CN110577855A - Hemp seed oil rich in cannabidiol and preparation method thereof - Google Patents

Hemp seed oil rich in cannabidiol and preparation method thereof Download PDF

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Publication number
CN110577855A
CN110577855A CN201810581523.8A CN201810581523A CN110577855A CN 110577855 A CN110577855 A CN 110577855A CN 201810581523 A CN201810581523 A CN 201810581523A CN 110577855 A CN110577855 A CN 110577855A
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hemp
extraction
cannabidiol
seed oil
hemp seed
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朱元庄
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Shanxi Han Ma Biological Science And Technology Co Ltd
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Shanxi Han Ma Biological Science And Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/108Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/12Refining fats or fatty oils by distillation
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/16Refining fats or fatty oils by mechanical means

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention relates to hemp seed oil rich in cannabidiol and a preparation method thereof. The method comprises the following steps: shelling: carrying out shelling treatment on the dried fructus cannabis to obtain fructus cannabis and shells; crushing: crushing the dried hemp leaves and hemp seeds to obtain hemp material powder; and (3) extraction: performing subcritical extraction on the hemp material powder to obtain an extract liquid; desolventizing: evaporating the extract under reduced pressure to remove the extraction solvent to obtain an extraction concentrated solution; centrifuging: centrifuging the extraction concentrated solution to obtain supernatant, namely the cannabis sativa oil rich in cannabidiol. The method uses the compound of the hemp leaves and the hemp seeds as extraction raw materials, and obtains the hemp seed oil rich in cannabidiol (the content of the cannabidiol is 0.20-0.28%) by the subcritical extraction technology, and simultaneously, the method has higher oil yield and recovery rate (80% -95% and 25% -28% respectively).

Description

Hemp seed oil rich in cannabidiol and preparation method thereof
Technical Field
The invention relates to the technical field of hemp development, in particular to hemp seed oil rich in cannabidiol and a preparation method thereof.
background
The cannabis sativa, also known as China hemp and industrial hemp, is a herbaceous plant which has short sunshine, is annual and has palm-shaped division and is mostly male and female heterozygote, and is one of the traditional medicinal materials and health-care food raw materials in China. The national ministry of health 2002 documents list fructus cannabis in a list of articles which are both medicines and foods, so that the development and utilization of fructus cannabis foods are regulated and guaranteed. This also provides conditions and support for the development of the hemp plant leaves. In recent years, as people have been increasingly aware of cannabis and have been deeply studied about the strong physiological functions of processed products thereof, it is common in various countries to release the restriction on the development of cannabis and products thereof. With the continuous enlargement of the planting area of the cannabis sativa and the annual increase of the yield of the cannabis sativa. The oil content of the fructus cannabis is 30% -40%, the proportion of linoleic acid and linolenic acid is close to 2.5, and the proportion is the optimal proportion of fatty acid required by human body. The hemp seed oil is a high-quality substance with homology of medicine and food, contains rich trace mineral elements such as phosphorus, iron, potassium, magnesium, zinc and the like, also contains extremely rich phytosterol, can obviously reduce serum cholesterol through dietary intake, and has good antibacterial and anti-inflammatory effects; the gamma-tocopherol with the highest content in the hemp seed oil has obvious effects on coronary heart disease, tumor prevention and treatment, DNA loss reduction and the like; researchers have also found that hemp seed oil is suitable as an antioxidant dietary resource, which exceeds olive oil in terms of its ability to scavenge DPPH radicals; in addition, the hemp seed oil contains more than 60 phenolic chemical substances and has good oxidation resistance. Wherein Cannabidiol (CBD) is one of polyphenols. Unlike Tetrahydrocannabinol (THC), CBD is a non-addictive component, has the effects of blocking the influence of THC on human nervous system, and has a series of physiological activity functions of treating epilepsy, relieving fatigue, reducing blood fat, resisting thrombus and the like. Therefore, the hemp oil rich in CBD is prepared, the utilization value of the hemp plant by-products is improved, and the application range of the hemp plant by-products is extended to high-end products such as functional edible oil; and at present, an industrialized extraction process is not formed yet and is applied to the preparation of the cannabis oil rich in CBD, so that the product has a good market prospect.
The traditional edible oil preparation technology mainly adopts pre-pressing and solvent leaching, and then refines crude oil through processes of chemical degumming, chemical deacidification, high-temperature decolorization, high-temperature deodorization and the like, and the product mainly comprises first-grade oil and second-grade oil. The main disadvantage is that chemical reagents are used, natural active substances such as vitamin E, phytosterol and carotenoid in the oil are lost due to over-refining, and on the other hand, trans-fatty acid is easily generated in the high-temperature refining process and harmful substances such as polycyclic aromatic hydrocarbon are brought in. For example, CN1563306A discloses a preparation method and application of hemp seed oil, which comprises shelling, cold pressing, filtering, centrifuging to obtain cold pressed hemp seed oil, extracting cold pressed cake with propane or butane, refining the obtained extract oil, and performing antioxidant treatment to obtain refined hemp seed oil. CN 102816631A discloses a method for extracting hemp seed oil by an acid-method extrusion-puffing aqueous enzymatic method, which comprises the steps of pretreating hemp seeds by sulfuric acid, then carrying out extrusion-puffing, and then carrying out aqueous enzymatic oil preparation. CN 103289819A discloses a process for extracting fructus cannabis oil by supercritical carbon dioxide, which has the advantages of no pollution, no solvent residue, low extraction temperature, safe use and the like. But the supercritical extraction cost is too high, and the method is not suitable for popularization and application of industrial actual production. And the hemp seed oil prepared by the technology does not relate to the content measurement of the CBD component.
Disclosure of Invention
Based on the above, the invention provides the preparation method of the hemp seed oil rich in Cannabidiol (CBD), the oil yield of the preparation method is high, the prepared hemp seed oil is high in nutritive value, rich in cannabidiol, good in health care function and improved in added value of the product.
The specific technical scheme is as follows:
A method for preparing Cannabidiol (CBD) -rich hemp seed oil comprises the following steps:
(1) Shelling: carrying out shelling treatment on the dried fructus cannabis to obtain fructus cannabis and shells;
(2) Crushing: crushing the dried hemp leaves and hemp seeds to obtain hemp material powder;
(3) and (3) extraction: performing subcritical extraction on the hemp material powder to obtain an extract liquid;
(4) Desolventizing: evaporating the extract under reduced pressure to remove the extraction solvent to obtain an extraction concentrated solution;
(5) Centrifuging: centrifuging the extraction concentrated solution to obtain supernatant, namely the cannabis sativa oil rich in cannabidiol.
In some of these embodiments, the hemp leaves comprise 10% to 35% of the hemp seed by mass.
In some of these embodiments, the hemp leaves comprise 15% to 35% of the hemp seed by mass.
In some of these embodiments, the hemp leaves comprise 15% to 25% of the hemp seed by mass.
In some of these embodiments, the hemp leaves comprise 18% to 22% of the hemp seed by mass.
In some of the embodiments, the extraction solvent for subcritical extraction is butane and ethanol in a volume ratio of 1: 0-1.
In some of the embodiments, the extraction solvent for subcritical extraction is butane and ethanol in a volume ratio of 1: 0.4-0.6.
In some of these embodiments, the process parameters of the subcritical extraction include: the extraction pressure is 0.3-0.7MPa, the extraction temperature is 30-50 ℃, the extraction time is 0.5-3 hours, and the extraction times are 2-5 times.
In some embodiments, the volume ratio of the amount of the extraction solvent to the hemp material powder in the extraction step is 0.8-1.5: 1.
In some embodiments, the volume ratio of the amount of the extraction solvent to the hemp material powder in the extraction step is 0.9-1.1: 1.
in some of these embodiments, the moisture content of the dried hemp seed and the dried hemp leaf is no greater than 5%. If the raw materials contain much water, the raw materials are easy to mildew and agglomerate in the storage process, and most of the raw materials enter the product after extraction. Meanwhile, experiments show that when the water content of the raw material is more than 5%, the extracted product is turbid, the product quality and the extraction rate are influenced, and therefore the raw material needs to be properly dried.
in some embodiments, the particle size of the hemp material powder is 0.5-5 mm.
In some embodiments, the reduced pressure evaporation temperature is 30-65 ℃ and the pressure is 0.05-0.1 MPa.
In some of these embodiments, the reduced pressure evaporation temperature is 40-50 ℃.
In some embodiments, the rotation speed of the centrifugation is 4000-7000r/min, and the time is 5-10 min.
the invention also provides the cannabis sativa oil rich in cannabidiol.
The specific technical scheme is as follows:
Hemp seed oil rich in cannabidiol is prepared by the preparation method. The cannabidiol content of the cannabis sativa kernel oil rich in cannabidiol is 0.2-0.28%.
The hemp seed oil rich in cannabidiol and the preparation method thereof have the following advantages and beneficial effects:
The invention firstly uses the compound of the hemp leaves and the hemp seeds as the extraction raw material, and obtains the hemp seed oil rich in cannabidiol (the content of the cannabidiol is 0.2-0.28%) by the subcritical extraction technology, and simultaneously, the method has higher oil yield and recovery rate (80% -95% and 25% -28% respectively). The method is used for extracting at normal temperature or low temperature, can avoid thermal denaturation and oxidative denaturation of various functional components to the maximum extent, can retain the characteristics and nutritional ingredients of target products, and is rich in cannabidiol. The obtained hemp seed oil has high nutritive value, can be used as edible oil, has good health care function, can be developed into health care oil and oil for cosmetics, has extremely high added value of products, and is beneficial to the comprehensive utilization of hemp raw materials and the development and production of high added value products.
The proportion of the hemp leaves and hemp seeds in the raw materials to be extracted and the proportion of the extraction solvent to the raw materials are further optimized, and a composite solvent (butane and ethanol) and proper extraction process parameters are adopted in a matching manner, so that the high oil yield and the high content of cannabidiol in the obtained hemp seed oil can be better considered, and the high content of cannabidiol can be improved as far as possible while the high oil yield is ensured.
The method is a low-temperature and low-pressure processing process, has low energy consumption, can recycle the solvent in the extraction process, does not discharge three wastes, is an efficient, low-consumption, green and environment-friendly extraction technology, has the advantages of mild reaction, environmental friendliness, low energy consumption and production cost, simple operation, good product quality, high extraction efficiency and the like, and is very suitable for industrial production.
drawings
FIG. 1 is a graph showing the appearance of the hemp seed oil products obtained in example 1 and comparative example 1.
FIG. 2 is a gas phase diagram of a hemp seed oil product obtained in example 1 (upper panel) and comparative example 1 (lower panel).
Detailed Description
For a better understanding of the present invention, the following examples are given in connection with the accompanying drawings, which are not intended to limit the scope of the present invention. In the following examples and comparative examples, the Cannabidiol (CBD) content was determined by gas chromatography, with specific measurements as follows:
The measurement was carried out using an Agilent HP-5 column, model Agilent 7890A gas phase apparatus. The chromatographic conditions were as follows: the carrier gas is helium, and the flow rate is 1.00 ml/min; column temperature procedure: the initial temperature is 100 ℃, the temperature is kept for 5 minutes, the temperature is programmed to 250 ℃ at the speed of 10 ℃/minute, the temperature is raised to 300 ℃ at the speed of 5 ℃/minute, and the temperature is kept for 10 minutes; the temperature of a sample inlet is 250 ℃, the temperature of a detector is 250 ℃, and the split ratio is 10: 1; hydrogen flow rate 30 ml/min, air flow rate 300 ml/min; automatic sample injection is carried out, and the sample injection amount is 2.0 mu L. And preparing standard solutions with different concentrations, performing the operation, and drawing a peak area-CBD concentration standard curve. The sample volume of the sample solution is 2.0 mu L, and the content of CBD in the product is calculated according to the standard curve.
Example 1
A method for preparing cannabis sativa oil rich in Cannabidiol (CBD) comprises the following steps:
pretreatment of raw materials: cleaning folium Cannabis and fructus Cannabis with water, drying with vacuum drying equipment, squeezing fructus Cannabis to remove shell to obtain fructus Cannabis, and pulverizing folium Cannabis and fructus Cannabis (water content of 3%) to particle size of 1-5 mm.
Metering the volume of the crushed hemp leaves and hemp seeds (collectively called hemp material powder, wherein the hemp leaves account for 35 percent of the weight of the hemp seeds), filling the hemp leaves and the hemp seeds into a closed extraction tank, and mixing the materials according to the volume of the hemp material powder: injecting an extraction solvent with the volume of 1:1, mixing, and performing subcritical extraction; wherein the extraction solvent comprises butane and ethanol at a volume ratio of 1:0.5, the extraction pressure is 0.5MPa, the extraction temperature is 40 ℃, the extraction time is 2 hours, and the extraction times are 4 times;
Desolventizing: and after the last extraction is finished, carrying out reduced pressure evaporation to completely gasify subcritical butane and ethanol liquid, controlling the temperature at 45 ℃ and the pressure at 0.1MPa in the evaporation process, and finally discharging the extracted cannabis sativa extract concentrated solution from the bottom of the separation kettle.
Centrifuging: centrifuging the extracted concentrated solution at 4000r/min for 10min, and collecting the supernatant to obtain cannabis sativa oil rich in cannabidiol.
The extraction rate of the hemp seed oil extracted in the embodiment is 85%, the recovery rate is 26%, the peroxide value is 2.12mmol/kg, the acid value is 3.23mg/g (both the acid value is less than or equal to 4.0mg K/g, and the peroxide value is less than or equal to 7.0mmol/kg) which meet the sanitary standards for the acid value and the peroxide value of edible vegetable oil (crude oil) in the edible oil classification management in China, the saponification value (KOH) is 179mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 280ppm (see the upper graph in FIG. 2).
Example 2
A preparation method of cannabis sativa kernel oil rich in cannabidiol CBD comprises the following steps:
Pretreatment of raw materials: cleaning folium Cannabis and fructus Cannabis with water, drying with vacuum drying equipment, squeezing fructus Cannabis to remove shell to obtain fructus Cannabis, and pulverizing folium Cannabis and fructus Cannabis (water content of 4%) to particle size of 1-5 mm.
Metering the volume of the crushed hemp leaves and hemp seeds (collectively called hemp material powder, wherein the hemp leaves account for 10 percent of the weight of the hemp seeds), filling the hemp leaves and the hemp seeds into a closed extraction tank, and mixing the materials according to the volume of the hemp material powder: injecting an extraction solvent with the volume of 1:1, mixing, and performing subcritical extraction; wherein the extraction solvent comprises butane and ethanol at a volume ratio of 1:0.3, the extraction pressure is 0.3MPa, the extraction temperature is 30 deg.C, the extraction time is 3 hr, and the extraction times are 5 times.
Desolventizing: and after the last extraction is finished, carrying out reduced pressure evaporation to completely gasify subcritical butane and ethanol liquid, controlling the temperature at 45 ℃ and the pressure at 0.05 in the evaporation process, and finally discharging the extracted cannabis sativa extract concentrated solution from the bottom of the separation kettle.
Centrifuging: centrifuging the extracted concentrated solution at 7000r/min for 5min, and collecting the supernatant to obtain cannabis sativa oil rich in cannabidiol.
The hemp seed oil extracted in the example has the extraction rate of 90 percent, the recovery rate of 25 percent, the peroxide value of 2.61mmol/kg, the acid value of 3.73mg/g, the saponification value (KOH) of 170mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 203 ppm.
Example 3
A preparation method of cannabis sativa kernel oil rich in cannabidiol CBD comprises the following steps:
pretreatment of raw materials: cleaning folium Cannabis and fructus Cannabis with water, drying with vacuum drying equipment, squeezing fructus Cannabis to remove shell to obtain fructus Cannabis, and pulverizing folium Cannabis and fructus Cannabis (water content of 3%) to particle size of 1-5 mm.
Metering the volume of the crushed hemp leaves and hemp seeds (collectively called hemp material powder, wherein the hemp leaves account for 20 percent of the weight of the hemp seeds), filling the hemp leaves and the hemp seeds into a closed extraction tank, and mixing the materials according to the volume of the hemp material powder: injecting an extraction solvent with the volume of 1:1, mixing, and performing subcritical extraction; wherein the extraction solvent comprises butane and ethanol at a volume ratio of 1:1, the extraction pressure is 0.5MPa, the extraction temperature is 50 deg.C, the extraction time is 0.5 hr, and the extraction times are 5 times.
Desolventizing: and after the last extraction is finished, carrying out reduced pressure evaporation to completely gasify subcritical butane and ethanol liquid, controlling the temperature at 45 ℃ and the pressure at 0.1MPa in the evaporation process, and finally discharging the extracted cannabis sativa extract concentrated solution from the bottom of the separation kettle.
Centrifuging: centrifuging the extracted concentrated solution at 4000r/min for 10min, and collecting the supernatant to obtain cannabis sativa oil rich in cannabidiol.
The hemp seed oil extracted in the example has an extraction rate of 88%, a recovery rate of 27%, a peroxide value of 2.43mmol/kg, an acid value of 3.54mg/g, a saponification value (KOH) of 168mg/g, and a GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 265 ppm.
example 4
a method for preparing cannabidiol-enriched CBD-enriched hemp seed oil, which is basically the same as in example 1, and is different in that hemp leaves account for 5%, 20% and 50% of the weight of hemp seed, respectively, and the obtained cannabidiol-enriched hemp seed oil is respectively marked as hemp seed oil a, hemp seed oil B and hemp seed oil C.
the extraction rate of the hemp seed oil A is 91%, the recovery rate is 25%, the peroxide value is 2.15mmol/kg, the acid value is 3.35mg/g, the saponification value (KOH) is 176mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 135 ppm.
the extraction rate of the hemp seed oil B is 93 percent, the recovery rate is 28 percent, the peroxide value is 2.14mmol/kg, the acid value is 3.30mg/g, the saponification value (KOH) is 175mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 273 ppm.
the extraction rate of the hemp seed oil C is 65%, the recovery rate is 23%, the peroxide value is 2.10mmol/kg, the acid value is 2.15mg/g, the saponification value (KOH) is 170mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 282 ppm.
Example 5
A method of producing hemp seed oil enriched in cannabidiol CBD, substantially as in example 1, the difference being in the volume of hemp seed powder: the volumes of the solvents are respectively 1:0.5 and 1:3, and the prepared hemp seed oil rich in cannabidiol is respectively marked as hemp seed oil D and hemp seed oil E.
The extraction rate of the hemp seed oil D is 70%, the recovery rate is 25%, the peroxide value is 2.32mmol/kg, the acid value is 3.25mg/g, the saponification value (KOH) is 185mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 252 ppm.
The extraction rate of the hemp seed oil E is 73 percent, the recovery rate is 25 percent, the peroxide value is 2.31mmol/kg, the acid value is 3.20mg/g, the saponification value (KOH) is 180mg/g, and the GC analysis result shows that the content of Cannabidiol (CBD) in the hemp seed oil is 256 ppm.
Comparative example 1
A preparation method of cannabis sativa kernel oil rich in cannabidiol CBD comprises the following steps:
Pretreatment of raw materials: cleaning fructus Cannabis with water, drying with vacuum drying equipment, squeezing, removing shell to obtain fructus Cannabis (water content of 3%), and pulverizing to particle size of 1-5 mm.
And (2) measuring the volume of the crushed fructus cannabis, filling the crushed fructus cannabis into a closed extraction tank, and mixing the volume of the fructus cannabis powder: injecting an extraction solvent with the volume of 1:1, mixing, and performing subcritical extraction; wherein the extraction solvent comprises butane and ethanol at a volume ratio of 1:0.5, the extraction pressure is 0.5MPa, the extraction temperature is 40 deg.C, the extraction time is 2 hr, and the extraction times are 4 times.
Desolventizing: evaporating under reduced pressure to completely gasify subcritical butane and ethanol liquid after the last extraction, controlling the temperature at 45 deg.C and the pressure at 0.1MPa during evaporation, and discharging the extracted oleum Sesami (extraction concentrate) from the bottom of the separation kettle.
centrifuging: centrifuging the extracted cannabis oil at 4000r/min for 10min, and taking supernatant to obtain cannabis oil rich in cannabidiol.
The hemp seed oil extracted in this comparative example had an extraction rate of 91%, a recovery rate of 26%, a peroxide value of 2.41mmol/kg, an acid value of 2.91mg/g, a saponification value (KOH) of 124mg/g, and GC analysis showed that the content of Cannabidiol (CBD) in the hemp seed oil was 103ppm (see lower panel in FIG. 2).
the technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A preparation method of cannabis sativa oil rich in cannabidiol is characterized by comprising the following steps:
Shelling: carrying out shelling treatment on the dried fructus cannabis to obtain fructus cannabis and shells;
Crushing: crushing the dried hemp leaves and hemp seeds to obtain hemp material powder;
and (3) extraction: performing subcritical extraction on the hemp material powder to obtain an extract liquid;
desolventizing: evaporating the extract under reduced pressure to remove the extraction solvent to obtain an extraction concentrated solution;
Centrifuging: centrifuging the extraction concentrated solution to obtain supernatant, namely the cannabis sativa oil rich in cannabidiol.
2. A method of producing cannabidiol-enriched hemp seed oil as claimed in claim 1 wherein the hemp leaves comprise between 10% and 35% of the hemp seed mass.
3. A method of producing cannabidiol-enriched hemp seed oil as claimed in claim 2 wherein the hemp leaves comprise between 15% and 25% of the hemp seed mass.
4. A process for the preparation of cannabidiol-enriched hemp seed oil as claimed in any of claims 1 to 3 wherein the extraction solvent for the subcritical extraction is butane and ethanol in a volume ratio of 1:0 to 1.
5. a process for the preparation of cannabidiol-enriched hemp seed oil as claimed in any one of claims 1 to 3 wherein the process parameters of the subcritical extraction include: the extraction pressure is 0.3-0.7MPa, the extraction temperature is 30-50 ℃, the extraction time is 0.5-3 hours, and the extraction times are 2-5 times.
6. the method of any one of claims 1-3, wherein the volume ratio of the amount of extraction solvent used in the extraction step to the hemp seed powder is 0.8-1.5: 1.
7. A method of producing cannabidiol-enriched hemp seed oil as claimed in any one of claims 1 to 3, wherein the moisture content of the dried hemp seed and the dried hemp leaf is not more than 5%.
8. A process for the preparation of cannabidiol-enriched hemp seed oil as claimed in any of claims 1 to 3 wherein the hemp material powder has a particle size of 0.5 to 5 mm.
9. A process for the preparation of cannabidiol-enriched hemp seed oil as claimed in any one of claims 1 to 3 wherein the temperature of the reduced pressure evaporation is 30-65 ℃ and the pressure is 0.05-0.1 MPa; and/or the rotation speed of the centrifugation is 4000-7000r/min, and the time is 5-10 min.
10. Hemp seed oil enriched in cannabidiol, characterised in that it is obtained by a process according to any one of claims 1 to 9.
CN201810581523.8A 2018-06-07 2018-06-07 Hemp seed oil rich in cannabidiol and preparation method thereof Pending CN110577855A (en)

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CN112690453A (en) * 2020-12-30 2021-04-23 北京常春藤经贸有限责任公司 Composition, compound oil and application thereof

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CN105535111A (en) * 2016-02-16 2016-05-04 晋城市汉恩宝生物科技有限公司 Cannabis sailve extract rich in cannabidiol and preparation method of cannabis sailve extract
CN107898826A (en) * 2017-11-01 2018-04-13 云南谷益美农业开发有限公司 The preparation method of the numb medicinal extract of fire containing cannabidiol

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CN105061554A (en) * 2015-08-12 2015-11-18 晋城市汉恩宝生物科技有限公司 CBD (cannabidiol)-rich fructus cannabis concentrate protein powder and preparation method thereof
CN105535111A (en) * 2016-02-16 2016-05-04 晋城市汉恩宝生物科技有限公司 Cannabis sailve extract rich in cannabidiol and preparation method of cannabis sailve extract
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* Cited by examiner, † Cited by third party
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CN112690453A (en) * 2020-12-30 2021-04-23 北京常春藤经贸有限责任公司 Composition, compound oil and application thereof

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