CN112048377A - Extraction method of cannabis oil rich in polyphenol - Google Patents
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Abstract
The invention discloses a method for extracting cannabis oil rich in polyphenol, and belongs to the technical field of edible oil processing. The method comprises the following steps of (1) firstly adjusting the moisture content of the hemp seeds, and then pretreating the hemp seeds by microwaves; (2) crushing the pretreated hemp seeds, taking n-hexane as an extraction solvent, extracting for 30 minutes at the ultrasonic temperature of 30 ℃ and the ultrasonic power of 120W, wherein the material-liquid ratio is 1:7g/ml, and carrying out vacuum distillation on the ultrasonic material liquid after suction filtration to obtain crude hemp seed oil; (3) decolorizing with activated carbon adsorption to obtain fragrant oleum Sesami. The extraction process of the invention greatly improves the oil yield of the hemp seeds, which can reach 39.25 percent, and all basic indexes of the hemp seeds accord with the national standard. In addition, compared with the traditional prepared cannabis oil, the cannabis sativa oil prepared by the invention has the advantages that the content of tetrahydrocannabinol is obviously reduced, the content of other plant polyphenols is obviously improved, and the cannabis sativa oil has high nutritional and health-care values.
Description
Technical Field
The invention relates to a method for extracting cannabis oil rich in polyphenol, and belongs to the technical field of edible oil processing.
Background
The cannabis sativa is also named as hemp, black sesame and the like, belongs to the cannabis genus of Moraceae family, is one of traditional medicinal materials and health care raw materials in China, and is listed in the list of articles which are not only medicines but also foods. Hemp oil extracted from fructus cannabis is the most common household oil in the Guangxi Bama area of China, and is also representative of long-life food in the Bama area. The content of unsaturated fatty acid in oleum Sesami is up to 90%, wherein the content of polyunsaturated fatty acid is 70-80%, and the content of linoleic acid and alpha-linolenic acid are 50-70% and 15-25%. Research shows that the hemp seed oil has certain auxiliary curative effects of easing pain, resisting inflammation, regulating blood pressure, preventing cardiovascular and cerebrovascular diseases and the like because of rich nutrient components.
Plant polyphenol, also known as plant tannin, is a secondary metabolite of the largest variety in plants and is commonly found in vegetables, fruits, Chinese herbal medicines and plant seeds. Research has found that polyphenol has activities of antioxidation, antibiosis and antivirus; in practical application, the health-care food has the effects of resisting browning, reducing blood sugar and blood pressure, preventing cardiovascular diseases and the like. In the food industry, plant polyphenol is used as an active substance for resisting oxidation and scavenging free radicals, can prevent the automatic oxidation of oil and has good antioxidation effect on oil and food containing oil. In addition, the plant polyphenol also has good bacteriostatic effect, so the plant polyphenol can be widely used as a preservative in the preservation of foods rich in animal and vegetable oil and the like. Cannabinoids are a class of plant polyphenols and are also the major active ingredients in cannabis plants. The main cannabinoids in cannabis include Tetrahydrocannabinol (THC), Cannabidiol (CBD), Cannabinol (CBN), Cannabigerol (CBG), etc. Wherein THC has illusive effect on human body, so as to reduce the content of tetrahydrocannabinol, increase the content of other plant polyphenols in the cannabis sativa oil, and improve the application value of the cannabis sativa oil.
There are several patents disclosing the preparation of cannabis oil and methods for increasing the polyphenol content of vegetable oils. For example, patent CN 107418710 a discloses a preparation method of hemp oil, which comprises drying hemp seeds and preparing the hemp oil by squeezing; patent CN 106554847 a discloses a preparation method of tea oil rich in tea polyphenol, which mainly comprises the steps of squeezing, purifying, column loading, alkali extraction, water washing, concentrating and the like on tea leaves and tea oil seeds, so as to improve the content of tea polyphenol in the tea oil; patent CN 109439427A discloses a preparation method of peony seed meal oil rich in polyphenol, wherein the seed meal oil rich in polyphenol is obtained by mixing ethanol and cake meal, heating and refluxing, centrifugal separation and reduced pressure concentration.
The various methods disclosed in the above patents have the problems of complicated processing technology, low oil yield, resource waste and the like, and lack of relevant researches on the cannabis oil rich in plant polyphenol. Therefore, a method for preparing the hemp seed oil rich in plant polyphenol, which has simple processing technology and high oil yield and can meet the requirement of industrial development, is urgently needed.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing hemp seed oil rich in polyphenol by microwave pretreatment and ultrasonic extraction coupling. The method can improve the oil yield of the hemp seeds, effectively reduce the content of tetrahydrocannabinol and improve the content of other plant polyphenols.
The invention discloses a method for extracting hemp seed oil rich in polyphenol, which comprises the steps of pretreating hemp seeds by microwaves, crushing the pretreated hemp seeds, and extracting by using an ultrasonic-assisted extraction solvent to obtain the hemp seed oil.
In one embodiment of the invention, the water content of the hemp seeds is controlled to be 8-12% before microwave pretreatment, and the percentage is mass percent.
In one embodiment of the present invention, the microwave power is 600-1000W, and the microwave time is 6-10 min.
In one embodiment of the invention, the extraction solvent comprises one or more of n-hexane, petroleum ether and diethyl ether.
In one embodiment of the present invention, the feed-liquid ratio of the hemp seeds to the extraction solvent is 1: (10-20), unit: g/mL.
In one embodiment of the present invention, the ultrasound-assisted extraction conditions are: the temperature is 20-40 ℃, the ultrasonic power is 100-300W, and the extraction time is 20-40 min.
In one embodiment of the invention, the material liquid after ultrasonic treatment is filtered and then is distilled under reduced pressure to obtain crude cannabis oil, the crude cannabis oil is centrifuged, and impurities are removed to obtain cannabis crude oil; adding the hemp crude oil into a reaction kettle, adding activated carbon for reaction, and separating to obtain the fragrant hemp oil.
The invention discloses hemp seed oil obtained by applying the method; the content of polyphenol in the hemp oil is higher than 70mg/100g, and the content of tetrahydrocannabinol in the hemp oil is lower than 60 mg/kg.
The invention discloses application of the hemp seed oil in the fields of food, chemical industry and pharmacy.
The invention discloses a cannabis oil soft capsule, which is prepared by mixing the cannabis oil and walnut oil serving as raw materials according to a mass ratio of (2-10) to 1, and adding gelatin. The prepared soft capsule has the characteristics of high nutritive value and food therapy.
The invention discloses an anti-inflammation and stasis-removing essential oil, which comprises 80-90% of the cannabis sativa oil, 1-5% of sweet osmanthus fragrans champ essential oil, 1-5% of aloe essential oil and 1-5% of tea tree essential oil. The essential oil has the advantages of promoting blood circulation, removing blood stasis, diminishing inflammation, relieving pain, moistening skin and the like.
The invention has the beneficial effects that:
compared with the prior art, the invention has the beneficial effects that: the preparation process of the hemp seed oil rich in polyphenol provided by the invention utilizes a microwave pretreatment coupled ultrasonic extraction mode, is beneficial to instantaneous rupture of cell walls and organisms of hemp seeds, enhances release of oil and active ingredients in cells, promotes more oil to be extracted, develops a new process of a hemp seed oil technology, is beneficial to improvement of the added value of hemp resources, and is simple in preparation process and easy to realize industrialization. The sesame oil prepared by the method has the oil yield of 39.25 percent, the polyphenol content of 95.28mg/100g, the tetrahydrocannabinol content of 57.33mg/kg, and the prepared sesame oil has good color and flavor and strong fragrance of the hemp.
Drawings
FIG. 1 is a graph showing the effect of microwave power on the polyphenol content of hemp oil;
FIG. 2 is a graph showing the effect of microwave time on the polyphenol content of hemp oil;
FIG. 3 is a graph showing the effect of water content in the raw materials on the polyphenol content of cannabis oil.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The method for measuring the content of polyphenol in the cannabis oil comprises the following steps:
(1) activating a diol-based solid phase extraction column by using 10mL of methanol and 10mL of n-hexane in sequence at the flow rate of 2.0 mL/min;
(2) accurately weighing 3g (accurate to 0.001g) of cannabis oil, dissolving in 5mL of n-hexane, enabling the solution to pass through a diol-based solid-phase extraction column at the flow rate of 1.0mL/min, then leaching the extraction column with 10mL of n-hexane, discarding all effluent liquid, finally eluting with 10mL of methanol, collecting all eluent, drying with weak nitrogen in a 45 ℃ water bath, dissolving residues in 2mL of methanol-water solution, carrying out vortex oscillation for 1min, freezing for 16h at-18 ℃, centrifuging for 5min at 10000rpm at 4 ℃, taking supernatant, and testing.
(3) Transferring 1mL of gallic acid working solution, water (blank) and sample solution to be detected into a graduated test tube by using a pipette, adding 0.5mL of forinophenol reagent, 2mL of 7.5% sodium carbonate solution and 6.5mL of water, carrying out vortex oscillation for 1min, reacting in a 70 ℃ water bath for 30min, and measuring the absorbance under the condition of 750nm wavelength by using a 10mm cuvette. If the absorbance is not between 0.1 and 0.8, the sample weighing of the sample to be measured or the dilution of the solution to be measured should be properly adjusted, and then the measurement is carried out again.
(4) And drawing a standard curve according to the absorbance (A) of the gallic acid working solution and the concentration of the gallic acid in each working solution.
The content of phenolic substances in the cannabis oil is calculated according to the following formula.
In the formula:
x-the polyphenol content in vegetable oil in milligrams per kilogram (mg/kg);
c-the concentration of polyphenols, in micrograms per milliliter (. mu.g/mL), was determined from a standard curve;
d is the dilution multiple of the sample after constant volume, if the sample is not diluted, D is 1;
2-volume of the eluent is fixed after evaporation to dryness, and the unit is milliliter (mL);
m is the sample mass in grams (g).
The conditions for sample solution preparation were: accurately weighing 1g (accurate to 0.001g) of cannabis oil in a 15mL centrifuge tube, adding 5mL of methanol, vortexing, shaking and uniformly mixing for 60s, centrifuging, taking the supernatant in another 15mL centrifuge tube, repeatedly extracting for two times, combining the supernatants, placing the combined supernatant in a horizontal position at-20 ℃ for 2h, taking 10mL of the supernatant, drying the supernatant under N2, adding 2mL of acetonitrile for redissolving, and filtering the supernatant through a 0.22 mu m polytetrafluoroethylene filter membrane to obtain a sample solution to be detected.
Tetrahydrocannabinol detection conditions:
(1) chromatographic conditions are as follows: a chromatographic column: hypersil GOLD C18 column (100X 2.1mm, 1.9 μm). Mobile phase: phase A was ultrapure water (containing 0.1% acetic acid) and phase B was acetonitrile (containing 0.1% acetic acid). The gradient elution procedure was: 0-8min, 40-90% B; 8-12min, 90% B; 12-13min, 90-40% B; 13-20min, 40% B. The sample introduction amount was 2. mu.L, the flow rate was 0.3mL/min, and the column temperature was 35 ℃.
(2) Mass spectrum conditions: electrospray ion source (ESI), Multiple Reaction Monitoring (MRM) mode, negative ion scanning mode. The capillary voltage is 3kV, the ion source temperature is 110 ℃, the desolvation temperature is 400 ℃, desolvation gas and taper hole gas are both N2, the desolvation gas flow rate is 600L/h, and the taper hole gas flow rate is 50L/h.
Example 1:
(1) uniformly spraying water on the hemp seed raw material, and standing at 4 ℃ for 24 hours, wherein the water content of the hemp seed is controlled to be 9%.
(2) Treating the hemp seeds by using microwave treatment equipment, and simultaneously inspecting the influence of different microwave powers and microwave times on the polyphenol content in the hemp seed oil, wherein the microwave power is 600-1000W, and the microwave time is 6-10 min;
(3) crushing pretreated hemp seeds, taking n-hexane as an extraction solvent, extracting for 30min at the ultrasonic temperature of 30 ℃ and the ultrasonic power of 120W according to the material-liquid ratio of 1:7g/ml, carrying out suction filtration on the ultrasonic feed liquid, carrying out reduced pressure distillation to obtain crude hemp seed oil, centrifuging the collected hemp seed oil for 5min at 5000r/min, removing impurities to obtain hemp crude oil, and storing at 4 ℃ for detection;
(4) adding crude oil into a reaction kettle, adding 4% equivalent of activated carbon, stirring under 0.1MPa, heating at 110 deg.C for 30min, cooling, centrifuging at 4500r/min for 15min, and separating to obtain oleum Sesami with faint scent.
As shown in FIG. 1, the microwave pretreatment can significantly increase the polyphenol content in the hemp oil, and the polyphenol content increases and then decreases with the increase of the microwave power, and the polyphenol content reaches the highest value when the microwave power is 800W.
As can be seen from FIG. 2, the microwave pretreatment can significantly increase the polyphenol content in the hemp oil, and the polyphenol content increases first and then decreases with the increase of the microwave time, and the polyphenol content reaches the highest value when the microwave time is 8 min. According to the implementation method, the determination shows that under the conditions that the water content is 9%, the microwave power is 800W and the time is 8min, the oil yield of the cannabis oil is 39.25%, the polyphenol content is 95.28mg/100g, and the tetrahydrocannabinol content is remarkably reduced to 57.33 mg/kg.
Example 2:
(1) uniformly spraying water on the hemp seed raw material, and standing at 4 ℃ for 24 hours, wherein the water content of the hemp seed is controlled to be 8%.
(2) Treating the hemp seeds by using microwave treatment equipment, wherein the microwave power is 800W, and the microwave time is 8 min;
(3) crushing pretreated hemp seeds, taking n-hexane as an extraction solvent, extracting for 30min at the ultrasonic temperature of 30 ℃ and the ultrasonic power of 120W according to the material-liquid ratio of 1:7g/ml, carrying out suction filtration on the ultrasonic feed liquid, carrying out reduced pressure distillation to obtain crude hemp seed oil, centrifuging the collected hemp seed oil for 5min at 5000r/min, removing impurities to obtain hemp crude oil, and storing at 4 ℃ for detection;
(4) adding crude oil into a reaction kettle, adding 4% equivalent of activated carbon, stirring under 0.1MPa, heating at 110 deg.C for 30min, cooling, centrifuging at 4500r/min for 15min, and separating to obtain fragrant oleum Sesami; through determination, the oleum Sesami oil yield under the condition is 35.58%, the polyphenol content is 73.59mg/100g, and the tetrahydrocannabinol content is 60.37 mg/kg.
Example 3:
(1) uniformly spraying water on the hemp seed raw material, and standing at 4 ℃ for 24 hours, wherein the water content of the hemp seed is controlled to be 12%.
(2) Treating the hemp seeds by using microwave treatment equipment, wherein the microwave power is 800W, and the microwave time is 8 min;
(3) crushing pretreated hemp seeds, taking n-hexane as an extraction solvent, extracting for 30min at the ultrasonic temperature of 30 ℃ and the ultrasonic power of 120W according to the material-liquid ratio of 1:7g/ml, carrying out suction filtration on the ultrasonic feed liquid, carrying out reduced pressure distillation to obtain crude hemp seed oil, centrifuging the collected hemp seed oil for 5min at 5000r/min, removing impurities to obtain hemp crude oil, and storing at 4 ℃ for detection;
(4) adding crude oil into a reaction kettle, adding 4% equivalent of activated carbon, stirring under 0.1MPa, heating at 110 deg.C for 30min, cooling, centrifuging at 4500r/min for 15min, and separating to obtain fragrant oleum Sesami; through determination, the oleum Sesami oil yield under the condition is 32.98%, the polyphenol content is 87.69mg/100g, and the tetrahydrocannabinol content is 62.42 mg/kg.
As can be seen from FIG. 3, the moisture content of the raw materials also had an effect on the polyphenol content of the hemp oil, with the highest polyphenol content at a moisture content of 9%.
Example 4:
(1) uniformly spraying water on the hemp seed raw material, and standing at 4 ℃ for 24 hours, wherein the water content of the hemp seed is controlled to be 9%.
(2) Treating the hemp seeds by using microwave treatment equipment, wherein the microwave power is 800W, and the microwave time is 8 min;
(3) crushing pretreated hemp seeds, taking n-hexane as an extraction solvent, extracting for 30min at the ultrasonic temperature of 30 ℃ and the ultrasonic power of 120W according to the material-liquid ratio of 1:7g/ml, carrying out suction filtration on the ultrasonic feed liquid, carrying out reduced pressure distillation to obtain crude hemp seed oil, centrifuging the collected hemp seed oil for 5min at 5000r/min, removing impurities to obtain hemp crude oil, and storing at 4 ℃ for detection;
(4) adding crude oil into a reaction kettle, adding 2% equivalent of activated carbon, stirring under 0.1MPa, heating at 110 deg.C for 30min, cooling, centrifuging at 4500r/min for 15min, and separating to obtain fragrant oleum Sesami; through determination, the content of polyphenol in the cannabis sativa oil under the condition is 85.47mg/100g, and the content of tetrahydrocannabinol in the cannabis sativa oil is 65.36 mg/kg.
Example 5: essential oil for diminishing inflammation and dissipating blood stasis
The essential oil formula is mainly prepared from the following components in percentage by volume: 90% of hemp oil, 2% of cinnamon essential oil, 5% of aloe essential oil and 3% of tea tree essential oil. The essential oil has the advantages of promoting blood circulation, removing blood stasis, diminishing inflammation, relieving pain, moistening skin and the like.
Example 6: hemp seed oil soft capsule
A cannabis oil soft capsule is prepared by mixing the cannabis oil and walnut oil according to a mass ratio of 5:1, and adding gelatin to prepare the cannabis oil soft capsule. The prepared soft capsule has the characteristics of high nutritive value and food therapy.
Comparative example 1:
hemp seeds were treated as in example 1, with the difference that: microwave treatment and ultrasonic treatment are omitted, the hemp seeds are directly extracted by normal hexane after being crushed, and other conditions are the same as those in example 1. The determination shows that the sesame oil yield is 25.68%, the polyphenol content is 33.79mg/100g, and the tetrahydrocannabinol content is 65.41 mg/kg.
Comparative example 2:
the hemp seeds were pretreated by microwave as in example 1, with the difference that: and (3) directly extracting the pretreated hemp seeds by using normal hexane, omitting ultrasonic extraction, and performing other detection processes in the same way as in example 1. The determination shows that the sesame oil yield is 28.51 percent, the polyphenol content is 66.25mg/100g, and the tetrahydrocannabinol content is 68.58 mg/kg.
Comparative example 3:
the fructus cannabis is directly extracted by ultrasonic after being crushed, and the method is different from the method in the embodiment 1 in that the microwave pretreatment is omitted, and the other conditions are the same as the embodiment 1. The determined oil yield of the cannabis sativa oil is 32.49%, the polyphenol content is 36.25mg/100g, and the tetrahydrocannabinol content is 82.63 mg/kg.
Comparative example 4:
the fructus cannabis is pretreated by an oven, the heating temperature is 140 ℃, and the treatment time is 30 min. The preparation method and detection process of cannabis oil are the same as example 1. The difference from example 1 is the pretreatment of the hemp seed. The determination shows that the sesame oil yield is 31.19%, the polyphenol content is 45.39mg/100g, and the tetrahydrocannabinol content is 79.33 mg/kg.
Comparative example 5:
the fructus Cannabis is pretreated by infrared at 140 deg.C for 30 min. The preparation method and detection process of cannabis oil are the same as example 1. The difference from example 1 is the pretreatment of the hemp seed. Through determination, the oil yield of the cannabis sativa oil is 33.68%, the polyphenol content is 53.84mg/100g, and the tetrahydrocannabinol content is 72.65 mg/kg.
Combining the above examples and comparative examples, it was found that: (1) the moisture content of the hemp seeds has influence on the pretreatment and the polyphenol content in the hemp oil, when the moisture content of the hemp seeds is too low, a burnt taste is generated in the pretreatment process, active substances are damaged, the polyphenol content is reduced, the oil yield is reduced due to the high moisture content, and the polyphenol content is also reduced; (2) the microwave treatment power and time have important influence on the quality of the hemp seed oil, the microwave treatment power is low, the microwave treatment time is short, the moisture migration in the hemp seeds is not obvious, the release efficiency of trace substances of the hemp seed oil is low, the polyphenol content is obviously lower than the content under the optimal condition, the microwave treatment time is too high, and the components in the hemp seeds can be damaged, so that the polyphenol content is reduced; (3) the ultrasonic action not only can obviously improve the oil yield of the hemp seeds, but also can further improve the content of the plant polyphenol in the hemp seed oil on the premise of microwave pretreatment. Therefore, the microwave pretreatment and the ultrasonic extraction are coupled, so that the oil yield of the hemp seeds can be effectively improved, the content of tetrahydrocannabinol in the hemp seed oil is obviously reduced, the content of other plant polyphenols is improved, and the synergistic effect is realized.
TABLE 1 comparison of the oil yield and polyphenol content of the hemp oil of the examples and comparative examples
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for extracting cannabis oil rich in polyphenol is characterized by comprising the steps of pretreating cannabis seeds by microwaves, crushing the pretreated cannabis seeds, and extracting by using an ultrasonic-assisted extraction solvent to obtain the cannabis oil.
2. The method of claim 1, wherein the moisture content of the hemp seeds is controlled to be 8-12% before the microwave pretreatment; the microwave power is 600-1000W, and the microwave time is 6-10 min.
3. The method of claim 1 or 2, wherein the extraction solvent comprises one or more of n-hexane, petroleum ether, and diethyl ether.
4. The method according to any one of claims 1 to 3, wherein the feed-to-liquid ratio of the hemp seed to the extraction solvent is 1: (10-20).
5. The method according to any one of claims 1 to 4, wherein the ultrasound-assisted extraction conditions are: the temperature is 20-40 ℃, the ultrasonic power is 100-300W, and the extraction time is 20-40 min.
6. The method according to any one of claims 1 to 5, wherein the ultrasonically treated feed liquid is subjected to suction filtration and then is subjected to reduced pressure distillation to obtain crude cannabis oil, the crude cannabis oil is centrifuged, and impurities are removed to obtain cannabis crude oil; adding the hemp crude oil into a reaction kettle, adding activated carbon for reaction, and separating to obtain the fragrant hemp oil.
7. A hemp oil obtained by the method of any one of claims 1 to 6; the content of polyphenol in the hemp oil is higher than 70mg/100g, and the content of tetrahydrocannabinol in the hemp oil is lower than 60 mg/kg.
8. The use of the cannabis oil of claim 7 in the food, chemical and pharmaceutical fields.
9. A cannabis oil soft capsule is characterized in that the preparation method of the soft capsule is to mix the cannabis oil and walnut oil according to the mass ratio of (2-10) to 1, and then add gelatin to prepare the cannabis oil soft capsule.
10. An anti-inflammatory and stasis-removing essential oil, which is characterized in that the essential oil formula comprises 80-90% of the cannabis sativa oil, 1-5% of the cinnamomum subavenium essential oil, 1-5% of the aloe essential oil and 1-5% of the tea tree essential oil according to claim 7.
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