CN107970156B - Preparation method of ginsenoside extract for daily chemical products - Google Patents
Preparation method of ginsenoside extract for daily chemical products Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61K8/96—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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61K8/63—Steroids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61K8/67—Vitamins
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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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
- A61K2800/10—General cosmetic use
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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
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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
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
Abstract
The invention discloses a preparation method of a ginsenoside extract for daily chemicals, and relates to the technical field of daily chemical preparation. The invention firstly utilizes alkanol/alkanoic acid, tetrahydrofuran and water to form a supermolecule solvent; then sequentially adopting a superfine grinding technology, a microwave ultrasonic wave auxiliary extraction technology, an ethanol-salt double aqueous phase extraction technology, a supermolecular solvent purification technology and a supercritical CO technology2Extracting and purifying the saponin in the ginseng by an extraction technology; and finally, evaporating the solvent in the extract to dryness to obtain the ginsenoside extract for the daily chemical products. The method is green and environment-friendly, the operation is simple, and the obtained extract ginsenoside has high concentration and also contains active ingredients such as vitamins, amino acids and the like. The ginsenoside extract prepared by the invention can be directly used in daily chemicals such as shampoo, shower gel, face cream, toner and the like.
Description
Technical Field
The invention relates to the technical field of preparation of daily chemicals, in particular to a preparation method of a ginsenoside extract for daily chemicals.
Background
With the improvement of living standard of people, daily chemicals become necessities in life. After the 21 st century, consumers have more natural and safe components of daily chemical products, and the development of natural daily chemical products is more and more paid more attention by people.
Ginseng is dried root of Panax ginseng belonging to Araliaceae, and has effects of invigorating primordial qi, restoring pulse, relieving depletion, invigorating spleen, benefiting lung, promoting fluid production, and tranquilizing mind. Ginsenoside in Ginseng radix is its main active ingredient, and has skin caring and ultraviolet resisting effects. The ginseng extract has strong antibacterial and anti-inflammatory effects, is a natural additive of high-grade cosmetics, and has remarkable curative effects on freckles, chloasma, butterfly spots and senile skin pigmentation of women. Because ginseng contains various ginsenosides, amino acids, vitamins and minerals, the ginseng has the effects of promoting blood circulation of subcutaneous capillaries, increasing nutrition supply of skin, preventing arteriosclerosis, regulating skin moisture balance and the like when added into a skin care product. Therefore, it can delay skin aging, prevent skin from drying and dehydrating, and increase skin elasticity, thereby playing the roles of protecting skin luster and tenderness, and preventing and reducing skin wrinkles, and the ginseng active substance also has the function of inhibiting the reduction of melanin, so that the skin is white and smooth. Researches show that most of the ginsenoside has obvious antioxidant effect, and at the present stage, the ginsenoside has great application prospect as an antioxidant active substance in daily chemicals.
At present, most of preparation methods of the ginseng extract use a large amount of organic solvents, so that the environment is polluted, and the obtained extract cannot be directly used in daily chemicals. Patent CN 105343143 a "a ginsenoside extract and its preparation method" uses ultra-low temperature to freeze-thaw ginseng, then uses methanol to extract ginseng, and then uses saturated petroleum ether and n-butanol to purify the extract in turn to obtain the ginsenoside extract. The method has simple operation and low cost. However, the extract obtained by the method mainly contains protopanoxadiol, the content of saponin of the extract is low, the extract cannot be directly used in the daily chemical industry, a large amount of volatile organic solvent is used during extraction, the health of operators is possibly harmed, and meanwhile, the environmental pollution is easily caused. Therefore, it is important to develop a method for producing a ginseng extract for green and efficient daily use chemicals.
Disclosure of Invention
The preparation method is simple to operate, green, environment-friendly, convenient and fast, has high extraction efficiency, and the obtained extract saponin acid has high purity, does not contain organic solvents, has good skin affinity, and can be directly applied to daily chemicals.
In order to solve the above problems, the present invention provides the following technical solutions: a method for preparing ginsenoside extract for daily chemical products is characterized by comprising the following steps:
(1) mixing n-octyl alcohol, n-hexane, n-decyl alcohol or alkanoic acid which is one of n-caprylic acid, n-hexanoic acid and n-decanoic acid with tetrahydrofuran and water according to the volume percentage of 20-30%, 30-40% and 40-50%, performing vortex centrifugation to obtain a system which is divided into two phases, and taking out the upper phase to obtain the supramolecular solvent;
(2) drying ginseng in a vacuum oven at 60-80 ℃, crushing the ginseng in a traditional Chinese medicine crusher, sieving the crushed ginseng with a 60-mesh sieve, further crushing the crushed ginseng into cell-level ultrafine powder, soaking 6.5kg of the cell-level ultrafine powder in petroleum ether overnight, filtering the soaked ginseng, drying filter residues, mixing the dried filter residues with 30-55L ethanol (40-60 v/v) -aqueous solution, filtering the mixture to obtain clear liquid after 200 plus 400W ultrasonic power, 100 plus 200W microwave power and 35-50 ℃ microwave-ultrasonic treatment for 20-40min, extracting residues with ethanol-water for 2-3 times, merging supernate, and concentrating the supernate under reduced pressure to obtain a ginsenoside crude extract with the density of 1.1-1.2 g/mL;
(3) adding salt solution into the ginsenoside crude extract, performing vortex to form two aqueous phases, taking out the upper phase, performing reduced pressure distillation, concentrating, adding supramolecular solvent, performing vortex for 20s, centrifuging, removing supernatant, taking out solid, and drying to obtain primarily purified ginsenoside extract;
(4) transferring the primarily purified ginsenoside extract to supercritical CO2In the extraction device, the ginsenoside extract is further purified and extracted under the conditions that the pressure is 20-28 MPa, the extraction temperature is 40-60 ℃, ethanol 50-90% (v/v) -water is used as an entrainer and the flow rate of fluid is 25-30L/h, and the solvent in the extract is removed, so that the ginsenoside extract for the natural products used in daily chemicals is obtained.
Further, a large number of reversed-phase micelles exist in the supramolecular solvent in the step (1), and the average particle size of the reversed-phase micelles is 100-200 nm.
Further, the salt solution in the step (3) is one of ammonium sulfate, sodium citrate and dipotassium hydrogen phosphate; the concentration of the salt solution is 0.25-0.5 g/mL; the addition amount of the salt solution is 30-60% of the total volume of the aqueous two phases; the addition amount of the supramolecular solvent is 20-35% of the total volume of the concentrated solution.
Further, the total content of ginsenoside in the ginsenoside extract in the step (4) is not less than 70%, and other components are micromolecular amino acid and vitamin; the ginsenoside extract can be directly used in daily chemicals such as shampoo, shower gel, face cream, toner and the like.
Due to the adoption of the preparation method, compared with the prior art, the invention has the following beneficial effects:
the invention adopts the ultramicro-pulverization technology and the microwave ultrasonic wave auxiliary extraction technology, and utilizes ultrasonic waves to destroy plant fine powder in the ginseng fine powderThe cell wall accelerates the leaching rate of active ingredients, improves the extraction efficiency and shortens the operation time; purifying the crude extract of Ginseng radix by ethanol-salt aqueous two-phase extraction, and removing strong polar compounds from the extract by using two-phase partition coefficient difference; removing nonpolar impurities in the extract by utilizing the strong adsorbability and limiting property of the supramolecular solvent to further purify the extract; by using supercritical CO2Further purifying the ginseng extract by an extraction technology to obtain a high-purity ginsenoside extract; the method is green and environment-friendly, is simple to operate, and the obtained extract ginsenoside has high concentration and also contains active ingredients such as vitamins and amino acids. The ginsenoside extract prepared by the invention can be directly used in daily chemicals such as shampoo, shower gel, face cream, toner and the like.
Detailed Description
The invention will be further described in detail with reference to the following specific examples:
the first embodiment is as follows:
mixing n-octanol, tetrahydrofuran and water according to a ratio of 15: 35: mixing the materials according to the volume ratio of 50, performing vortex centrifugation, separating the system into two phases, and taking out the upper phase to obtain the n-octanol-tetrahydrofuran-water supramolecular solvent; drying ginseng in a vacuum drying oven at 60 ℃, crushing the ginseng by a traditional Chinese medicine crusher, sieving the crushed ginseng by a sieve of 60 meshes, further crushing the ginseng into cell-level ultrafine powder, soaking 6.5kg of the ginseng cell-level ultrafine powder in 70L of petroleum ether overnight, filtering the soaked ginseng cell-level ultrafine powder, drying filter residues, mixing the dried filter residues with 40L of 65% ethanol-water solution system, filtering the mixture after 30min of microwave-ultrasonic treatment under the conditions of 400W of ultrasonic power, 150W of microwave power and 40 ℃ to obtain clear liquid, extracting the residues for 3 times by using ethanol-water, merging the clear liquid, and concentrating the clear liquid under reduced pressure until the density is 1.1-1.2g/mL to obtain a ginsenoside crude extract; adding 0.35g/mL sodium sulfate solution accounting for 20% of the total volume of the aqueous phase into the ginsenoside crude extract, performing vortex forming to obtain an aqueous phase, taking out the upper phase, performing reduced pressure distillation and concentration, adding n-octanol-tetrahydrofuran-water supramolecular solvent accounting for 20% of the total volume of the concentrated solution, performing vortex 20s, performing centrifugation, removing the supernatant, taking out the solid part, and drying to obtain a primarily purified ginsenoside extract; transferring the primarily purified ginsenoside extract into a supercritical CO2 extraction device, further purifying and extracting the ginsenoside extract under the conditions of pressure of 25MPa, extraction temperature of 55 ℃, 80% ethanol-water as an entrainer and fluid flow of 26L/h, and removing the solvent in the extract to obtain the ginsenoside extract for the chemical products for daily use, wherein the purity of the ginsenoside is 78%.
Example two:
mixing n-decanoic acid, tetrahydrofuran and water according to the weight ratio of 20: 30: mixing the materials according to a volume ratio of 50, performing vortex centrifugation, separating the system into two phases, and taking out the upper phase to obtain the n-octanol-tetrahydrofuran-water supramolecular solvent; drying ginseng in a vacuum drying oven at 60 ℃, crushing the ginseng by a traditional Chinese medicine crusher, sieving the crushed ginseng by a sieve of 60 meshes, further crushing the ginseng into cell-level ultrafine powder, soaking 6.5kg of the ginseng cell-level ultrafine powder in 500mL of petroleum ether overnight, filtering the soaked ginseng cell-level ultrafine powder, drying filter residues, mixing the dried filter residues with 45L of 70% ethanol-water solution system, filtering the mixture after 30min of microwave-ultrasonic treatment under the conditions of 500W of ultrasonic power, 200W of microwave power and 35 ℃, extracting residues for 2 times by using ethanol-water, merging supernate, and concentrating the supernate under reduced pressure until the density is 1.1-1.2g/mL to obtain a ginsenoside crude extract; adding 0.3g/mL sodium citrate solution which is 20% of the total volume of the aqueous two phases into the ginsenoside crude extract, then carrying out vortex to form the aqueous two phases, removing the supernatant, taking out the upper phase, carrying out reduced pressure distillation and concentration, adding n-decanoic acid-tetrahydrofuran-water supramolecular solvent which is 25% of the total volume of the concentrated solution, carrying out vortex for 20s, carrying out centrifugation, taking out the solid part, and drying to obtain a primarily purified ginsenoside extract; transferring the primarily purified ginsenoside extract to supercritical CO2Further purifying and extracting the ginsenoside extract in an extraction device under the conditions of pressure of 26MPa, extraction temperature of 50 ℃, 80% ethanol-water as an entrainer and fluid flow of 25L/h, and removing a solvent in the extract to obtain the ginsenoside extract for daily chemicals with the purity of the total ginsenoside of 76%.
Example three:
n-hexanol, tetrahydrofuran and water are mixed according to the weight ratio of 15: 35: mixing the materials according to the volume ratio of 50, performing vortex centrifugation, separating the system into two phases, and taking out the upper phase to obtain n-hexanol-tetrahydrofuran-water supramolecular solvent; drying Ginseng radix in a vacuum drying oven at 60 deg.C, pulverizing with a Chinese medicinal pulverizer, sieving with a 60 mesh sieve, and further pulverizing into powderSoaking 6.5kg of ginseng cell-level ultrafine powder in 450mL of petroleum ether overnight, filtering, drying the filter residue, mixing with 60L of 60% ethanol-water solution system, performing microwave-ultrasonic treatment at 400W of ultrasonic power and 200W of microwave power and 30 ℃ for 25min, filtering to obtain clear solution, extracting the residue with ethanol-water for 3 times, mixing the clear solution, and concentrating the clear solution under reduced pressure to obtain ginsenoside crude extract with density of 1.1-1.2 g/mL; adding 0.25g/mL dipotassium hydrogen phosphate solution accounting for 30% of the total volume of the aqueous two phases into the ginsenoside crude extract, performing vortex forming to obtain the aqueous two phases, taking out the upper phase, performing reduced pressure evaporation and concentration, adding n-hexanol-tetrahydrofuran-water supramolecular solvent accounting for 25% of the total volume of the concentrated solution, performing vortex 20s, performing centrifugation, removing the supernatant, taking out the solid part, and drying to obtain a primarily purified ginsenoside extract; transferring the primarily purified ginsenoside extract to supercritical CO2Further purifying and extracting the ginsenoside extract in an extraction device under the conditions of 26MPa of pressure, 50 ℃ of extraction temperature, 80% ethanol-water as an entrainer and 26.2L/h of fluid flow, and removing a solvent in the extract to obtain the ginsenoside extract for the daily chemicals with the purity of total ginsenoside of 79%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A method for preparing ginsenoside extract for daily chemical products is characterized by comprising the following steps:
(1) mixing n-octyl alcohol, n-hexane, n-decyl alcohol or alkanoic acid which is one of n-caprylic acid, n-hexanoic acid and n-decanoic acid with tetrahydrofuran and water according to the volume percentage of 20-30%, 30-40% and 40-50%, performing vortex centrifugation to obtain a system which is divided into two phases, and taking out the upper phase to obtain the supramolecular solvent;
(2) drying ginseng in a vacuum oven at 60-80 ℃, crushing the ginseng in a traditional Chinese medicine crusher, sieving the crushed ginseng with a 60-mesh sieve, further crushing the crushed ginseng into cell-level ultrafine powder, soaking 6.5kg of the cell-level ultrafine powder in 65-100L petroleum ether overnight, filtering, drying filter residues, mixing the dried filter residues with 30-55L ethanol-water solution, filtering to obtain clear liquid after 200-400W ultrasonic power, 100-200W microwave power and 35-50 ℃ microwave-ultrasonic power for 20-40min, extracting residues with ethanol-water for 2-3 times, combining the clear liquid, and concentrating the clear liquid under reduced pressure to obtain a ginsenoside crude extract with the density of 1.1-1.2 g/mL; the ethanol in the ethanol-water solution accounts for 40-80%;
(3) adding salt solution into the ginsenoside crude extract, performing vortex to form two aqueous phases, taking out the upper phase, performing reduced pressure distillation, concentrating, adding supramolecular solvent, performing vortex for 20s, centrifuging, removing supernatant, taking out solid, and drying to obtain primarily purified ginsenoside extract; the salt solution is one of ammonium sulfate, sodium citrate and dipotassium hydrogen phosphate; the concentration of the salt solution is 0.25-0.5 g/mL; the addition amount of the salt solution is 30-60% of the total volume of the aqueous two phases; the addition amount of the supramolecular solvent is 20-35% of the total volume of the concentrated solution;
(4) transferring the primarily purified ginsenoside extract into a supercritical CO2 extraction device, further purifying and extracting the ginsenoside extract under the conditions that the pressure is 20-28 MPa, the extraction temperature is 40-60 ℃, 50-90% (v/v) ethanol-water is taken as an entrainer and the flow of fluid is 25-30L/h, and removing the solvent in the extract to obtain the ginsenoside extract used as a natural product for daily chemicals.
2. The method for preparing ginsenoside extract used in daily chemicals as claimed in claim 1, wherein a large number of reverse micelles exist in the supramolecular solvent in the step (1), and the average particle size of the reverse micelles is 100-200 nm.
3. The method for preparing a ginsenoside extract used in daily chemicals according to claim 1, wherein the ginsenoside extract in the step (4) contains ginsenoside not less than 70% and other components including small molecular amino acids and vitamins; the ginsenoside extract can be directly used in shampoo, shower gel, face cream and skin toner daily chemical products.
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| CN108902678A (en) * | 2018-06-06 | 2018-11-30 | 广东皇麦世家食品有限公司 | A kind of preparation method of the weight-reducing oatmeal containing algal polysaccharides |
| CN114588188A (en) * | 2022-03-16 | 2022-06-07 | 浙江长典药物技术开发有限公司 | Method for extracting ginsenoside and extract obtained by method |
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| US20130178436A1 (en) * | 2012-01-10 | 2013-07-11 | Korea Institute Of Science And Technology | Composition for preventing, improving, or treating renal disease including maillard browning reaction products of panax species plant extract |
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