CN112779092A - CBD refined oil special for cosmetics and preparation method thereof - Google Patents
CBD refined oil special for cosmetics and preparation method thereof Download PDFInfo
- Publication number
- CN112779092A CN112779092A CN202011541442.9A CN202011541442A CN112779092A CN 112779092 A CN112779092 A CN 112779092A CN 202011541442 A CN202011541442 A CN 202011541442A CN 112779092 A CN112779092 A CN 112779092A
- Authority
- CN
- China
- Prior art keywords
- cbd
- temperature
- solution
- decoloring
- ethanol solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of plant extraction, and discloses special CBD refined oil for cosmetics and a preparation method thereof, and particularly relates to colorless or yellowish transparent special CBD refined oil for cosmetics and a process method thereof, wherein the special CBD refined oil for cosmetics is prepared by using industrial hemp flowers and leaves as raw materials, adopting a carbon dioxide supercritical extraction technology and a physical adsorption decoloring technology, and performing ultralow-temperature dewaxing, decoloring, impurity removal, concentration, short-path molecular distillation, preparative chromatography precision separation and purification, and concentration.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and particularly relates to CBD refined oil special for cosmetics and a preparation method thereof.
Background
The industrial hemp CBD is a very safe and effective skin care ingredient. It has the functions of relieving, diminishing inflammation, activating cell and promoting cell regeneration. The additive amount of CBD in the product reaches 0.1 percent, so that the product has good effect and is an ideal effect additive. The CBD series of skin care products are considered to be an excellent solution for repair and anti-aging, applicable to all skin types, including sensitive skin. There may be a wider selection of CBD range skin care products by consumers in the coming years. Full spectrum (or broad spectrum) CBD oils, mainly have efficacy in skin: improving xerosis cutis, relieving pruritus, relieving itching, relieving inflammation, relieving dermatitis, acne, seborrhea, and hair growth disorder, and can be used for developing acne-removing, allergy-relieving, soothing, sunscreen, and hair caring products.
CBD has effects of promoting natural healing and anti-inflammatory, promoting skin hydration, and can be used for improving dermatitis symptoms such as acne, eczema and psoriasis. The skin care products added with the industrial hemp components are many, but the products added with the CBD components are few and few, and the industrial hemp cosmetic development and production can be really realized at home due to the high entry threshold and the technical bottleneck of separation and purification for extracting the CBD from the flowers and leaves of the industrial hemp. The report of CBD refined oil special for domestic research cosmetics is not found so far.
Disclosure of Invention
In order to solve the technical problems, the invention provides the CBD refined oil special for the cosmetics and the preparation method thereof, all solvents are safe and environment-friendly carbon dioxide and ethanol water systems, and the solvents are adsorbed and decolored by a physical method.
In order to achieve the purpose, the invention adopts the technical scheme that: a CBD refined oil special for cosmetics and a preparation method thereof comprise the following steps:
a CBD refined oil special for cosmetics and a preparation method thereof are characterized by comprising the following steps:
(1) pretreatment of raw materials: sieving the dried industrial hemp flowers and leaves by a vibrating screen to remove hemp seeds, hemp stalks and sandstone impurities;
(2) drying and crushing: drying the flower and leaf raw material obtained after pretreatment in the step (1) for 0.5-3 h at 95-125 ℃ by using hot air belt type drying equipment until the moisture content is less than 5%, and crushing the flower and leaf raw material to 60-100 meshes by using a crusher to obtain a primary raw material;
(3) carbon dioxide supercritical extraction: performing carbon dioxide supercritical extraction on the crushed primary raw material obtained in the step (2) to obtain an extract and residue with the CBD content of 10-15%;
(4) pretreatment: and (4) carrying out extraction on the CBD extract obtained in the step (3) according to the proportion of the concentrated extract to the absolute ethyl alcohol of 1: 8(w/w), uniformly mixing, freezing, degreasing and dewaxing at the ultralow temperature of-25 to-70 ℃ for 4 to 8 hours, and centrifuging and filtering to obtain a dewaxing treatment solution;
(5) primary silica gel decoloring: putting the dewaxing treatment liquid obtained in the step (4) on a silica gel column, carrying out adsorption decoloration by using silica gel with the sample loading amount of 2-4%, and eluting by using 95% (vol) food grade ethanol to obtain a first-stage decoloration treatment liquid;
(6) low-temperature concentration: carrying out vacuum reduced pressure low-temperature concentration on the decolorized solution obtained in the step (5) at-0.05 to-0.08 MPa, wherein the temperature is 50-55 ℃, and obtaining an intermediate product, namely a first-grade concentrated paste;
(7) and (3) secondary active carbon decolorization: and (4) conveying the dewaxed concentrated paste obtained in the step (6) to an activated carbon decoloring tank, and mixing the concentrated paste with absolute ethyl alcohol according to a ratio of 1: 10(w/w), uniformly mixing, adding 2-5% of activated carbon for decolorization, controlling the temperature to be 45-60 ℃ and the decolorization time to be 40-60min, and filtering and separating to obtain secondary decolorized liquid;
(8) low-temperature concentration: carrying out vacuum reduced low-temperature concentration on the secondary decolorized solution obtained in the step (7) at-0.05-0.08 MPa to obtain secondary decolorized intermediate CBD concentrated paste;
(9) molecular distillation: performing short-range molecular distillation on the CBD concentrated paste obtained in the step (8) at the temperature of 90-170 ℃, removing impurities with large molecular weight to obtain light phase components, and simultaneously fully decarboxylating and converting CBDA in the crude oil into CBD to obtain CBD full spectrum oil with the CBD content of 25-38%;
(10) industrial preparative chromatographic separation and purification: conveying the CBD full spectrum oil of the step (9) to a sample tank, and performing oil extraction on the CBD full spectrum oil by using a 1: 1, then loading the sample on a high-pressure chromatographic column with the sample loading amount of 30-50 mgCBD/mL, and adopting 50-95% ethanol solution (vol) for eluent analysis at the pressure of 20-40 bar; performing accurate separation by an industrial preparation high performance liquid chromatography system, firstly balancing with 40-60% ethanol solution, then carrying out analytical elution with 50-85% ethanol solution for 5-10 times of column volume to remove foreimpurities, then eluting with 50-95% ethanol solution for 5-10 times of column volume to elute target components, and collecting eluent rich in the target components to obtain CBD component enrichment solution; according to the atlas of CBD in the eluent, combining the detection result, accurately cutting the enriched liquid of the foreimpurity and CBD components into different storage tanks;
(11) and (3) decoloring and filtering with diatomite for three times: and (4) decoloring the CBD component liquid in the step (10) for 45-60 min by using an adsorption decoloring agent.
(12) Low-temperature vacuum concentration: and (3) carrying out vacuum reduced pressure low-temperature concentration on the decolorized liquid obtained in the step (11) at-0.05-0.08 MPa to obtain the CBD refined oil special for cosmetics, which is colorless, transparent or yellowish and has the CBD content of 30-60%.
Further, in the step (5), the elution time is 30-60 min.
Further, in the step (6), vacuum reduced pressure concentration is carried out at the pressure of-0.05 to-0.08 MPa and the temperature of 50 to 55 ℃.
Further, the method is characterized in that in the step (9), the vacuum degree during molecular distillation is 20-110 Pa.
Further, in the step (10), the adsorption medium of the chromatographic column is polyamide adsorption resin or octadecyl bonding modified silica gel resin.
Further, in the step (10), the sample loading amount is 30-50 mgCBD/mL, 50-95% ethanol solution (VOL) is adopted for analysis eluent, and the pressure is 20-40 bar.
Further, in the step (10), the analysis solution is balanced by 40-60% ethanol solution, then 50-85% ethanol solution is used for carrying out analysis elution for 5-10 times of column volume to remove the foreimpurities, and then 50-95% ethanol solution is used for eluting the target component for 5-10 times of column volume.
Further, in the step (11), the adsorption decolorant is one or more of diatomite, clay and kaolin.
The beneficial technical effects of the invention are as follows:
in the technical scheme of the invention, compared with CBD broad-spectrum oil with black brown or other colors obtained by the traditional process, the CBD refined oil special for cosmetics is finally obtained by three-stage decoloring process treatment.
According to the technical scheme, the pigment generated in the CBD broad-spectrum oil production and processing process is subjected to hierarchical decolorization treatment through a three-level decolorization process technology, and finally the final product is subjected to fine decolorization treatment through a physical adsorption decolorizer decolorization process, so that the colorless transparent or yellowish CBD refined oil special for cosmetics is obtained.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A CBD refined oil special for cosmetics and a preparation method thereof comprise the following steps:
(1) pretreatment of raw materials: sieving the dried industrial hemp flowers and leaves by a vibrating screen to remove hemp seeds, hemp stalks and sandstone impurities;
(2) drying and crushing: drying the flower and leaf raw material obtained after the pretreatment in the step (1) for 1.5h at 105 ℃ by using hot air belt type drying equipment to obtain a dried industrial hemp flower and leaf raw material with the moisture of less than 5%; crushing the raw materials to 90 meshes by a crusher to obtain a primary raw material of industrial hemp flowers and leaves;
(3) carbon dioxide supercritical extraction: performing carbon dioxide supercritical extraction on the crushed dried flower and leaf raw material obtained in the step (2) to obtain an extract and residue with the CBD content of 12%;
(4) pretreatment: and (4) carrying out extraction on the CBD extract obtained in the step (3) according to the proportion of the concentrated extract to the absolute ethyl alcohol of 1: 8(w/w), uniformly mixing, freezing, degreasing and dewaxing at the ultralow temperature of-50 ℃ for 6 hours, and centrifuging and filtering to obtain a dewaxing treatment solution;
(5) primary silica gel decoloring: putting the dewaxing treatment liquid obtained in the step (4) on a silica gel column, carrying out adsorption and decoloration by using silica gel with the sample loading amount of 2%, and eluting by using 95% (vol) food grade ethanol to obtain a primary decoloration treatment liquid;
(6) low-temperature concentration: concentrating the decolorized solution obtained in step (5) at-0.07 MPa under reduced pressure and low temperature at 50 deg.C to obtain intermediate product of first-grade concentrated paste;
(7) and (3) secondary active carbon decolorization: and (4) conveying the dewaxed concentrated paste obtained in the step (6) to an activated carbon decoloring tank, and mixing the concentrated paste with absolute ethyl alcohol according to a ratio of 1: 10(w/w), uniformly mixing, adding activated carbon for decoloring, wherein the use amount of the decolored activated carbon is 3% (w/w), the temperature is 50 ℃, the decoloring time is 45min, and filtering and separating to obtain secondary decolored liquid;
(8) low-temperature concentration: carrying out vacuum reduced pressure low-temperature concentration on the secondary decolorized solution obtained in the step (7) at-0.07 MPa to obtain secondary decolorized intermediate CBD concentrated paste;
(9) molecular distillation: performing short-range molecular distillation on the CBD concentrated paste obtained in the step (8) at the temperature of 165 ℃ and the vacuum degree of 30Pa, removing high-molecular-weight impurities to obtain a light-phase component, and simultaneously fully decarboxylating and converting CBDA in the concentrated paste into CBD to obtain CBD full-spectrum oil with the CBD content of 31%;
(10) industrial preparative chromatographic separation and purification: conveying the CBD full spectrum oil of the step (9) to a sample tank, and performing oil extraction on the CBD full spectrum oil by using a 1: 1, then loading the sample on a high-pressure chromatographic column with the sample loading of 40mgCBD/mL, and adopting 75% ethanol solution (vol) as an analytical eluent at the pressure of 30 bar; the separation is carried out accurately by an industrial preparative high performance liquid chromatography system. Balancing with 55% ethanol solution, eluting with 70% ethanol solution 10 times the column volume to remove impurities, eluting with 80% ethanol solution 10 times the column volume to elute target components, and collecting eluate rich in target components to obtain CBD component enriched solution; according to the atlas of CBD in the eluent, combining the detection result, accurately cutting the enriched liquid of the foreimpurity and CBD components into different storage tanks;
(11) and (3) decoloring and filtering with diatomite for three times: coating the CBD component solution obtained in the step (10) with diatomite and argil, wherein the dosage of an adsorption decolorant is 10%, and then performing cyclic decoloration and filtration for 50min through a diatomite filter;
(12) low-temperature vacuum concentration: and (3) concentrating the filtrate obtained in the step (11) at 50 ℃ under vacuum and reduced pressure at-0.07 MPa to obtain the special CBD refined oil for cosmetics, which is colorless and transparent and has the CBD content of 56%.
Example 2
A CBD refined oil special for cosmetics and a preparation method thereof comprise the following steps:
(1) pretreatment of raw materials: sieving the dried industrial hemp flowers and leaves by a vibrating screen to remove hemp seeds, hemp stalks and sandstone impurities;
(2) drying and crushing: drying the flower and leaf raw material obtained after pretreatment in the step (1) for 1.5h at 121 ℃ by using hot air belt type drying equipment to obtain a dried industrial hemp flower and leaf raw material with the moisture of less than 5%; crushing the raw materials into 80 meshes by a crusher to obtain a primary raw material of industrial hemp flowers and leaves;
(3) carbon dioxide supercritical extraction: performing carbon dioxide supercritical extraction on the crushed dried flower and leaf raw material obtained in the step (2) to obtain an extract and residue with the CBD content of 11%;
(4) pretreatment: and (4) carrying out extraction on the CBD extract obtained in the step (3) according to the proportion of the concentrated extract to the absolute ethyl alcohol of 1: 8(w/w), evenly mixing, freezing, degreasing and dewaxing at the ultralow temperature of-60 ℃ for 6 hours, and centrifuging and filtering to obtain the dewaxing treatment fluid.
(5) Primary silica gel decoloring: putting the dewaxing treatment liquid obtained in the step (4) on a silica gel column, carrying out adsorption and decoloration by using silica gel with the sample loading amount of 3%, and eluting by using 95% (vol) food grade ethanol to obtain a primary decoloration treatment liquid;
(6) low-temperature concentration: concentrating the decolorized solution obtained in step (5) at-0.07 MPa under reduced pressure and low temperature at 50 deg.C to obtain intermediate product of first-grade concentrated paste;
(7) and (3) secondary active carbon decolorization: and (4) conveying the dewaxed concentrated paste obtained in the step (6) to an activated carbon decoloring tank, and mixing the concentrated paste with absolute ethyl alcohol according to a ratio of 1: 10(w/w), uniformly mixing, adding activated carbon for decolorization, wherein the use amount of the decolorized activated carbon is 3.5% (w/w), the temperature is 50 ℃, the decolorization time is 60min, and filtering and separating to obtain secondary decolorized liquid;
(8) low-temperature concentration: carrying out vacuum reduced pressure low-temperature concentration on the secondary decolorized solution obtained in the step (7) at-0.07 MPa and 50 ℃ to obtain a secondary decolorized intermediate CBD concentrated paste;
(9) molecular distillation: carrying out short-range molecular distillation on the CBD concentrated paste obtained in the step (8) at the temperature of 170 ℃ and the vacuum degree of 70Pa, removing impurities with large molecular weight to obtain a light phase component, and simultaneously fully decarboxylating and converting the CBDA in the concentrated paste into CBD to obtain CBD full-spectrum oil with the CBD content of 34%;
(10) industrial preparative chromatographic separation and purification: conveying the CBD full spectrum oil of the step (9) to a sample tank, and performing oil extraction on the CBD full spectrum oil by using a 1: 1, then loading the sample on a high-pressure chromatographic column with the sample loading of 50mgCBD/mL, and adopting 65% ethanol solution (vol) as an analytical eluent at the pressure of 30 bar; the separation is carried out accurately by an industrial preparative high performance liquid chromatography system. Balancing with 50% ethanol solution, eluting with 65% ethanol solution 10 times the column volume to remove impurities, eluting with 80% ethanol solution 10 times the column volume to elute target components, and collecting eluate rich in target components to obtain CBD component enriched solution; according to the CBD map in the eluent, accurately cutting the enriched liquid of the foreimpurity and CBD components into different storage tanks by combining the detection result;
(11) and (3) bleaching and filtering with carclazyte for the third time: coating the CBD component liquid obtained in the step (10) with argil, wherein the consumption of an adsorption decolorant is 10%, and then performing cyclic decoloration and filtration for 60min through a diatomite filter;
(12) low-temperature vacuum concentration: and (3) concentrating the filtrate obtained in the step (11) at 50 ℃ under vacuum and reduced pressure at-0.07 MPa to obtain the CBD refined oil special for cosmetics, which is yellowish in color and has the CBD content of 50.3%.
Example 3
A CBD refined oil special for cosmetics and a preparation method thereof comprise the following steps:
(1) pretreatment of raw materials: sieving the dried industrial hemp flowers and leaves by a vibrating screen to remove hemp seeds, hemp stalks and sandstone impurities;
(2) drying and crushing: drying the flower and leaf raw material obtained after the pretreatment in the step (1) for 1h at 125 ℃ by using hot air belt type drying equipment to obtain a dry industrial hemp flower and leaf raw material with the moisture of less than 5%; crushing the raw materials into 80 meshes by a crusher to obtain a primary raw material of industrial hemp flowers and leaves;
(3) carbon dioxide supercritical extraction: performing carbon dioxide supercritical extraction on the crushed dried flower and leaf raw material obtained in the step (2) to obtain an extract and residue with the CBD content of 12.5%;
(4) pretreatment: and (4) carrying out extraction on the CBD extract obtained in the step (3) according to the proportion of the concentrated extract to the absolute ethyl alcohol of 1: 8(w/w), evenly mixing, freezing, degreasing and dewaxing at the ultralow temperature of-65 ℃ for 5 hours, and centrifuging and filtering to obtain the dewaxing treatment fluid.
(5) Primary silica gel decoloring: and (3) putting the dewaxing treatment liquid obtained in the step (4) on a silica gel column, carrying out adsorption and decoloration by using silica gel, and eluting by using 95% (vol) food-grade ethanol to obtain a primary decoloration treatment liquid.
(6) Low-temperature concentration: concentrating the decolorized solution obtained in step (5) at-0.07 MPa under reduced pressure and low temperature at 50 deg.C to obtain intermediate product of first-grade concentrated paste;
(7) and (3) secondary active carbon decolorization: and (4) conveying the dewaxed concentrated paste obtained in the step (6) to an activated carbon decoloring tank, and mixing the concentrated paste with absolute ethyl alcohol according to a ratio of 1: 10(w/w) and adding active carbon for decoloring. Decolorizing with activated carbon at 50 deg.C for 60min at 3% (w/w), filtering, and separating to obtain secondary decolorized solution;
(8) low-temperature concentration: carrying out vacuum reduced pressure low-temperature concentration on the secondary decolorized solution obtained in the step (7) at-0.07 MPa and 50 ℃ to obtain a secondary decolorized intermediate CBD concentrated paste;
(9) molecular distillation: performing short-range molecular distillation on the CBD concentrated paste obtained in the step (8) at the temperature of 180 ℃ and the vacuum degree of 110Pa, removing impurities with large molecular weight to obtain light-phase components, and simultaneously fully decarboxylating and converting CBDA in the concentrated paste into CBD to obtain CBD full-spectrum oil with the CBD content of 35.5%;
(10) industrial preparative chromatographic separation and purification: conveying the CBD full spectrum oil of the step (9) to a sample tank, and performing oil extraction on the CBD full spectrum oil by using a 1: 1, then loading the sample on a high-pressure chromatographic column with the sample loading of 45mgCBD/mL, and adopting 67% ethanol solution (vol) as an analytical eluent at the pressure of 30 bar; the separation is carried out accurately by an industrial preparative high performance liquid chromatography system. Balancing with 55% ethanol solution, eluting with 65% ethanol solution 10 times the column volume to remove impurities, eluting with 75% ethanol solution 10 times the column volume to elute target components, and collecting eluate rich in target components to obtain CBD component enriched solution; according to the CBD map in the eluent, accurately cutting the enriched liquid of the foreimpurity and CBD components into different storage tanks by combining the detection result;
(11) and (3) carrying out third decolorization and filtration: and (3) carrying out combined decolorization on the CBD component liquid obtained in the step (10) by using diatomite, kaolin and clay, wherein the total consumption of an adsorption decolorizer is 8%, and the proportion of the diatomite, the kaolin and the clay is 5: 3: 2, coating, and then performing circulating decoloration filtration for 60min by using a diatomite filter to obtain decoloration filtrate.
(12) Low-temperature vacuum concentration: and (3) concentrating the filtrate obtained in the step (11) at 50 ℃ under vacuum and reduced pressure at-0.07 MPa to obtain the special CBD refined oil for cosmetics, which is colorless and transparent and has the CBD content of 52%.
Data comparison of CBD essential oil specially used for preparing cosmetics for three times
The invention relates to CBD refined oil special for cosmetics and a preparation method thereof, and the finally obtained CBD broad-spectrum oil is colorless transparent or micro-butter-shaped liquid, and the CBD content is more than 50 percent. The CBD broad-spectrum oil finally obtained by the invention does not contain any other organic solution and solid residue, is CBD refined oil special for cosmetics and a preparation method thereof, and has important significance for CBD extraction of industrial hemp leaves.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Those of ordinary skill in the art will understand that: the components in the devices in the embodiments may be distributed in the devices in the embodiments according to the description of the embodiments, or may be correspondingly changed in one or more devices different from the embodiments. The components of the above embodiments may be combined into one component, or may be further divided into a plurality of sub-components.
Finally, it should be noted that: although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.
Claims (10)
1. A CBD refined oil special for cosmetics and a preparation method thereof are characterized by comprising the following steps:
(1) pretreatment of raw materials: sieving the dried industrial hemp flowers and leaves by a vibrating screen to remove hemp seeds, hemp stalks and sandstone impurities;
(2) drying and crushing: drying the flower and leaf raw material obtained after pretreatment in the step (1) for 0.5-3 h at 95-125 ℃ by using hot air belt type drying equipment until the moisture content is less than 5%, and crushing the flower and leaf raw material to 60-100 meshes by using a crusher to obtain a primary raw material;
(3) carbon dioxide supercritical extraction: performing carbon dioxide supercritical extraction on the crushed primary raw material obtained in the step (2) to obtain an extract and residue with the CBD content of 10-15%;
(4) pretreatment: and (4) carrying out extraction on the CBD extract obtained in the step (3) according to the proportion of the concentrated extract to the absolute ethyl alcohol of 1: 8(w/w), uniformly mixing, freezing, degreasing and dewaxing at the ultralow temperature of-25 to-70 ℃ for 4 to 8 hours, and centrifuging and filtering to obtain a dewaxing treatment solution;
(5) primary silica gel decoloring: putting the dewaxing treatment liquid obtained in the step (4) on a silica gel column, carrying out adsorption decoloration by using silica gel with the sample loading amount of 2-4%, and eluting by using 95% (vol) food grade ethanol to obtain a first-stage decoloration treatment liquid;
(6) low-temperature concentration: carrying out vacuum reduced pressure low-temperature concentration on the decolorized solution obtained in the step (5) at-0.05 to-0.08 MPa, wherein the temperature is 50-55 ℃, and obtaining an intermediate product, namely a first-grade concentrated paste;
(7) and (3) secondary active carbon decolorization: and (4) conveying the dewaxed concentrated paste obtained in the step (6) to an activated carbon decoloring tank, and mixing the concentrated paste with absolute ethyl alcohol according to a ratio of 1: 10(w/w), uniformly mixing, adding 2-5% of activated carbon for decolorization, controlling the temperature to be 45-60 ℃ and the decolorization time to be 40-60min, and filtering and separating to obtain secondary decolorized liquid;
(8) low-temperature concentration: carrying out vacuum reduced low-temperature concentration on the secondary decolorized solution obtained in the step (7) at-0.05-0.08 MPa to obtain secondary decolorized intermediate CBD concentrated paste;
(9) molecular distillation: performing short-range molecular distillation on the CBD concentrated paste obtained in the step (8) under the conditions of 20-110 Pa and 90-170 ℃, removing impurities with large molecular weight to obtain light-phase components, and simultaneously fully decarboxylating and converting CBDA in the crude oil into CBD to obtain CBD full-spectrum oil with the CBD content of 25-38%;
(10) industrial preparative chromatographic separation and purification: conveying the CBD full spectrum oil of the step (9) to a sample tank, and performing oil extraction on the CBD full spectrum oil by using a 1: 1, then loading the sample on a high-pressure chromatographic column with the sample loading amount of 30-50 mgCBD/mL, and adopting 50-95% ethanol solution (vol) for eluent analysis at the pressure of 20-40 bar; performing accurate separation by an industrial preparation high performance liquid chromatography system, firstly balancing with 40-60% ethanol solution, then carrying out analytical elution with 50-85% ethanol solution for 5-10 times of column volume to remove foreimpurities, then eluting with 50-95% ethanol solution for 5-10 times of column volume to elute target components, and collecting eluent rich in the target components to obtain CBD component enrichment solution; according to the atlas of CBD in the eluent, combining the detection result, accurately cutting the enriched liquid of the foreimpurity and CBD components into different storage tanks;
(11) and (3) decoloring and filtering with diatomite for three times: and (4) decoloring the CBD component liquid in the step (10) for 45-60 min by using an adsorption decoloring agent.
(12) Low-temperature vacuum concentration: and (3) carrying out vacuum reduced pressure low-temperature concentration on the decolorized liquid obtained in the step (11) at-0.05-0.08 MPa to obtain the CBD refined oil special for cosmetics, which is colorless and transparent or yellowish and has the CBD content of 30-60%.
2. The method according to claim 1, wherein in the step (5), the elution time is 30 to 60 min.
3. The method according to claim 1, wherein in the step (6), the vacuum concentration is carried out at a pressure of-0.05 to-0.08 MPa and a temperature of 50 to 55 ℃.
4. The method according to claim 1, wherein in the step (9), the molecular distillation is performed under a vacuum degree of 20 to 110Pa and at a temperature of 90 ℃ to 170 ℃.
5. The method as claimed in claim 1, wherein in step (10), the adsorption medium of the chromatographic column is polyamide adsorption resin or octadecyl bonding modified silica gel resin.
6. The method according to claim 1, wherein in the step (10), the sample loading amount is 30 to 50mgCBD/mL, the desorption eluent is 50 to 95% ethanol solution (VOL), and the pressure is 20 to 40 bar.
7. The method according to claim 1, wherein in the step (10), the solution is a 40-60% ethanol solution, the solution is a 50-85% ethanol solution, the elution precursor is 5-10 times the column volume, the solution is a 50-95% ethanol solution, and the elution volume is 5-10 times the column volume.
8. The method of claim 1, wherein in step (11), the adsorption decolorant is one or more of diatomite, clay and kaolin.
9. The method of claim 1, wherein in step (11), the adsorption decoloring time is 40-60 min.
10. A cosmetic CBD refined oil produced by the method of any of claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011541442.9A CN112779092A (en) | 2020-12-23 | 2020-12-23 | CBD refined oil special for cosmetics and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011541442.9A CN112779092A (en) | 2020-12-23 | 2020-12-23 | CBD refined oil special for cosmetics and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112779092A true CN112779092A (en) | 2021-05-11 |
Family
ID=75751955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011541442.9A Withdrawn CN112779092A (en) | 2020-12-23 | 2020-12-23 | CBD refined oil special for cosmetics and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112779092A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113652305A (en) * | 2021-07-27 | 2021-11-16 | 中南林业科技大学 | Elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and preparation method thereof |
-
2020
- 2020-12-23 CN CN202011541442.9A patent/CN112779092A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113652305A (en) * | 2021-07-27 | 2021-11-16 | 中南林业科技大学 | Elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107011125B (en) | Method for enriching cannabidiol | |
| Tan et al. | Extraction and purification of anthocyanins: A review | |
| Zagklis et al. | Purification of grape marc phenolic compounds through solvent extraction, membrane filtration and resin adsorption/desorption | |
| CN103626814A (en) | Method for separating anthocyanins monomer from lycium ruthenicum fruits | |
| CN101003557A (en) | Method for preparing extractive of olive leaves rich in oleuropein in high purity | |
| CN112661613A (en) | Method for industrial clean production of cannabidiol CBD broad-spectrum oil | |
| CN103467540A (en) | Method for extracting salidroside from rhodiola | |
| CN102285953A (en) | Method for separating and purifying blueberry anthocyanidin by using HP2MGL macroporous resin | |
| CN102766125A (en) | Extraction and purification method for black rice anthocyanin | |
| CN110724589B (en) | Method for preparing cannabidiol and coproducing cannabis full spectrum oil | |
| CN106074263B (en) | Herbal extract and application thereof in cosmetics | |
| CN103232346A (en) | Production process for extraction of chlorogenic acid from green coffee bean | |
| CN102851114A (en) | Method for extracting grape seed oil and proanthocyanidin | |
| CN112661612A (en) | Method for large-scale preparation of high-purity CBD through post-decarboxylation and supercritical extraction | |
| Gu et al. | Purification of R-phycoerythrin from Gracilaria lemaneiformis by centrifugal precipitation chromatography | |
| CN110981921B (en) | Continuous method for synchronously extracting multiple effective components from figs | |
| CN112779092A (en) | CBD refined oil special for cosmetics and preparation method thereof | |
| CN111393539A (en) | Preparation method for co-producing tea polysaccharide, theanine and caffeine in summer and autumn tea | |
| CN110786513A (en) | Method for extracting and purifying hemp full spectrum oil | |
| CN1272331C (en) | Method of extracting effective components in kudzu vine root | |
| CN103333922B (en) | High-yield cinnabarin obtaining method | |
| CN102432420A (en) | Method for extracting and separating beta-elemene from Lantana camara | |
| CN103936563B (en) | A kind of method extracting trans-resveratrol from grape vine | |
| CN102432419A (en) | Method for extracting and separating beta-elemene from Eupatorium adenophorum | |
| CN113801003A (en) | Industrial extraction method of cannabidiol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210511 |