CN111803411B

CN111803411B - Skin care product containing schisandra chinensis extract and preparation method thereof

Info

Publication number: CN111803411B
Application number: CN202010499851.0A
Authority: CN
Inventors: 周有财
Original assignee: Heilongjiang Aolida Naide Pharmaceutical Co ltd
Current assignee: Heilongjiang Aolida Naide Pharmaceutical Co ltd
Priority date: 2020-06-04
Filing date: 2020-06-04
Publication date: 2023-06-23
Anticipated expiration: 2040-06-04
Also published as: CN111803411A

Abstract

The invention provides a skin care product containing shizandra extract, which comprises the following components: 26-30 parts of jojoba oil; 26-30 parts of schisandra chinensis extract; 5-10 parts of lanolin; the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%. Compared with the prior art, the invention takes jojoba oil, schisandra chinensis extract and lanolin as core active substances, can quickly permeate into the deep layer of skin to fundamentally inhibit and remove various free radicals harmful to skin health, repair DNA damage of skin cells, recover cell activity, promote skin metabolism, effectively repair and whiten skin, delay skin aging, and enable the skin to be immediately compact, moist, flat and smooth; can also keep the skin moist for a long time, increase the skin elasticity, lighten the skin color, keep the skin tender, smooth, compact and elastic, and can show the attractive and bright white and bright air color in a shorter time.

Description

Skin care product containing schisandra chinensis extract and preparation method thereof

Technical Field

The invention belongs to the technical field of skin care products, and particularly relates to a skin care product containing shizandra berry extract and a preparation method thereof.

Background

Fructus Schisandrae chinensis is dried mature fruit of Schisandra chinensis Schisandra chinensis of Magnoliaceae, and has effects of astringing, invigorating qi, promoting salivation, invigorating kidney, and calming heart. The lignanoid compound with the biphenyl cyclooctadiene structure in the schisandra is a main bioactive component and mainly comprises schisandra fruit B, schisandra fruit A, schisandra fruit alcohol A and the like, wherein the content of the schisandra fruit B is generally between 0.1 and 0.4 percent.

According to the records of books, the schisandra chinensis has the effects of regulating skin, maintaining beauty, keeping young, prolonging life and the like. Fructus Schisandrae chinensis in Shennong Ben Cao Jing as the upper product; the shizandra berry is called as 'pleasant to human body', has rich nutrition and has the function of ruddy complexion and fair skin; plum fashion: wu Wei Zi is good at nourishing and is good at north. Scientific experiments prove that: the lignans contained in the schisandra chinensis can enhance the energy production of adenine nucleoside triphosphate (ATP) or granuliform (cell energy bank), protect granuliform from oxidative stress, slow down the skin aging process and keep the general supplementary antioxidant products of youth vigor, and the energy against free radicals is very limited. Some antioxidant substances can only remove one free radical at a time from each antioxidant, and the obtained antioxidant substances can only remove one free radical. The schisandrin B can completely remove free radicals generated by aerobic metabolism, effectively remove free radicals generated by anaerobic metabolism, and can directly promote the human body to activate antioxidant substances by oneself while removing free radicals and inhibiting the formation of peroxidized lipid, thereby improving the antioxidant capacity of the human body, and the antioxidant effect is more comprehensive, lasting and more effective. Therefore, the schisandra chinensis extract can be widely applied to various component preparations, health-care foods, medicines and skin care products.

In recent years, research shows that the schisandrin B not only has various biological activities of resisting tumor, protecting liver, resisting ulcer, resisting virus and the like, but also has better effect of scavenging free radicals. The schisandrin B is added into cosmetics and has the functions of resisting oxidation, resisting aging, beautifying and protecting health. However, in the prior art, the skin care products added with the schisandra chinensis extract are fewer and the comprehensive utilization rate of schisandra chinensis is not high, so that the schisandra chinensis is still to be further developed.

Disclosure of Invention

In view of the above, the technical problem to be solved by the invention is to provide a skin care product containing schisandra chinensis extract with the functions of antioxidation, anti-aging, beauty, health care and restoration and a preparation method thereof.

The invention provides a skin care product containing shizandra extract, which comprises the following components:

26-30 parts of jojoba oil;

26-30 parts of schisandra chinensis extract;

5-10 parts of lanolin;

the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%.

Preferably, the method further comprises:

preferably, the emulsifier is selected from cetyl stearyl alcohol and/or squalane; the essence is selected from one or more of propyl heptyl octoate, p-tert-butyl cyclohexyl acetate and ethyl salicylate; the emulsion type matrix is selected from polydimethylsiloxane.

Preferably, the method comprises the steps of:

preferably, the schisandra chinensis extract is prepared according to the following method:

s1) crushing the schisandra chinensis to obtain schisandra chinensis powder;

s2) performing supercritical carbon dioxide extraction on the schisandra chinensis powder to obtain a supercritical extract;

s3) dissolving the supercritical extract with an organic solvent, eluting and separating through silica gel column chromatography, and concentrating to obtain concentrated fraction of the schisandra chinensis extract;

s4) dissolving the concentrated fraction of the schisandra chinensis extract in a mixed solvent of hexane and isopropanol, and performing low-temperature crystallization to obtain a crude schisandra chinensis extract product;

s5) purifying the crude schisandra chinensis product by hexane to obtain the schisandra chinensis extract.

Preferably, the mesh number of the schisandra chinensis powder is 30-50 mesh; the extraction pressure of the supercritical carbon dioxide extraction is 20-30 MPa; the extraction temperature is 30-50 ℃; the extraction time is 1.5-2.5 h.

Preferably, the step S3) specifically includes:

a) Dissolving the supercritical extract with an organic solvent, performing silica gel column chromatography, eluting with a first eluent, separating, and concentrating to obtain lignan concentrated fraction; the organic solvent is petroleum ether; the first eluent is petroleum ether; the flow rate of the first eluent in the step A) is 3-7 ml/min;

B) Dissolving the lignan concentrated fraction with a second organic solvent, performing silica gel column chromatography, eluting with a second eluent, separating, and concentrating to obtain concentrated fraction of fructus Schisandrae extract; the second organic solvent is a mixed solvent of petroleum ether and acetone; the volume ratio of petroleum ether to acetone in the second organic solvent is (90-97): (10-3); the second eluent is a mixed solvent of petroleum ether and acetone; the volume ratio of petroleum ether to acetone in the second eluent is (90-97): (10-3);

the flow rate of the second eluent in the step B) is 3-7 ml/min.

Preferably, in the step S4), the volume ratio of hexane to isopropanol is 1: (1.5-2.5); the temperature of low-temperature crystallization is-10 ℃ to-30 ℃;

the mass volume ratio of the schisandrin B concentrated fraction to the mixed solvent in the step S4) is 1g: (1-3) ml.

The invention also provides a preparation method of the skin care product containing the schisandra chinensis extract, which comprises the following steps:

s1) mixing 26-30 parts by weight of schisandra chinensis extract, 5-10 parts by weight of lanolin, 2-5 parts by weight of vitamin A, 2-5 parts by weight of vitamin C, 0.5-2 parts by weight of emulsifier, 2-6 parts by weight of essence, 1-5 parts by weight of emulsion matrix and 10000-20000 parts by weight of water, and performing ultrasonic high-speed dispersion to obtain a mixture;

S2) mixing 26-30 parts by weight of jojoba oil with the mixture, and performing ultrasonic high-speed dispersion to obtain a skin care product;

Preferably, the ultrasonic frequency of the ultrasonic high-speed dispersion in the step S1) is 20-40 KHz; the speed of ultrasonic high-speed dispersion is 5000-5400 r/min; the time is 30-60 min;

the ultrasonic frequency of the ultrasonic high-speed dispersion in the step S2) is 20-35 KHz; the speed of ultrasonic high-speed dispersion is 4800-5200 r/min.

The invention provides a skin care product containing shizandra extract, which comprises the following components: 26-30 parts of jojoba oil; 26-30 parts of schisandra chinensis extract; 5-10 parts of lanolin; the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%. Compared with the prior art, the invention takes jojoba oil, schisandra chinensis extract and lanolin as core active substances, can quickly permeate into the deep layer of skin to fundamentally inhibit and remove various free radicals harmful to skin health, repair DNA damage of skin cells, recover cell activity, promote skin metabolism, effectively repair and whiten skin, delay skin aging, and enable the skin to be immediately compact, moist, flat and smooth; the skin can be kept moist for a long time, the skin elasticity is increased, the skin color is improved, the skin is kept tender, smooth, compact and elastic, the skin is enabled to reappear the youth luster, the skin can show the attractive and bright white and bright air color in a shorter time, and enough protection is provided for the tender skin.

Detailed Description

The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

26-30 parts of jojoba oil;

26-30 parts of schisandra chinensis extract;

5-10 parts of lanolin;

The sources of all the raw materials are not particularly limited, and the raw materials can be sold in the market or self-made.

The skin care product provided by the invention takes jojoba oil, schisandra chinensis extract and lanolin as main active components, wherein jojoba oil is an emollient and a solvent; in some embodiments provided herein, the jojoba oil is preferably present in an amount of 26 parts by weight; in some embodiments provided herein, the jojoba oil is preferably present in an amount of 28 parts by weight; in other embodiments provided by the present invention, the jojoba oil is preferably present in an amount of 30 parts by weight.

In some embodiments provided herein, the schisandra chinensis extract is preferably present in an amount of 26 parts by weight; in some embodiments provided herein, the schisandra chinensis extract is preferably present in an amount of 28 parts by weight; in other embodiments provided by the present invention, the schisandra chinensis extract is preferably contained in an amount of 30 parts by weight; the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%.

In the present invention, the schisandra chinensis extract is preferably prepared according to the following method: comprising the following steps: s1) crushing the schisandra chinensis to obtain schisandra chinensis powder; s2) performing supercritical carbon dioxide extraction on the schisandra chinensis powder to obtain a supercritical extract; s3) dissolving the supercritical extract with an organic solvent, eluting and separating through silica gel column chromatography, and concentrating to obtain concentrated fraction of the schisandra chinensis extract; s4) dissolving the concentrated fraction of the schisandra chinensis extract in a mixed solvent of hexane and isopropanol, and performing low-temperature crystallization to obtain a crude schisandra chinensis extract product; s5) purifying the crude schisandra chinensis extract by hexane to obtain the schisandra chinensis extract.

According to the invention, the schisandra chinensis is preferably subjected to airing and drying treatment; the drying is preferably carried out outdoors; the time for the drying is preferably 1 to 3 days, more preferably 2 days.

The dried schisandra chinensis is preferably crushed after removing impurities; the crushing is preferably performed by using a crusher; after crushing, screening by a screen to obtain the schisandra chinensis powder; in order to reduce the scattering distance between the fluid and the solute in the natural parent body, the natural raw materials should be subjected to crushing pretreatment. The pretreatment of raw materials requires uniform crushing, and excessive coarse or excessive fine particles can influence the mass transfer effect, and the larger the particle size is, the smaller the material particles are. In the present invention, the mesh number of the schisandra chinensis powder is preferably 30 to 50 mesh, more preferably 40 mesh.

Extracting the schisandra chinensis powder by supercritical carbon dioxide to obtain a supercritical extract; extraction pressure is an important operating parameter in supercritical extraction processes. The pressure of the supercritical fluid is the main factor affecting the solubility of the extract in the fluid, and it directly affectsTo extract efficiency, it is therefore necessary to find the most suitable pressure for extraction of a particular product. Supercritical fluids have a similar viscosity to gases, a similar density and dissolution capacity to liquids. The diffusion coefficient of a solute in a solvent is generally proportional to the density of the solvent and inversely proportional to the viscosity of the solvent. As the pressure increases, the fluid density increases, the dissolution capacity increases, and after a certain pressure is reached, the solvent density reaches a certain value, the influence of the pressure on the density becomes less obvious, and the increase of the extraction rate becomes gentle. And meanwhile, after the pressure reaches a certain level, the pressure resistance and the sealing performance of the equipment are very strict, so that the cost of extraction is obviously increased under the condition of small variation of the product yield. Therefore, generally in the SFE process, when the extraction pressure meets a certain extraction rate, the extraction rate is not increased by increasing the pressure. The pressure of the supercritical carbon dioxide extraction in the invention is preferably 20-30 MPa; temperature is another very important and active parameter of the supercritical extraction process. On one hand, the thermal motion of the solute is accelerated due to the temperature rise, the vapor pressure is increased, and the supercritical CO2 extraction is a mass transfer process like other extraction processes, so that the increase of the vapor pressure of the solute inevitably leads to the increase of the extraction rate; on the other hand, due to the rise in temperature, the solvent CO ₂ The density of (c) becomes smaller and the size of the density determines the dissolving capacity of the solute, so that the temperature is increased and the dissolving capacity is reduced. Therefore, the temperature rise may cause an increase, a constant or a decrease in the extract yield; it is determined by the reduction of CO by heating ₂ The density and the increased diffusion coefficient are competing effects. In the present invention, the extraction temperature is preferably 30 to 50 ℃; the extraction time is preferably 1.5 to 2.5 hours. The obtained supercritical extract is preferably preserved in dark at low temperature, more preferably in brown bottle with bottle stopper; the low temperature is preferably 2 to 10 ℃.

The supercritical extraction has the remarkable advantages of high efficiency and high yield, can selectively separate various substances, and can effectively reduce impurities and control the content. In addition, the method has the obvious advantages of quick extraction time, short production period, convenient operation, low power consumption and high efficiency, and is very suitable for industrialized large-scale preparation of traditional Chinese medicinal materials.

Dissolving the supercritical extract with an organic solvent, and eluting and separating through a silica gel column chromatography; in order to increase the purity of the elution, specific preference is given to: a) Dissolving the supercritical extract with an organic solvent, performing silica gel column chromatography, eluting with a first eluent, separating, and concentrating to obtain lignan concentrated fraction; b) Dissolving the lignan concentrated fraction with a second organic solvent, performing silica gel column chromatography, eluting with a second eluent, separating, and concentrating to obtain concentrated fraction of fructus Schisandrae extract; the mass volume ratio of the supercritical extract to the organic solvent is preferably 1g: (1-3) ml, more preferably 1g: (1.5-2.5) ml, and more preferably 1g:2ml; the organic solvent is preferably petroleum ether; the mass ratio of the supercritical extract to the silica gel column is preferably 1: (1 to 3), more preferably 1: (1.5 to 2.5), and more preferably 1:2; the first eluent is preferably petroleum ether; the flow rate of the first eluent is preferably 3-7 ml/min; in the present invention, when the first eluent is used for elution, the effluent is preferably monitored by TLC, and before the schisandrin B is eluted, the effluent is preferably collected and concentrated, so that a fatty oil concentrated fraction can be obtained; concentrating the eluent containing schisandrin B to obtain lignan concentrated fraction; dissolving the lignan concentrated fraction with a second organic solvent; the mass volume ratio of the lignan concentrated fraction to the second organic solvent is preferably 1g: (0.5 to 1.5) ml, more preferably 1g:1ml; the second organic solvent is preferably a mixed solvent of petroleum ether and acetone; the volume ratio of petroleum ether to acetone in the second organic solvent is preferably (90-97): (10 to 3), more preferably (90 to 95): (10 to 5), more preferably (92 to 95): (8-5), most preferably 95:5, a step of; dissolving, performing silica gel column chromatography, and eluting with a second eluent; the mass ratio of the lignan concentrated fraction to the silica gel column is preferably 1: (5 to 15), more preferably 1: (8-12), and more preferably 1:10; the second eluent is preferably a mixed solvent of petroleum ether and acetone; the volume ratio of petroleum ether to acetone in the second eluent is preferably (90-97): (10 to 3), more preferably (90 to 95): (10 to 5), more preferably (92 to 95): (8-5), most preferably 95:5, a step of; the dosage of the second eluent is preferably 6-10 times of the volume of the silica gel column; the flow rate of the second eluent is preferably 3-7 ml/min; in the present invention, the effluent is preferably monitored by TLC, which indicates that single point schisandrin b has been collected and elution is complete; concentrating the eluent to obtain concentrated fraction of fructus Schisandrae extract.

The silica gel column chromatography has good adsorption function and separation function, is convenient to control time and has strong compression resistance. The column chromatography silica gel has good thermal stability and chemical stability, and can selectively adsorb and purify isomer components from multicomponent solution.

Dissolving the concentrated fraction of the schisandra chinensis extract in a mixed solvent of hexane and isopropanol, and performing low-temperature crystallization to obtain a crude schisandra chinensis extract; wherein, the volume ratio of hexane to isopropanol is preferably 1: (1.5 to 2.5), more preferably 1: (1.8 to 2.2), and more preferably 1:2; the mass volume ratio of the concentrated fraction of the schisandra chinensis extract to the mixed solvent is preferably 1g: (1-3) ml, more preferably 1g: (1.5-2.5) ml, and more preferably 1g:2ml; the temperature of the low-temperature crystallization is preferably-10 ℃ to-30 ℃, more preferably-15 ℃ to-25 ℃, and still more preferably-20 ℃; the time of the low-temperature crystallization is preferably 8-15 h, and more preferably 10-12 h; after crystallization at low temperature, preferably vacuum filtering to obtain crude schisandra extract; more preferably, the crude schisandra extract is obtained after filtration and washing by cold hexane.

Purifying the crude schisandra chinensis extract by hexane; the purification method is preferably rinsing; more preferably, hexane elution and purification at 0-8 ℃, still more preferably hexane elution and purification at 0-5 ℃, still more preferably hexane elution and purification at 2-4 ℃, and most preferably hexane elution and purification at 3 ℃ are adopted to obtain the schisandra chinensis extract.

According to the invention, preferably, schisandrin B is used as a reference substance, and HPLC analysis is adopted to detect the content of schisandrin B in the schisandra extract; the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is preferably 25-95 wt%; the HPLC column is preferably a Nova-PakC184 μm (3.9 mm. Times.300 mm) column; the mobile phase is preferably a mixed solution of acetonitrile and water; the volume ratio of acetonitrile to water is preferably (50-60): (50 to 40), more preferably (53 to 57): (47 to 47), and more preferably 55:45; the fluidity of the mobile phase is preferably 0.5 to 2ml/min, more preferably 0.5 to 1.5ml/min, still more preferably 1ml/min; elution is preferably monitored during HPLC by absorbance at 254 nm.

The schisandrin B extract is obtained by sequentially carrying out supercritical carbon dioxide extraction technology, silica gel column chromatography and hexane purification, the preparation process is simple, the operation condition is mild, the active ingredient retention effect is good, the schisandrin B extract is suitable for extracting natural products, and is especially suitable for extracting low-molecular, low-polarity, lipophilic and low-boiling-point schisandrin B, the schisandrin B extract is suitable for industrial production, and the schisandrin B content in the prepared schisandrin B extract is high.

The skin care product provided by the invention is added with lanolin as an emollient; in some embodiments provided herein, the lanolin content is preferably 5 parts by weight; in other embodiments provided by the present invention, the lanolin content is preferably 10 parts by weight.

According to the present invention, the skin care product preferably further comprises 2 to 5 parts by weight of vitamin A, more preferably 2 to 4 parts by weight of vitamin A; in some embodiments provided herein, the vitamin a is preferably present in an amount of 2 parts by weight; in some embodiments provided herein, the vitamin a is preferably present in an amount of 4 parts by weight; in other embodiments provided by the present invention, the vitamin A content is preferably 3 parts by weight.

The skin care product provided by the invention is preferably added with 0.5 to 2 parts by weight of emulsifying agent, more preferably 1 to 2 parts by weight and even more preferably 2 parts by weight; the emulsifier is preferably a nonionic emulsifier, more preferably cetostearyl alcohol and/or squalane; the squalane is preferably natural squalane.

The skin care product provided by the invention preferably further comprises 2-6 parts by weight of essence, more preferably 3-6 parts by weight, still more preferably 4-6 parts by weight and most preferably 5 parts by weight; the essence is preferably one or more of propyl heptyl octoate, p-tert-butyl cyclohexyl acetate and ethyl salicylate; the essence is insoluble in water, is easily dissolved in partial organic solvent, is safe and harmless to human body, and can be used as essence to be added into various skin care products, so that the skin care products have pleasant fragrance.

According to the present invention, it is preferable to further comprise 1 to 5 parts by weight of an emulsion-type base which functions by mixing with a surfactant such as lanolin as an emulsion-type base; more preferably 2 to 5 parts by weight, still more preferably 3 to 4 parts by weight, most preferably 4 parts by weight; the emulsion-type matrix is preferably polydimethylsiloxane.

According to the invention, water is preferably also included in an amount of 10000 to 20000 parts by weight; in some embodiments provided herein, the water is preferably present in an amount of 10000 parts by weight; in some embodiments provided herein, the water content is preferably 15000 parts by weight; in other embodiments provided by the present invention, the water content is preferably 20000 parts by weight; the water is preferably deionized water.

In the present invention, the skin care product is preferably a cream.

According to the present invention, the skin care product most preferably comprises:

the invention takes jojoba oil, schisandra chinensis extract and lanolin as core active substances, can quickly permeate into the deep layer of skin to fundamentally inhibit and remove various free radicals harmful to skin health, repair DNA damage of skin cells, restore cell activity, promote skin metabolism, effectively repair and whiten skin, delay skin aging, and enable the skin to be immediately compact, moist, flat and smooth; the skin can be kept moist for a long time, the skin elasticity is increased, the skin color is improved, the skin is kept tender, smooth, compact and elastic, the skin is enabled to reappear the youth luster, the skin can show the attractive and bright white and bright air color in a shorter time, and enough protection is provided for the tender skin.

The invention also provides a preparation method of the skin care product containing the schisandra chinensis extract, which comprises the following steps: s1) mixing 26-30 parts by weight of schisandra chinensis extract, 5-10 parts by weight of lanolin, 2-5 parts by weight of vitamin A, 2-5 parts by weight of vitamin C, 0.5-2 parts by weight of emulsifier, 2-6 parts by weight of emulsifier, 1-5 parts by weight of emulsion matrix and 10000-20000 parts by weight of water, and performing ultrasonic high-speed dispersion to obtain a mixture; s2) mixing 26-30 parts by weight of jojoba oil with the mixture, and performing ultrasonic high-speed dispersion to obtain a skin care product; the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%.

The schisandra extract, lanolin, vitamin A, vitamin C, emulsifying agent, essence, emulsion matrix, water and jojoba oil are all described above, and are not described here again.

Mixing 26-30 parts by weight of schisandra chinensis extract, 5-10 parts by weight of lanolin, 2-5 parts by weight of vitamin A, 2-5 parts by weight of vitamin C, 0.5-2 parts by weight of emulsifying agent, 2-6 parts by weight of essence, 1-5 parts by weight of emulsion matrix and 10000-20000 parts by weight of water, and performing ultrasonic high-speed dispersion to obtain a mixture; the ultrasonic frequency of the ultrasonic high-speed dispersion is preferably 20-40 KHz; the speed of ultrasonic high-speed dispersion is preferably 5000-5400 r/min, more preferably 5100-5200 r/min, and even more preferably 5200r/min; the time is preferably 30 to 60 minutes, more preferably 40 to 50 minutes, still more preferably 45 minutes.

Mixing 26-30 parts by weight of jojoba oil with the mixture, and performing ultrasonic high-speed dispersion to obtain a skin care product; the ultrasonic frequency of the ultrasonic high-speed dispersion is preferably 20-35 KHz, more preferably 30KHz; the speed of ultrasonic high-speed dispersion is preferably 4800 to 5200r/min, more preferably 4900 to 5200r/min, still more preferably 5000r/min.

Pure natural golden jojoba oil, schisandra chinensis extract, lanolin and the like are adopted as raw materials, so that no toxic or side effect is caused; meanwhile, the invention adopts the original preparation process of the schisandra chinensis extract to realize rapid and strong collision of materials, so that plant cells are instantaneously broken, low-temperature and rapid full-component extraction is realized, and thus, the thermosensitive components are effectively prevented from being oxidized and degraded. The special process is adopted to further improve the yield of the schisandra chinensis extract, mainly schisandra chinensis B extract, and reduce the cost of the skin care product. The skin care product prepared by the invention has light texture, is not greasy, relieves dry skin, can keep the skin moist for a long time, increases skin elasticity, resists wrinkles, lightens skin color, effectively resists aging, and makes the skin beautiful and refreshing.

In order to further illustrate the present invention, the following examples are provided to describe in detail a skin care product containing shizandra berry extract and a preparation method thereof.

The reagents used in the examples below are all commercially available.

Example 1: selection of extraction pressure

1.1 weighing 5 parts of schisandra chinensis powder with the same mass, wherein 200g of each part of schisandra chinensis powder is sieved by a 40-mesh sieve, the extraction temperature is set to be 40 ℃, and the extraction pressures are respectively 15MPa, 20MPa, 25MPa, 30MPa and 35MPa, and the extraction time is 2 hours.

Along with the gradual increase of the extraction pressure, the content of the schizandrin B is also gradually increased. This is because supercritical CO increases with pressure ₂ As the density of the polymer increases, the dissolution capacity increases. When the extraction pressure is increased from 15MPa to 30MPa, the content of schizandrin B is obviously increased. When the pressure reaches 35MPa, the content of schizandrin B is increased, but the increase amplitude is small. Therefore, the two are not linearly related, which may be related to supercritical CO ₂ Is related to the compressibility of the composition. Supercritical CO at low pressure ₂ High compressibility, supercritical CO ₂ The compressibility is small. In addition, when the extraction pressure is relatively high, the color of the extract is deepened, which may be caused by an increase in the pigment content of the extract.

In view of practical applicability of production, the extraction pressure should be selected to be in the range of 20 to 30 MPa.

1.2 100g of Schisandra chinensis extract was dissolved in 200mL of petroleum ether and the extract was applied in a preliminary silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether eluting silica gel column at about 3-7 mL/split. Before eluting schizandrin b, the effluent was pooled and concentrated using a rotary evaporator under reduced pressure to obtain a fatty oil concentrate fraction. Collecting eluate containing schizandrin B into pool, and concentrating to obtain lignan concentrated fraction. And (3) immediately after the elution of the schizandrin B is finished, replacing the eluting solution with acetone.

1.3A lignan concentrate fraction 20g was dissolved in 20mL of petroleum ether/acetone (95:5, v/v (volume ratio)) and the fraction was applied in a preparative silica gel column (20 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether acetone (95:5, v/v (volume ratio)) eluting the silica gel column at about 3-7 mL/split. The permeate fraction showed that single point schizandrin b had been pooled and concentrated to obtain a concentrated fraction of schizandrin extract.

1.4 dissolving the concentrated fraction of Schisandra chinensis extract in hexane to isopropanol (volume ratio 1:2), keeping at-20℃overnight. The crude schisandra extract is then separated from the mother liquor by vacuum filtration and then washed with cold hexane.

1.5 purifying, grinding the crude schisandra extract into powder, leaching with cold n-hexane at 3 ℃, and filtering, and repeating leaching steps until the powder becomes pure white to obtain the schisandra extract.

Example 2: selection of extraction temperature

2.1 weighing 5 parts of schisandra chinensis powder with the same mass, wherein each part of schisandra chinensis powder is 200g, and sieving the schisandra chinensis powder by a 40-sieve. The extraction pressure is controlled at 25MPa, the extraction temperature is respectively 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃ and the extraction time is 2h.

When the extraction temperature is lower than 40 ℃, the content of schizandrin increases with the increase of the temperature. After the temperature reaches above 40 ℃, the content of schizandrin is reduced along with the rise of the temperature, because the vapor pressure and the diffusion coefficient of the components to be separated are greatly improved when the temperature is raised, the molecular movement is aggravated, the association opportunity of solutes and solvents is increased, and the dissolving capacity is improved. However, after the temperature rises above 40 ℃, CO ₂ The density is reduced sharply, the volatility and diffusion coefficient of the separated components are increased sufficiently to compensate the dissolution caused by the density changeDecline in ability, overall result is decline in schisandrin b content.

The effects of the above factors are comprehensively considered, and the influence of energy consumption is considered, so that the extraction temperature is finally selected to be 30-50 ℃.

2.2 dissolving 100g of Schisandra chinensis extract in 200mL of petroleum ether and applying the extract in a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether eluting silica gel column at about 3-7 mL/split. Before eluting schizandrin b, the effluent was pooled and concentrated using a rotary evaporator under reduced pressure to obtain a fatty oil concentrate fraction. Collecting eluate containing schizandrin B into pool, and concentrating to obtain lignan concentrated fraction. And (3) immediately after the elution of the schizandrin B is finished, replacing the eluting solution with acetone.

2.3A lignan concentrated fraction 20g was dissolved in 20mL of petroleum ether/acetone (95:5, v/v (volume ratio)) and applied in a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether acetone (95:5, v/v (volume ratio)) eluting the silica gel column at about 3-7 mL/split. The permeate fraction showed that single point schizandrin b had been pooled and concentrated to obtain a concentrated fraction of schizandrin extract.

2.4 dissolving the concentrated fraction of Schisandra chinensis extract in hexane to isopropanol (volume ratio 1:2), keeping at-20 ℃ for the whole night. The crude schisandra extract is then separated from the mother liquor by vacuum filtration and then washed with cold hexane.

2.5 purifying, grinding the crude schisandra extract into powder, adding cold n-hexane at 3 ℃ for leaching, and carrying out suction filtration, wherein the leaching step can be repeated until the powder becomes pure white, so as to obtain the schisandra extract.

Example 3: selection of raw material particle size

3.1 weighing 5 parts of schisandra chinensis powder with the same mass, wherein each part of schisandra chinensis powder is 200g, and sieving the schisandra chinensis powder with 20, 30, 40, 50 and 60 meshes respectively. The extraction pressure is controlled at 25MPa, the extraction temperature is 40 ℃, and the extraction time is 2h.

When the granularity of the material is 40 meshes, the content of the schisandrin B is highest, and the granularity is too coarse or too fineIn supercritical CO ₂ And (5) extracting. When the granularity of the raw materials is increased from 20 meshes to 40 meshes, the mass transfer area of the materials and the solvent is gradually increased along with the gradual reduction of the raw material particles, so that the dissolution of the components is facilitated. When the particle size of the raw material exceeds 40 mesh, the bulk density of the raw material in the extraction tank is greatly increased, so that the active ingredient is difficult to enter the solvent body through the material layer. That is, while increasing the mass transfer area, at the same time the mass transfer coefficient is also reduced, the end result is a reduced rate of mass transfer. Moreover, too fine materials can also block the pipeline of the extraction equipment, affecting the normal extraction. Therefore, the materials are not easy to be too fine, and the granularity is preferably 30-50 meshes.

3.2 dissolving 100g of Schisandra chinensis extract in 200mL of petroleum ether and applying the extract in a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether eluting silica gel column at about 3-7 mL/split. Before eluting schizandrin b, the effluent was pooled and concentrated using a rotary evaporator under reduced pressure to obtain a fatty oil concentrate fraction. Collecting eluate containing schizandrin B into pool, and concentrating to obtain lignan concentrated fraction. And (3) immediately after the elution of the schizandrin B is finished, replacing the eluting solution with acetone.

3.3A 20g fraction of lignan concentrate was dissolved in 20mL of petroleum ether/acetone (95:5, v/v (volume ratio)) and applied to a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether acetone (95:5, v/v (volume ratio)) eluting the silica gel column at about 3-7 mL/split. The permeate fraction showed that single point schizandrin b had been pooled and concentrated to obtain a concentrated fraction of schizandrin extract.

3.4 dissolving the concentrated fraction of Schisandra chinensis extract in hexane to isopropanol (volume ratio 1:2), keeping at-20℃overnight. The crude schisandra extract is then separated from the mother liquor by vacuum filtration and then washed with cold hexane.

3.5 purifying, grinding the crude schisandra extract into powder, leaching with cold n-hexane at 3 ℃, and filtering, and repeating leaching steps until the powder becomes pure white to obtain the schisandra extract.

Example 4: selection of extraction time

Supercritical CO ₂ The extraction process can be divided into three stages, namely an initial extraction stage, a conversion stage and a final extraction stage. Supercritical CO at initial stage of extraction ₂ Less substances are extracted in unit time because the substances are not in good contact with solute, and the substances enter a conversion stage along with the extension of time, the mass transfer reaches a good state, the extraction amount gradually increases until the final stage of extraction, and the extraction amount in unit time is reduced because the content of the extracted substances in the materials is reduced.

4.1 weighing 5 parts of schisandra chinensis powder with the same mass, wherein 200g of the schisandra chinensis powder is sieved by a 40-mesh sieve, the extraction pressure is controlled to be 25MPa, the extraction temperature is 40 ℃, and the extraction time is respectively 1h, 1.5h, 2h, 2.5h and 3h.

The content of the schisandrin is gradually increased along with the extension of time, the content of the schisandrin is not obviously increased along with the time after 2.5 hours, the extraction rate reaches the limit, and little benefit is obtained after the extension of time, so that the schisandrin is also a waste of energy. Moreover, the color of the extract is light in the initial stage and deep in the later stage, and is mainly caused by the dissolution of some heavy components and pigments, so that the time is not required to be too long. The extraction time is preferably 1.5-2.5 h.

4.2 dissolving 100g of Schisandra chinensis extract in 200mL of petroleum ether and applying the extract in a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether eluting silica gel column at about 3-7 mL/split. Before eluting schizandrin b, the effluent was pooled and concentrated using a rotary evaporator under reduced pressure to obtain a fatty oil concentrate fraction. Collecting eluate containing schizandrin B into pool, and concentrating to obtain lignan concentrated fraction. And (3) immediately after the elution of the schizandrin B is finished, replacing the eluting solution with acetone.

4.3A lignan concentrated fraction 20g was dissolved in 20mL of petroleum ether/acetone (95:5, v/v (volume ratio)) and applied in a preparative silica gel column (200 g,4.5 cm. Times.30 cm). The effluent was monitored by TLC using petroleum ether acetone (95:5, v/v (volume ratio)) eluting the silica gel column at about 3-7 mL/split. The permeate fraction showed that single point schizandrin b had been pooled and concentrated to obtain a concentrated fraction of schizandrin extract.

4.4 dissolving the concentrated fraction of Schisandra chinensis extract in hexane to isopropanol (volume ratio 1:2), keeping at-20 ℃ for the whole night. The crude schisandra extract is then separated from the mother liquor by vacuum filtration and then washed with cold hexane.

4.5 purifying, grinding the schisandrin B crystal into powder, leaching with cold n-hexane at 3 ℃, and filtering, and repeating leaching steps until the powder becomes pure white to obtain the schisandra extract.

Comparative example 1: reflux extraction of fructus Schisandrae extract

Pulverizing fructus Schisandrae, adding 10% calcium salt precipitant, reflux-extracting with 95% ethanol water solution (7 mL/g) for 2 times, extracting for 2 hr each time, mixing the ethanol extractive solutions, and recovering solvent under reduced pressure to obtain concentrated solution of fructus Schisandrae alcohol extract; the calcium salt precipitant is CaO.

The other steps were the same as in example 3.

Comparative example 2: and a petroleum ether-ethyl acetate binary solvent system is used in the second elution.

Loading the schisandrin B crystallization mother liquor into a silica gel chromatographic column, adding an eluent to elute for 6-10 column volumes, combining fractions containing schisandrin B, recovering the solvent under reduced pressure until the solvent is dried, adding a proper amount of n-hexane for dissolution, standing for 1-3 days, and carrying out suction filtration to obtain a schisandrin B crude product; the eluent is a petroleum ether-ethyl acetate binary solvent system with the volume ratio of 95:5; the other conditions were the same as in example 3, and the number of the schisandra powder used was 30 to 50 mesh.

Comparative example 3: the purification step was recrystallised from absolute ethanol.

Ethanol recrystallization: dissolving the crude schisandra extract in 6-10 times of absolute ethyl alcohol, suction-filtering, standing the filtrate for 1-3 days, suction-filtering, and drying to obtain the schisandra extract. The other conditions were the same as in example 3, and the number of the schisandra powder used was 30 to 50 mesh.

The quality standard of the schisandra chinensis extract with the effects of antioxidation, anti-aging, beauty and health care, which is obtained by the process, is that schisandra chinensis B is taken as an index component, and HPLC is adopted for testing, and the quality standard is as follows:

precisely weighing about 10mg of the schisandra chinensis extract, placing into a 25ml measuring flask, adding methanol to dissolve the schisandra chinensis extract, shaking the schisandra chinensis extract uniformly, and fixing the volume to a scale to obtain a sample solution. Precisely weighing Schisandrin B reference substance 10mg, placing into 25ml measuring flask, adding methanol to dissolve, shaking, and fixing volume to scale to obtain reference substance solution. Sucking 20 μl of each of the sample solution and the reference solution, and injecting into HPLC for analysis to detect schisandrin B content.

HPLC was performed using a Nova-PakC184 μm (3.9 mm. Times.300 mm) column. The mobile phase was acetonitrile and water (55:45, v/v (volume ratio)) at a flow rate of 1 ML/min. Samples (20. Mu.L) were injected and elution was monitored using Ultraviolet (UV) absorbance at 254 nm. The test results are shown in Table 1.

The content of schisandrin B measured by HPLC accounts for 25% -95% of the dry weight of the active site (schisandra extract), the equipment used in the process is simple and easy to obtain, the cost is low, and the process has a complete production flow, is very suitable for preparing schisandra extract on a large scale, and meets the production requirements of modern industrialization.

TABLE 1 detection results of Schisandra chinensis extract

As can be seen from Table 1, the amount of schisandrin B obtained by the supercritical extraction method is far higher than that by the reflux extraction, and the method can be used for preparing the schisandra chinensis extract on a large scale.

In view of the practical applicability of production, the variables should be controlled within the following ranges at the time of processing:

(1) extraction pressure: 20-30 MPa

(2) Extraction temperature: 30-50 DEG C

(3) Raw material particle size: 30-50 meshes

(4) Extraction time: 1.5 to 2.5 hours

When the secondary silica gel column chromatography eluent adopts petroleum ether-acetone and the purification mode adopts cold n-hexane for leaching, the content of the extracted schisandrin B is higher than that of other schisandrin B.

Example 5

The skin care product containing the schisandra chinensis extract in the embodiment comprises, by mass, 26 parts of jojoba oil, 2 parts of vitamin A, 2 parts of vitamin C, 26 parts of schisandra chinensis extract, 5 parts of lanolin, 2 parts of cetostearyl alcohol, 5 parts of propyl heptyl octoate, 4 parts of polydimethylsiloxane and 10000 parts of deionized water.

The preparation method comprises the following steps:

(1) Adding the vitamin A, the vitamin C, the schisandra chinensis extract obtained in the example 4, lanolin, cetostearyl alcohol, propyl heptyl octoate and polydimethylsiloxane into water, and dispersing at an ultrasonic high speed, wherein the ultrasonic frequency is 30KHz, the dispersing speed is 5200r/min, and the dispersing time is 45min;

(2) Adding the jojoba oil in parts by weight, and performing ultrasonic high-speed dispersion, wherein the ultrasonic frequency is 30KHz, and the dispersion speed is 5000r/min; mixing completely to obtain the final product.

Example 6

A skin care product containing shizandra extract in this example comprises, by mass, 28 parts of jojoba oil, 4 parts of vitamin A, 4 parts of vitamin C, 28 parts of shizandra extract obtained in example 4, 5 parts of lanolin, 2 parts of cetostearyl alcohol, 5 parts of propyl heptyl octoate, 4 parts of polydimethylsiloxane and 15000 parts of deionized water.

The preparation method comprises the following steps:

(1) Adding the vitamin A, the vitamin C, the schisandra chinensis extract, lanolin, cetostearyl alcohol, propyl heptyl octoate and polydimethylsiloxane into water, and performing ultrasonic high-speed dispersion, wherein the ultrasonic frequency is 30KHz, the dispersion speed is 5200r/min, and the dispersion time is 45min;

Example 7

A skin care product containing shizandra extract in this example comprises, by mass, 30 parts of jojoba oil, 3 parts of vitamin A, 3 parts of vitamin C, 30 parts of shizandra extract obtained in example 4, 10 parts of lanolin, 2 parts of cetostearyl alcohol, 5 parts of propyl heptyl octoate, 4 parts of polydimethylsiloxane and 20000 parts of deionized water.

The preparation method comprises the following steps:

(1) Adding the vitamin A, the vitamin C, the schisandrin B, the lanolin, the cetostearyl alcohol, the propyl heptyl octoate and the polydimethylsiloxane into water, and dispersing at an ultrasonic high speed, wherein the ultrasonic frequency is 30KHz, the dispersing speed is 5200r/min, and the dispersing time is 45min;

Comparative example 4 (no added Schisandra chinensis extract, other ingredients were contained in the same amounts as in example 6)

(1) Adding the vitamin A, the vitamin C, the lanolin, the cetostearyl alcohol, the propyl heptyl octoate and the polydimethylsiloxane into water, and performing ultrasonic high-speed dispersion, wherein the ultrasonic frequency is 30KHz, the dispersion speed is 5200r/min, and the dispersion time is 45min;

Comparative example 5 (no added cetostearyl alcohol, other component content same as in example 6)

(1) Adding the schisandra chinensis extract (obtained in example 4), vitamin A, vitamin C, lanolin, propyl heptyl octoate and polydimethylsiloxane into water, and performing ultrasonic high-speed dispersion, wherein the ultrasonic frequency is 30KHz, the dispersion speed is 5200r/min, and the dispersion time is 45min;

Comparative example 6 (vitamin A, vitamin C were not added, the other components were contained in the same amounts as in example 6)

(1) Adding the schisandra chinensis extract (obtained in example 4), lanolin, cetostearyl alcohol, propyl heptyl octoate and polydimethylsiloxane into water, and performing ultrasonic high-speed dispersion, wherein the ultrasonic frequency is 30KHz, the dispersion speed is 5200r/min, and the dispersion time is 45min;

The creams prepared in examples 5 to 7 and comparative examples 4 to 6 were continuously tried for 30 days by 100 persons aged 25 to 55 years, respectively, and the anti-aging effect of the creams prepared in the above examples was evaluated by comparative analysis. Wherein the anti-aging effect is the improvement of rough skin, skin elasticity, fine lines of eyes and mouth, wrinkles and the like, and the results are shown in Table 2.

TABLE 2 comprehensive scoring results for human trial evaluation

As can be seen from the results in Table 2, the improvement degree of each product in examples on skin dryness, skin elasticity, fine lines of eyes and mouth, wrinkles and the like is very remarkable, and the anti-wrinkle effect is remarkable as compared with the similar skin care products on the market. The greater the weight part of the schisandra chinensis extract, the higher the improvement degree. The skin care product containing the schisandra chinensis extract has comfortable skin feel, no irritation, obvious anti-wrinkle and anti-aging effects, and healthy and elastic skin after use.

Claims

1. A skin care product comprising schisandra chinensis extract, comprising:

26-30 parts of jojoba oil;

26-30 parts of schisandra chinensis extract;

5-10 parts of lanolin;

the schisandra chinensis extract takes schisandra chinensis B extract as an index component, and the content of the schisandra chinensis B extract is 25-95 wt%;

further comprises:

2-5 parts by weight of vitamin A;

2-5 parts by weight of vitamin C;

0.5 to 2 weight portions of emulsifying agent;

2-6 parts of essence;

1-5 parts by weight of a milk type matrix;

10000-20000 parts by weight of water;

the schisandra chinensis extract is prepared according to the following method:

s1) crushing the schisandra chinensis to obtain schisandra chinensis powder;

s2) performing supercritical carbon dioxide extraction on the schisandra chinensis powder to obtain a supercritical extract; the extraction pressure of the supercritical carbon dioxide extraction is 20-30 MPa; the extraction temperature is 30-50 ℃; the extraction time is 1.5-2.5 h;

s5) leaching and purifying the crude schisandra chinensis extract by using hexane at 0-8 ℃ to obtain the schisandra chinensis extract;

the step S3) specifically comprises the following steps:

a) Dissolving the supercritical extract with an organic solvent, performing silica gel column chromatography, eluting with a first eluent, separating, and concentrating to obtain lignan concentrated fraction; the organic solvent is petroleum ether; the first eluent is petroleum ether;

the volume ratio of hexane to isopropanol in the step S4) is 1: (1.5-2.5); the temperature of the low-temperature crystallization is-10 ℃ to-30 ℃.

2. A skin care product according to claim 1, characterized in that the emulsifier is selected from cetostearyl alcohol and/or squalane; the essence is selected from one or more of propyl heptyl octoate, p-tert-butyl cyclohexyl acetate and ethyl salicylate; the emulsion type matrix is selected from polydimethylsiloxane.

3. A skin care product according to claim 1, comprising:

26-30 parts of jojoba oil;

26-30 parts of schisandra chinensis extract;

5-10 parts of lanolin;

2-4 parts by weight of vitamin A;

2-4 parts by weight of vitamin C;

2 parts by weight of cetostearyl alcohol;

5 parts by weight of propyl heptyl octanoate;

4 parts by weight of polydimethylsiloxane;

10000 to 20000 parts by weight of water.

4. The skin care product according to claim 1, wherein the schisandra chinensis powder has a mesh number of 30-50 mesh.

5. The skin care product according to claim 1, wherein the flow rate of the first eluent in the step A) is 3-7 ml/min;

and B), the flow rate of the second eluent in the step B) is 3-7 ml/min.

6. The skin care product according to claim 1, wherein the mass-to-volume ratio of the concentrated fraction of schisandra chinensis extract to the mixed solvent in the step S4) is 1 g: (1-3) ml.

7. A method for preparing a skin care product containing shizandra extract as claimed in claim 1, comprising:

8. The method according to claim 7, wherein the ultrasonic frequency of the ultrasonic high-speed dispersion in the step S1) is 20 to 40 KHz; the speed of ultrasonic high-speed dispersion is 5000-5400 r/min; the time is 30-60 min;