CN108434050B - Supercritical extraction method of traditional Chinese medicine, traditional Chinese medicine extract and application of traditional Chinese medicine extract in shampoo - Google Patents
Supercritical extraction method of traditional Chinese medicine, traditional Chinese medicine extract and application of traditional Chinese medicine extract in shampoo Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9771—Ginkgophyta, e.g. Ginkgoaceae [Ginkgo family]
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/006—Antidandruff preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/12—Preparations containing hair conditioners
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q7/00—Preparations for affecting hair growth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/81—Preparation or application process involves irradiation
Abstract
The invention discloses a supercritical extraction method of traditional Chinese medicine, traditional Chinese medicine extract and application in shampoo, wherein the extraction method comprises the following steps: drying the Chinese medicinal composition, pulverizing, and breaking cell wall; performing supercritical extraction on the Chinese medicinal powder. The supercritical carbon dioxide fluid is used as a solvent for critical extraction, has the characteristics of low-temperature extraction and inertia protection, effectively improves the extraction efficiency of effective substances, can extract beneficial components in the traditional Chinese medicine to the maximum extent by extracting after processing and breaking the walls of the traditional Chinese medicine, prevents oxidation and dissipation of sensitive substances, avoids the activity loss of the beneficial components, can completely avoid any organic solvent in the extraction process, and keeps the full naturalness of the extract. The shampoo prepared from the Chinese medicinal extract has effects of nourishing blood, nourishing yin, nourishing, improving eyesight, dispelling pathogenic wind, preventing fever, blackening hair and beard, removing dandruff, relieving itching, nourishing scalp and hair, and promoting hair growth.
Description
Technical Field
The invention relates to a supercritical extraction method of traditional Chinese medicine, a traditional Chinese medicine extract and application in shampoo.
Background
The shampoo is a product which is mainly compounded by taking a surfactant as a main body, has the effects of cleaning the scalp and hair of a person and keeping the beauty of the scalp and hair, and is a daily chemical product which is used by people in large amount in daily life. The shampoo comprises the components of a surfactant, a stabilizer, a functional additive, a preservative, essence and the like, wherein the proper surfactant can achieve the effects of abundant foam, low stimulation, high cleanliness and weak degreasing capability, and the shampoo is not only a hair cleanser, but also has good hair care and hairdressing effects, and can make hair bright, beautiful and smooth after hair washing.
The main trend of shampoo products is to develop towards medium-high grade, functionality and component naturalization. The future shampoo is to enable hair to be easily combed, prevent dandruff from generating, thoroughly clean dandruff, nourish hair roots, remove peculiar smell of hair quality, enable hair to be healthier and brighter, leave pleasant fragrance after washing, and feel fresh and comfortable.
The product efficacy of the shampoo is more and more important, and the special function and the auxiliary function are continuously refined. Moistening and nourishing, natural efficacy, natural hairdressing, freshness, refreshing and the like are the development trends in the future. In addition to the traditional concepts of dandruff removal and the like, the concepts of sun protection, vitamins, fruit acids, natural extraction of animal/plant essences, Chinese herbal medicine conditioning, hair treatment, no-clean hair moistening and the like also permeate into the fields of hair washing and hair care in a dispute, and become new bright points of the shampoo.
At present, a medicament with small side effect and capable of effectively treating hair problems is urgently needed, and a Chinese herbal medicine formula has the advantages of safety, small side effect, simplicity, easiness in searching, high price, compatibility with people and the like. There is a wide demand for such shampoos by many groups.
Disclosure of Invention
In order to make up for the defects of the prior art, through years of research and experiments, the invention provides a traditional Chinese medicine supercritical extraction method, a traditional Chinese medicine extract and application in shampoo, and the shampoo is prepared from pure natural Chinese herbal medicines as main raw materials.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a supercritical extraction method of traditional Chinese medicine comprises the following steps: drying the Chinese medicinal composition to water content of 5-9wt%, and pulverizing to 30-100 mesh to obtain Chinese medicinal powder; mixing the traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: (0.002-0.005): (0.01-0.03) adding the mixture into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extract in a 3-7 deg.C environment for 80-120min, centrifuging to remove impurities, and vacuumizing in a vacuum box at 25-65 deg.C for 6-10h to obtain Chinese medicinal extract.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the Chinese medicinal composition to water content of 5-9wt%, and pulverizing to 30-100 mesh to obtain Chinese medicinal powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: (0.01-0.03), performing enzymolysis at 45-55 deg.C for 1-3h, and performing microwave treatment for 2-5min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: (0.002-0.005): (0.01-0.03) adding the mixture into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extract in a 3-7 deg.C environment for 80-120min, centrifuging to remove impurities, and vacuumizing in a vacuum box at 25-65 deg.C for 6-10h to obtain Chinese medicinal extract.
Preferably, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 1-10 parts of fleece-flower root, 1-10 parts of angelica, 1-10 parts of ligusticum wallichii, 1-10 parts of ginseng and 1-10 parts of pseudo-ginseng.
Preferably, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 3-9 parts of semen cuscutae, 3-9 parts of cistanche, 4-10 parts of radix rehmanniae and 4-10 parts of polygonum multiflorum.
Preferably, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 3-12 parts of ginkgo leaf, 1-10 parts of glossy privet fruit, 1-10 parts of sharpleaf galangal fruit, 1-10 parts of cassia occidentalis and 1-10 parts of tribulus terrestris.
Preferably, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 5-15 parts of amomum cardamomum, 5-15 parts of entada phaseoloides, 4-10 parts of marigold flower, 0.2-0.5 part of eucommia bark and 1-3 parts of Chinese fevervine.
The drying temperature is 35-45 ℃; the microwave power of the microwave treatment is 300-600W, and the microwave frequency is 2400-2500 MHz.
The stabilizer is catechin and/or eriodictyol. Preferably, the stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: (0.3-0.7).
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: (0.5-1.5): (3-7) mixing.
The supercritical extraction pressure is 30-45Mpa, extraction temperature is 30-50 deg.C, extraction time is 50-180min, and CO is added2The flow rate of the fluid is 10-20 kg/h.
The auxiliary extraction agent is lauric acid glyceride or sucrose decanoate.
A Chinese medicinal extract is prepared by supercritical extraction method.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo comprises the following raw materials in percentage by mass: 0.3-5% of traditional Chinese medicine extract and 4-20% of surfactant.
The surfactant is at least one of anionic surfactant, cationic surfactant, zwitterionic surfactant and non-ionic surfactant, the anionic surfactant can be selected from sodium lauryl sulfate, potassium lauryl phosphate, sodium lauryl polyether sulfate and sodium cocoyl glutamate, the cationic surfactant can be selected from cetyl trimethyl ammonium bromide and lauryl dimethyl benzyl ammonium chloride, the zwitterionic surfactant can be selected from cocamidopropyl betaine and 3-sulfopropyl hexadecyl dimethyl betaine, and the non-ionic surfactant can be polyoxyethylene hydrogenated castor oil, polyoxyethylene laurate and sodium lauryl polyether sulfate.
Preferably, the shampoo is prepared from the following raw materials in percentage by mass: 0.3-5% of traditional Chinese medicine extract, 5-7% of sodium cocoyl glutamate, 5-8% of cocamidopropyl betaine, 3-5% of sodium laureth sulfate and the balance of water.
The supercritical carbon dioxide fluid is used as a solvent for critical extraction, has the characteristics of low-temperature extraction and inertia protection, effectively improves the extraction efficiency of effective substances, can extract beneficial components in the traditional Chinese medicine to the maximum extent by extracting after processing and breaking the walls of the traditional Chinese medicine, prevents oxidation and dissipation of sensitive substances, avoids the activity loss of the beneficial components, can completely avoid any organic solvent in the extraction process, and keeps the full naturalness of the extract. The shampoo prepared from the Chinese medicinal extract has effects of nourishing blood, nourishing yin, nourishing, improving eyesight, dispelling pathogenic wind, preventing fever, blackening hair and beard, removing dandruff, relieving itching, nourishing scalp and hair, and promoting hair growth.
Detailed Description
ABTS (2, 2-diaza-bis (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt) radical scavenging ability test:
dissolving ABTS in methanol to prepare an ABTS solution of 7 mmol/L; mixing 5mL of ABTS solution with 88 mu L of 140mmol/L potassium thiosulfate solution, and standing overnight at room temperature in the dark to form ABTS+·Stock solution, ABTS to be produced+·Diluting the stock solution with methanol to make its absorbance at 734nm wavelength be 0.70 + -0.02 to obtain ABTS+·And (4) working fluid. ABTS taking+·Adding 4mL of working solution into test tubes with plugs, respectively adding 0.04g of Chinese medicinal extract, mixing uniformly by vortex, reacting in water bath at 30 deg.C for 15min, measuring absorbance A at 734nm, and making 3 replicates for each wine sample. A blank test was also run with 0.04g of methanol instead of antioxidant solution, and each concentration was measured in parallel 3 times. ABTS was calculated according to the following formula+·The clearance rate of (c):
ABTS+·clearance (%) ([ 1-A/A0)]× 100%, wherein A is the absorbance value of the sample solution, and A0 is the absorbance value of the blank solution.
And (3) testing the antibacterial performance:
the beef extract peptone agar culture medium for bacterial culture has the following specific formula: 3.0g of beef extract, 10g of peptone, 5.0g of sodium chloride, 20g of agar and 1000mL of water are heated to melt, and the pH value is adjusted to 7.4-7.6. Subpackaging, and sterilizing under high pressure and moist heat (121 deg.C, 20min) for use.
Strain: staphylococcus aureus (Staphylococcus aureus), Escherichia coli (Escherichia coli).
Transferring all tested strains to corresponding test tube slant culture medium, and repeating the inoculation of each strain. The bacteria are cultured in a biochemical incubator at 37 ℃ for 24h, and the mould is cultured at 28 ℃ for 48 h. 2 of each strain was used for the experiment, and the rest was refrigerated for further use.
Selecting each colony, inoculating to a plate, culturing for 24 hr, and preparing the colony with sterile normal saline to obtain 10-containing bacteria7CFU/mL of bacterial suspension. The preparation method comprises the following steps: respectively selecting a small amount of bacterial spores, washing with sterile normal saline, scattering glass beads, making into bacterial suspension, and adjusting the concentration of the bacterial suspension to 107CFU/mL, spare.
And (3) carrying out dry heat sterilization on a circular blank filter paper sheet with the diameter of 3cm at 160 ℃, and storing the blank filter paper sheet for later use under the aseptic condition. 0.1mL of each activated experimental bacterial suspension with the bacterial liquid concentration adjusted is sucked by a sterile pipettor and added into a culture dish poured with the culture medium, and the bacterial suspension is uniformly coated by a self-made glass coater sterilized by dry heat. Then, the filter paper sheets are clamped by using sterile tweezers and placed on different bacteria-containing culture dishes, 10 mu L of oral care solution is absorbed on each filter paper sheet by using a sterile pipettor, and each bacteria is made into two dishes in parallel. The corresponding extraction solvent was then used as a negative control. Culturing the bacteria in a biochemical incubator at a constant temperature of 37 ℃ for 24h, measuring the diameter of a bacteriostatic circle by a cross method, and taking an average value.
The raw materials in the examples are introduced:
sucrose decanoate, CAS number: 31835-06-0.
Sodium cocoyl glutamate, CAS No.: 68187-32-6.
Cocamidopropyl betaine, CAS No.: 86438-79-1.
Sodium laureth sulfate, CAS No.: 9004-82-4. In the embodiment of the invention, sodium laureth sulfate which is provided by Japan Kao corporation and has the model of EMAL 270S is adopted.
Polygonum multiflorum (Fallopia multiflora (Thunb.) Harald.) called Stephania cochinchinensis is a perennial twisted vine of Polygonum genus of Polygonaceae family, and is dark brown. The fleece-flower root has obvious effects of nourishing liver and kidney, benefiting essence and blood, strengthening bones and muscles, blacking hair, soothing nerves, stopping juice and the like. Can be used for treating blood deficiency, dizziness, asthenia, and sallow complexion; deficiency of liver and kidney essence and blood, vertigo, tinnitus, soreness and weakness of waist and knees, and early white hair; hyperlipidemia. The Chinese medicine fleece-flower root has the components of raw fleece-flower root and prepared fleece-flower root. The fleece-flower root adopted in the embodiment of the invention is prepared fleece-flower root, and has the functions of tonifying essence and blood, blackening beard and hair, strengthening bones and muscles and tonifying liver and kidney. In the embodiment of the invention, the polygonum multiflorum is purchased from four-medicine industry marketing limited company of Anhui province, China.
Angelica sinensis (Angelica sinensis), also known as Angelica sinensis (oliv.) Diels and Angelica shilaena, is the root of Angelica sinensis (oliv.) Diels of Umbelliferae. Has effects in nourishing blood, regulating menstruation, relieving pain, moistening dryness, smoothing intestine, resisting cancer, resisting aging, and enhancing immunity. In the embodiment of the invention, the angelica is purchased from dendrobium nobile drug industry sales limited company in Bozhou city.
Rhizoma Ligustici Chuanxiong (Ligusticum chuanxiong Hort), also called Shanju, XIANGGUO, is dried rhizome of Umbelliferae plant rhizoma Ligustici Chuanxiong. The "Rihuazi materia Medica" records: for treating wind, qi, strain, blood, internal fatigue, strengthening bones and muscles, dredging channels, breaking symptoms, nourishing blood, promoting granulation, relieving rhinorrhea, hematemesis, hematuria, hemorrhoid, fistula, cerebral carbuncle, back pain, scrofula, wart, scabies, pus discharge and blood stasis. In the embodiment of the invention, the ligusticum chuanxiong hort is purchased from Yu Yan Fang Chinese medicinal material limited company in the Annational city.
Ginseng (Panax ginseng c.a.mey), a perennial herbaceous plant. Ginseng has been classified as "superior" throughout the history. In Shen nong Ben Cao Jing, it is considered that Ginseng has the effects of tonifying five internal organs, calming the mind, stopping palpitation, eliminating pathogenic factors, improving eyesight, and improving intelligence. In the embodiment of the invention, ginseng is purchased from Yu Yan Fang Chinese medicinal material limited company in the Annational city.
Notoginseng radix is plant of Araliaceae of Umbelliferae. The root of the pseudo-ginseng is used as the medicinal part, and has the effects of removing blood stasis, stopping bleeding, reducing swelling and relieving pain. The compendium of materia Medica is recorded in Shi Yi (supplement to compendium of materia Medica): ginseng, radix Ginseng and Notoginseng are the most precious of the Chinese herbs, because it tonifies qi the first, and it tonifies blood the first, and its flavor is the same and the same. In the embodiment of the invention, pseudo-ginseng is purchased from Xiangguang medicinal materials Co., Ltd.
Catechin, CAS No.: 7295-85-4.
Eriodictyol, CAS: 552-58-9,
The cellulase is food-grade cellulase with the enzyme activity of 10 ten thousand U/g provided by Wuhan Baixing biological science and technology limited company.
The pectinase is food grade pectinase with the enzyme activity of 20 ten thousand U/g, which is provided by Wuhan Baixing biotechnology limited company.
Example 1
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing traditional Chinese medicine powder, a stabilizer and an auxiliary extracting agent according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizer is catechin.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 2
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizer is catechin.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 3
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, and performing enzymolysis at 50 deg.C for 2 hr to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The temperature of the drying was 40 ℃.
The stabilizer is catechin.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 4
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizer is catechin.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The auxiliary extraction agent is lauric glyceride.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 5
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizing agent is eriodictyol.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 6
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 500g of polygonum multiflorum, 600g of angelica, 600g of ligusticum wallichii, 400g of ginseng and 400g of pseudo-ginseng.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: 0.5, and mixing.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 7
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 700g of dodder, 600g of cistanche, 600g of rehmannia root and 800g of fleece-flower root.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: 0.5, and mixing.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 8
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 800g of ginkgo leaf, 400g of glossy privet fruit, 500g of sharpleaf galangal fruit, 500g of cassia seed and 500g of tribulus terrestris.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: 0.5, and mixing.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Example 9
The traditional Chinese medicine composition is prepared by mixing the following raw materials: 900g of amomum cardamomum, 800g of entada phaseoloides, 600g of marigold flower, 25g of eucommia bark and 200g of Chinese fevervine.
The supercritical extraction method of the traditional Chinese medicine comprises the following steps: drying the traditional Chinese medicine composition until the water content is 7 wt%, and then crushing to 50 meshes to obtain traditional Chinese medicine powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: 0.02 mixing, performing enzymolysis at 50 deg.C for 2h, and performing microwave treatment for 3min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: 0.003: 0.02 adding the extract into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extraction product in 5 deg.C environment, maintaining the temperature for 100min, centrifuging at 6000r/min for 20min to remove bottom precipitate impurities, and vacuumizing the supernatant in 45 deg.C vacuum box for 8h to obtain Chinese medicinal extract.
The drying temperature is 40 ℃; the microwave power of the microwave treatment is 500W, and the microwave frequency is 2450 MHz.
The stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: 0.5, and mixing.
The enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: 1: 5, mixing the components.
The supercritical extraction pressure is 35Mpa, the extraction temperature is 40 deg.C, the extraction time is 120min, and CO is added2The flow rate of the fluid was 15 kg/h.
The extraction aid is sucrose decanoate.
The application of the traditional Chinese medicine extract in shampoo.
The shampoo is prepared from the following raw materials in percentage by mass: 2% of traditional Chinese medicine extract, 6% of sodium cocoyl glutamate, 7% of cocamidopropyl betaine, 4% of sodium laureth sulfate and the balance of water. Heating water to 50 deg.C, adding other materials, and stirring to obtain shampoo.
Test example 1
The extracts of the chinese herbs of examples 1-6 were tested for their ability to scavenge free radicals and inhibit bacteria. Specific results are shown in table 1.
Table 1: ABTS free radical clearance data sheet
The Chinese medicine extract adopts supercritical IIThe carbon oxide fluid is used as a solvent for critical extraction, the process is researched and improved, microwave treatment is carried out after enzymolysis, the plant cell walls are destroyed, and beneficial components are extracted more easily; the effective components of the traditional Chinese medicine are easy to be converted and decomposed under the influence of light, oxygen and temperature, and a stabilizing agent is added to prevent the conversion and decomposition in the extraction process; CO 22The fluid has limited dissolving capacity for some components, and CO is further improved by adding an extraction aid2Extracting effective components by using a fluid; the method has the characteristics of low-temperature extraction and inertia protection, prevents oxidation and dissipation of 'sensitive' substances, enables extraction and separation to be easily combined into a whole, effectively improves the extraction efficiency of effective substances, can extract beneficial components in the traditional Chinese medicine to the maximum extent by extraction after the traditional Chinese medicine is processed and wall-broken, can completely avoid any organic solvent in the extraction process, and keeps the full naturalness of the extract. The Chinese medicinal extract has effects in nourishing blood, nourishing yin, improving eyesight, dispelling pathogenic wind, preventing fever, blackening hair and beard, removing dandruff, relieving itching, nourishing scalp and hair, and promoting hair growth.
Claims (3)
1. A supercritical extraction method of traditional Chinese medicine is characterized by comprising the following steps: drying the Chinese medicinal composition to water content of 5-9wt%, and pulverizing to 30-100 mesh to obtain Chinese medicinal powder; mixing the traditional Chinese medicine powder and the enzyme solution according to a mass ratio of 1: (0.01-0.03), performing enzymolysis at 45-55 deg.C for 1-3h, and performing microwave treatment for 2-5min to obtain pretreated Chinese medicinal powder; mixing pretreated traditional Chinese medicine powder, a stabilizer and an extraction aid according to a mass ratio of 1: (0.002-0.005): (0.01-0.03) adding the mixture into an extraction kettle for supercritical extraction to obtain an extraction product; placing the extract in a 3-7 deg.C environment for 80-120min, centrifuging to remove impurities, and vacuumizing in a vacuum box at 25-65 deg.C for 6-10h to obtain Chinese medicinal extract;
the enzyme solution is prepared from cellulase, pectinase and water according to a mass ratio of 1: (0.5-1.5): (3-7) mixing; the supercritical extraction pressure is 30-45Mpa, extraction temperature is 30-50 deg.C, extraction time is 50-180min, and CO is added2The flow rate of the fluid is 10-20 kg/h;
the drying temperature is 35-45 ℃; the microwave power of the microwave treatment is 300-; the stabilizing agent is prepared from catechin and eriodictyol in a mass ratio of 1: (0.3-0.7); the extraction aid is sucrose caprate;
the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 1-10 parts of fleece-flower root, 1-10 parts of angelica, 1-10 parts of ligusticum wallichii, 1-10 parts of ginseng and 1-10 parts of pseudo-ginseng.
2. A Chinese medicinal extract prepared by the supercritical extraction method of the Chinese medicament of claim 1.
3. The use of the herbal extract of claim 2 in a shampoo.
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