 40-100 mesh particles, adding 15-50% industrial ethanol, stirring, and standing for 10-40 min; starting the granulator, and making the flower and leaf into cylindrical granules with the diameter of 3-6mm and the length of 1-3 cm.
4. Subcritical extraction: putting hemp grains into an extraction tank, reducing pressure, adding n-butane, soaking, extracting for 2-5h at 25-40 deg.C for 2-3 times; the obtained extracting solution is roughly filtered by a filter screen of 100-mesh and 150-mesh, the obtained filtrate is kept stand and precipitated, and the supernatant is filtered by a filter screen of 200-mesh and 300-mesh; standing the obtained filtrate for precipitation, fine-filtering with a 300-400 mesh filter screen, heating the obtained filtrate (40-65 deg.C), and reducing pressure to obtain extract; and (3) cooling, compressing and recovering the n-butane.
5. Alcohol precipitation: adding ethanol at a ratio of 1:3-6 into the extract obtained by subcritical extraction, heating, stirring and dissolving; standing at normal temperature for 3-6 hr, filtering, and concentrating.
6. Mixing materials: pouring the concentrated extract into silica gel 4-7 times of the extract, starting a stirrer, setting the temperature at 60-80 deg.C, and stirring for 2-5 hr.
7. Column chromatography: loading the stirred gel material into a pre-column, preparing 30-60% ethanol/water eluent, and filling the column chromatography with macroporous resin.
8. Concentration: concentrating the separated multispectral oil segment until no ethanol is present.
9. And (3) extraction: adding n-hexane at a ratio of 1:2 into the obtained multispectral oil segment concentrated solution, extracting for 3 times, combining the extracts, concentrating, and draining to obtain multispectral oil, and performing vacuum rotary evaporation for 2-3 hours at a rotary evaporation temperature of 95-110 ℃.
10. Diluting and subpackaging: adding oleum Sesami into qualified multispectral oil at a ratio of 1:3-5, heating, mixing, standing, cooling, and packaging.
The invention has the beneficial effects that:
the method not only protects the active ingredients in the hemp multispectral oil from being damaged and oxidized, but also has the characteristics of complete extraction, easy product separation, large material input, energy conservation, low operation cost and the like; the prepared hemp full-spectrum oil is quickly absorbed by human body, has obvious effect and simultaneously has the unique health-care function of the hemp oil.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The specific implementation mode adopts the following technical scheme:
1. pretreatment: drying a certain amount of collected flowers and leaves in the sun on the spot until the moisture content is lower than 12%; and (4) drying in the sun, removing leaf stalks by using a self-made leaf removing machine, collecting crushed leaves, and coarsely crushing the obtained crushed leaves by using a crusher.
2. Dry heat treatment: collecting coarse hemp flower and leaf, spreading in 40 × 60cm drying plate with thickness of 2 cm; the drying oven was opened, the drying temperature was set at 110 ℃ and dried for 4 hours.
3. And (3) granulating: mixing the dried and heat treated leaves, pulverizing into 80 mesh particles, adding the pulverized particles into a mixing pot, adding 40% industrial ethanol, stirring for 5 min, and standing for 30 min; starting a granulator, and preparing the uniformly stirred hemp flower and leaf granules into cylindrical granules with the diameter of 4mm and the length of 1.5 cm; the prepared granules are poured into a drying bed to remove ethanol, and the obtained dried granules are screened by a 10-mesh screen to remove crushed powder.
4. Subcritical extraction: putting 20kg of hemp grains into an extraction tank, reducing pressure, adding n-butane for soaking, extracting for 2h at 30 ℃, and extracting for 2 times; coarsely filtering the obtained extractive solution with 100 mesh filter, standing the obtained filtrate for precipitation for 24 hr, and filtering the supernatant with 200 mesh filter screen; standing the obtained filtrate for precipitation for 24h, fine-filtering with a 300-mesh filter screen, heating the obtained filtrate to 45 ℃, and concentrating under reduced pressure to obtain 1.7kg of extract; and (3) cooling, compressing and recovering the n-butane.
5. Alcohol precipitation: putting the obtained extract into a 20L rotary evaporator, adding 10L industrial ethanol, heating to 70 deg.C, and dissolving for 1 h; after completely dissolving, standing at normal temperature for 6 hours, filtering with rapid filter paper, dissolving the filter residue with 5L industrial ethanol under heating for 0.5 hour, standing at normal temperature for 6 hours, mixing the filtrates, and concentrating to 2L.
6. Mixing materials: starting a small-sized mixer, adding 12kg of silica gel according to the obtained extract amount, pouring the concentrated hot-dipping paste into the mixer, setting the temperature at 70 ℃, and starting vacuum stirring for 5 hours.
7. Column chromatography: and (3) filling the stirred gel into a pre-column, knocking and jolting, firstly using 5 column volumes of ethanol water solution (30%) to pass through the column, collecting the front impurities, then using 52% (ethanol/water) eluent to elute, and judging and collecting according to thin-layer chromatography.
8. Concentration: the multispectral oil fractions obtained by separation are combined and concentrated in vacuum by a rotary evaporator until no ethanol is available.
9. And (3) extraction: pouring the obtained multi-spectrum oil-segment concentrated solution into an extraction tank, adding twice of n-hexane for extraction for three times, combining the extracts, concentrating and pumping the combined extracts by using a rotary evaporator, and carrying out rotary evaporation at the temperature of 95 ℃.
10. Diluting and subpackaging: detecting the dried multispectral oil, adding 5 times of edible oleum Sesami, heating, stirring, standing, cooling, and packaging.
The prepared hemp full-spectrum oil content meter is as follows:
the multispectral oil obtained in the experiment has comprehensive components and extremely low impurity content, the extraction and purification process has the advantages of complete extraction, large extraction amount, complete separation, greenness, no residue and the like, and the process method is very suitable for mass production.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for extracting and purifying hemp full-spectrum oil is characterized by comprising the following steps:
step 1, pretreatment: drying the collected flower leaves in the sun, removing leaf stalks after drying in the sun, and collecting crushed leaves and coarse crushing;
step 2, dry heat treatment: spreading the coarsely crushed hemp flowers and leaves in a drying tray, and drying at high temperature;
step 3, granulating: pulverizing the dried and heat treated leaves to obtain cylindrical granules;
step 4, subcritical extraction: putting hemp grains into an extraction tank, reducing pressure, adding n-butane for soaking, and extracting for 2-3 times;
and 5, alcohol precipitation: adding ethanol into the extract obtained by subcritical extraction, heating, stirring for dissolving, filtering, and concentrating;
step 6, stirring materials: pouring the concentrated extract into silica gel, and stirring to obtain uniform material gel;
and 7, column chromatography: macroporous resin is used as filler, and ethanol/water is used for elution;
step 8, concentration: concentrating the separated multispectral oil segment until no ethanol exists;
and 9, extraction: extracting the obtained multi-spectrum oil section concentrated solution by using normal hexane, concentrating and pumping;
step 10, diluting and subpackaging: dissolving the obtained multispectral oil with oleum Sesami, diluting, and packaging.
2. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: the water content of the hemp flowers and leaves in the step 1 is controlled below 10% after being aired, and the particles after coarse crushing are controlled to be about 20 meshes.
3. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: in the step 2, the hemp flowers and leaves are flatly paved in a drying disc, and the thickness is controlled to be 2-5 cm; the drying temperature is 100 ℃ and 150 ℃, and the drying time is 2-6 hours.
4. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: crushing the flowers and leaves subjected to the dry heat treatment in the step 3 into 40-100 mesh particles, adding 15-50% of industrial ethanol, uniformly stirring, and standing for 10-40 min; making into cylindrical granule with diameter of 3-6mm and length of 1-3 cm.
5. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: adding ethanol with the weight ratio of 1:3-6 into the extract obtained by subcritical extraction in the step 5, heating, stirring and dissolving; standing at normal temperature for 3-6 hr, filtering, and concentrating.
6. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: pouring the extract liquid obtained by concentration in the step 6 into silica gel, wherein the using amount of the silica gel is 4-7 times of that of the extract, stirring at the temperature of 60-80 ℃, and stirring for 2-5 hours.
7. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: the column chromatography packing in the step 7 is macroporous resin, and the eluent is 30-60% ethanol/water.
8. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: and (3) adding n-hexane with the ratio of 1:2 into the multispectral oil section concentrated solution obtained in the step (9) for extraction for 3 times, combining the extract solutions, concentrating and pumping to dryness, and performing vacuum rotary evaporation on the obtained multispectral oil for 2-3 hours at the rotary evaporation temperature of 95-110 ℃.
9. The method for extracting and purifying cannabis full spectrum oil according to claim 1, wherein the method comprises the following steps: and (3) adding the cannabis oil into the qualified multispectral oil detected in the step 10 according to the proportion of 1:3-5, heating and mixing uniformly, standing, cooling and packaging.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011399A (en) * | 2020-08-21 | 2020-12-01 | 滇麻生物科技(曲靖)有限公司 | Method for preparing polyphenol resin oil from industrial hemp |
| CN112206703A (en) * | 2020-09-29 | 2021-01-12 | 哈尔滨市汉博生物科技有限公司 | Pretreatment method before supercritical extraction of industrial hemp flowers and leaves |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011399A (en) * | 2020-08-21 | 2020-12-01 | 滇麻生物科技(曲靖)有限公司 | Method for preparing polyphenol resin oil from industrial hemp |
| CN112206703A (en) * | 2020-09-29 | 2021-01-12 | 哈尔滨市汉博生物科技有限公司 | Pretreatment method before supercritical extraction of industrial hemp flowers and leaves |
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