CN107157823B - Nano-liposome sunscreen emulsion and preparation method thereof - Google Patents
Nano-liposome sunscreen emulsion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano-liposome sunscreen emulsion and a preparation method thereof, wherein the nano-liposome sunscreen emulsion is prepared from a raw material composition containing the following components in percentage by weight, wherein the total weight of the raw material composition is 100 percent: 1-3 wt% of a cosmetic matrix, 1-3 wt% of a moisturizing factor base material, 10-20 wt% of a humectant, 2-5 wt% of a sophora flower bud/scutellaria baicalensis root composite extract, 10-20 wt% of lipid, 1-3 wt% of a seaweed extract, 0.01-0.1 wt% of an antioxidant, 5-10 wt% of a solubilizer and the balance of deionized water. The nano-liposome sunscreen emulsion provided by the invention has good sunscreen effect and stability.
Description
The technical field is as follows:
the invention belongs to the field of chemical and daily chemical products, and relates to a sunscreen emulsion, in particular to a nano liposome sunscreen emulsion and a preparation method thereof.
(II) technical background:
sunlight is composed of continuous electromagnetic waves and is divided into an ultraviolet region, a visible light region and an infrared region. Sunburn caused by exposure of the skin to solar radiation is mainly caused by Ultraviolet (UV) rays, and erythema often occurs during sunburn, and edema, blisters, desquamation and the like are accompanied in severe cases. The penetration of UV rays through the skin varies, leading to different biological effects, short wave sterilizing Ultraviolet (UVC), although having the highest energy, is mostly absorbed by stratospheric ozone. Truly contributing to sunburn of the skin are long wave black spot effect Ultraviolet (UVA) and medium wave red spot effect Ultraviolet (UVB). UVB is able to penetrate the upper stratum corneum layer of the skin surface, and prolonged exposure to UVB can cause DNA mutations that lead to skin cancer. UVA penetration through the dermis layer, which penetrates the epidermis, stimulates melanogenesis, leading to skin aging, and UVA potentiates the carcinogenic effects of UVB on the skin. The sunscreens in current day-to-day sunscreen preparations are mainly divided into Inorganic microparticles (Inorganic particles) and Organic uv absorbers (Organic uv absorbers). Inorganic particles such as nano titanium dioxide and zinc oxide can effectively attenuate ultraviolet rays, and are well dispersed in sunscreen products, so that the sunscreen products are convenient to use, but the safety of the products is easy to question by consumers due to the common use of the ultrafine particles. The artificial organic ultraviolet absorbent comprises benzophenones, salicylic acid derivatives, cinnamic acid derivatives and the like, and the artificial organic ultraviolet absorbent has a mature research on the absorption range of an ultraviolet band, for example, cresol troxazole trisiloxane has good absorption on UVA/B of 260-360 nm. However, the safe use of such sunscreens is not uniformly regulated in various countries, and problems such as contact dermatitis and the like may occur when the sunscreens are improperly used.
The extract of the scutellaria baicalensis is one of the traditional Chinese herbal medicines in China, the extract of the scutellaria baicalensis roots has the functions of resisting inflammation and allergic reaction, and can relieve the stimulation and allergy of chemical additives to the skin, the extract of the scutellaria baicalensis has the strong absorption function on the ultraviolet rays between 280nm and 320nm (UVA), and the extract of the Sophora japonica has good absorption on both UVA and UVB after being compounded with the extract of the scutellaria baicalensis, and has good absorption effect on the ultraviolet rays in cosmetics.
The main active substances of the sophora flower bud extract and the scutellaria baicalensis extract are rutin and baicalein which are insoluble or slightly soluble in water, and the commercial sunscreen product is usually a common emulsion containing the sophora flower bud extract or the scutellaria baicalensis extract. The nanoliposome emulsion can release active substances on skin continuously, and reduce irritation of cosmetics. However, since the liposome membrane is not a hard structure but forms a liquid envelope, other amphiphilic molecules in cosmetics, such as surfactants, can be inserted into the phospholipid layer, which destabilizes the liposome and even induces the particles to dissolve. In order to stabilize liposomes, conventional methods are low temperature storage, addition of nanoparticles and increasing the viscosity of the external phase. These methods, while effective, present problems of inconvenience in transportation, use, or other safety risks. Therefore, the method for finding the effective stabilizing method is very practical and valuable.
(III) the invention content:
the invention aims to provide a nano-liposome sunscreen emulsion with good sunscreen effect and stability and a preparation method thereof.
In order to achieve the first object, the invention adopts the following technical scheme:
a nanoliposome sunscreen emulsion is prepared from a raw material composition containing the following components in percentage by weight, wherein the content of each component is represented by the following weight percentage based on 100 percent of the total weight of the raw material composition:
wherein the cosmetic matrix is cetostearyl alcohol, the moisturizing factor base material is caprylic/capric triglyceride, the humectant is one or more of glycerol, propylene glycol and butanediol, the lipid is a mixture of soybean lecithin and cholesterol, the antioxidant is tocopherol acetate, and the solubilizer is one or more of tween-80 and propylene glycol dicaprylate/dicaprate;
the sophora flower bud/scutellaria baicalensis root composite extract is obtained by mixing a sophora flower bud extract and a scutellaria baicalensis extract according to the mass ratio of 2:1, wherein the sophora flower bud extract is obtained by extracting sophora flower buds with ethanol, cooling, crystallizing and refining, and the scutellaria baicalensis extract is obtained by performing enzymolysis on scutellaria baicalensis roots with cellulase, extracting with ethanol, filtering, removing a solvent and drying;
the preparation method of the seaweed extract comprises the following steps: the ulva fasciata is subjected to water extraction, alcohol precipitation, impurity removal, protein removal, purification and separation to obtain a seaweed extract.
In the present invention, the content of deionized water as "balance" means: the components of the raw material composition except the deionized water have limited weight percentage content, and after all the components are added, the deionized water is finally used for complementing to 100 percent.
The functions and effects of the specific ingredients of the raw material composition of the present invention will be described in detail hereinafter.
In the invention, the cosmetic matrix is cetostearyl alcohol, and has the effects of inhibiting greasy feeling, reducing viscosity of wax raw materials, stabilizing cosmetic emulsion and the like. The content of the cosmetic matrix is 1-3%, preferably 2%, based on 100% of the total weight of the raw material composition.
In the invention, the moisturizing factor base material is caprylic acid/capric acid triglyceride, is high-clear odorless grease, belongs to palm oil or coconut oil derivatives, and has the function of filtering ultraviolet rays. The content of the moisturizing factor base material is 1-3%, preferably 2%, based on 100% of the total weight of the raw material composition.
In the present invention, in the preparation of the sophora flower bud extract, the refining is preferably performed by recrystallization with ethanol, and the above operation may be repeated as many times as necessary. The main active substance rutin in the sophora flower bud extract, the rutin content in the sophora flower bud is about 20 percent, and the distribution is concentrated. Rutin can strongly absorb ultraviolet rays between 320nm and 400nm (UVB), can also inhibit key enzymes of allergic media, and has good anti-inflammation property. The scutellaria baicalensis is one of the traditional Chinese herbal medicines, and is firstly subjected to enzymolysis by using cellulase, preferably neutral cellulase before extraction, so that the raw material fibrous tissue is damaged, and the baicalein is easier to dissolve. The Scutellariae radix extract contains baicalein as main active ingredient, has antiinflammatory and antiallergic effects, and can relieve skin irritation and allergy caused by chemical additives. The baicalein has strong absorption effect on ultraviolet rays between 280nm and 320nm (UVA), and tests show that the inhibition rate of the baicalein with the concentration of 0.002 percent on the UVA phototoxicity reaches 75 percent. Rutin and baicalein are used as cosmetic raw materials in the bulletin about the name catalogue of the used cosmetic raw materials published by the State food and drug administration Master 2014, and in the CTFA and Chinese name catalogue of the International cosmetic raw material Standard 2010 edition, the report that the rutin and the baicalein are unsafe to be externally used is not found. The content of the sophora flower bud/scutellaria root composite extract is 2-5 percent based on 100 percent of the total weight of the raw material composition.
In the invention, the lipid is a mixture of soybean lecithin and cholesterol, and the mass ratio of the soybean lecithin to the cholesterol in the mixture is preferably 10-5: 1. wherein the soybean lecithin has higher unsaturated chain and yellowish color, has no bad smell, and cholesterol is easy to be mixed into the lecithin to enhance the double-layer structure of the lecithin. The content of the lipid is 10-20%, preferably 20%, based on 100% of the total weight of the raw material composition.
In the invention, the seaweed extract is prepared by water extraction and alcohol precipitation of ulva fasciata, active polysaccharide and water-soluble active substances in seaweed are dissolved out by hot water at a certain temperature, and the seaweed extract is obtained by removing impurities, removing proteins, purifying and separating after alcohol precipitation, preferably by using a Sevage reagent method. In order to accelerate the dissolution of the polysaccharide in the seaweed, the invention can also adopt physical means such as enzymolysis (such as cellulase enzymolysis), ultrasonic wave, microwave and the like to perform auxiliary extraction. The seaweed extract prepared by the invention contains seaweed polysaccharide as a main component, is an important active substance, not only has the moisturizing and skin moistening effects of natural polysaccharide, but also has the activities of resisting oxidation, inhibiting skin allergy, resisting inflammation and the like. In addition, other active substances such as kainic acid micromolecules contained in the seaweed extract can inhibit the activity of melanin-related enzyme in skin, and has whitening effect. The seaweed extract accounts for 1-3 percent of the total weight of the raw material composition as 100 percent.
In the invention, the antioxidant is tocopherol acetate which is used as an in-vivo antioxidant, can eliminate in-vivo free radicals and reduce the damage of ultraviolet rays to a human body. The content of the antioxidant is 0.01-0.1 percent based on 100 percent of the total weight of the raw material composition.
In the invention, the solubilizer is one or more of tween-80 and propylene glycol dicaprylate/dicaprate. The solubility of active substances such as rutin, baicalein and the like in the emulsion can be improved by the Tween-80 and the propylene glycol dicaprylate/dicaprate, so that the effect of promoting transdermal absorption is achieved. The content of the solubilizer is 5-10 percent, preferably 8-10 percent based on the total weight of the raw material composition as 100 percent.
The raw material composition of the nano-liposome sunscreen emulsion can also comprise other components according to actual needs.
Preferably, the raw materials of the nanoliposome sunscreen emulsion comprise a cosmetic matrix, a moisturizing factor base material, a humectant, a sophora flower bud/scutellaria baicalensis composite extract, lipid, a seaweed extract, an antioxidant, a solubilizer and deionized water.
The invention also provides a preparation method of the nano-liposome sunscreen emulsion, which comprises the following steps:
(1) weighing cetearyl alcohol, a mixture of soybean lecithin and cholesterol, a sophora flower bud/scutellaria baicalensis composite extract, a solubilizer, a moisturizing factor base material and an antioxidant according to the formula ratio, mixing and fully stirring at the temperature of 55-60 ℃ until an oil phase is uniform, and keeping the temperature for 5-15 min;
(2) weighing the humectant and the seaweed extract according to the formula ratio, dissolving in deionized water, heating to 55-60 ℃, stirring to form a uniform water phase, and keeping the temperature for 5-15 min;
(3) pumping the oil phase prepared in the step (1) into the water phase prepared in the step (2) for premixing, shearing at a high speed for 15-30 min by using a high-speed shearing machine, and preserving heat at 55-60 ℃ for 5-15 min to prepare a primary emulsion;
(4) and introducing the primary emulsion into an ultrahigh-pressure micro-jet nano dispersion homogenizer, homogenizing under the pressure of 68.9-137.9 MPa, extruding the homogenized dispersion liquid through a filter membrane with the average pore diameter of 100nm, and naturally cooling to room temperature to obtain the nano-liposome sunscreen emulsion.
Compared with the prior art, the nano-liposome sun-screening emulsion prepared by the invention has the following advantages:
1. the sophora flower bud extract and the scutellaria baicalensis extract are compounded, the compound has excellent antioxidant effect, can cover UVA and UVB wave bands when absorbing ultraviolet regions, and is a natural, safe and effective ultraviolet absorbent. The liposome can improve bioavailability of active substances such as flos Sophorae Immaturus/Scutellariae radix composite extract, etc., and can also improve skin condition. Therefore, the sophora flower bud/scutellaria baicalensis composite extract can effectively enhance and prolong the good effect of cosmetic repair by combining the slow release characteristic and the repair function of the liposome, so that the nano-liposome sun-screening emulsion prepared by the invention has an excellent sun-screening effect.
2. Compared with the common nano liposome emulsion, the added algal polysaccharide extract mainly plays a role in enhancing the liposome, algal polysaccharide molecules can be embedded among phospholipid molecules, so that a system forms a stable particle-membrane, the core diameter is smaller than that of the original phospholipid body, and the core diameter is more stable. The smaller diameter of the nano-liposome emulsion can easily permeate into the intercellular spaces of the stratum corneum and reach the lipid bilayer to be dissolved and release active substances, so that the prepared nano-liposome emulsion can better resist the damage of a surfactant and has good stability.
3. The anion groups in the seaweed extract enable the outer layer of the liposome after being embedded with polysaccharide molecules to have negative charges, and experiments prove that the effect of the liposome with the negative charges on the skin stratum corneum is better than that of the liposome with positive charges, and active substances carried by the liposome penetrate through the stratum corneum to have better antioxidant, anti-inflammatory and whitening nutritional effects on the skin.
(IV) description of the drawings
Figure 1 is a preparation scheme of nanoliposome sunscreen emulsion.
Fig. 2 is a particle size distribution diagram of the nanoliposome sunscreen emulsion.
FIG. 3 is a diagram of the mechanism of sunscreen of the composite extract of flos Sophorae Immaturus/Scutellariae radix.
FIG. 4 is a diagram showing the mechanism of action of the seaweed extract on liposomes, wherein (a) shows that polysaccharide molecules in the seaweed extract are intercalated between phospholipid molecules and the liposomes are negatively charged, and (b) shows that the cone structure stabilizes the barrier membrane in the system.
FIG. 5 is a UV absorption spectrum of each of the emulsions prepared in examples 1 and 2 and comparative example 1. The result shows that the sunscreen lotion containing the sophora flower bud/scutellaria baicalensis composite extract has better ultraviolet absorption in UVA-UVB, and the blank lotion has weaker ultraviolet absorption.
FIG. 6 is a graph showing the change of the average particle diameter of each of the emulsions prepared in examples 1 and 2 and comparative example 2 in 0 to 30 days at room temperature (20 ℃) and ξ potential measurement data, wherein a bar graph shows the particle diameter of the emulsion and a dotted point shows the potential of the emulsion, the average particle diameter and ξ potential of the emulsion reflect the relative stability of the emulsion, and the smaller the particle diameter, the higher the ξ potential (positive or negative), the better the stability of the emulsion.
(V) detailed description of the preferred embodiments
The technical solution of the present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited thereto:
example 1:
(1) pulverizing fresh dried flos Sophorae Immaturus into powder with average particle size of 60 mesh, adding 20 times of ethanol, heating and reflux extracting for 2 hr, filtering to remove solid impurities to obtain filtrate, and concentrating the filtrate to original volume by rotary evaporator
Cooling and crystallizing to obtain a crude product. Re-dissolving the crude product in 5 times (w/v) hot ethanol (50 deg.C), centrifuging at 8000r/min for 10min, collecting supernatant, rotary evaporating, concentrating, crystallizing, and repeating for 3 times to obtain refined flos Sophorae Immaturus extract. Pulverizing radix Scutellariae to average particle size of 30 mesh, adding 0.05 wt% neutral cellulase (15 wu/g, Ningxia and Kyobi Biotechnology Co., Ltd.) and 10 times of water, heating to 50 deg.C, and performing enzymolysis for 1.5 hr. Filtering, extracting the filter cake with 10 times volume of ethanol under reflux at 70 + -0.5 deg.C for 2 hr, repeating twice, mixing extractive solutions, filtering, distilling under reduced pressure to obtain powder, and drying to obtain Scutellariae radix extract. According to the mass ratio of 2:1 weighing and mixing the sophora flower bud extract and the scutellaria baicalensis extract to obtain the sophora flower bud/scutellaria baicalensis composite extract.
(2) Weighing 2.0g of cetearyl alcohol, 20.0g of a mixture of soybean lecithin and cholesterol (the mass ratio is 4: 1), 5.0g of sophora flower bud/scutellaria baicalensis composite extract, 8.0g of propylene glycol dicaprylate/dicaprate, 2.0g of caprylic/capric triglyceride and 0.05g of tocopheryl acetate, mixing at the temperature of 55 ℃, fully stirring to obtain a uniform oil phase, and keeping the temperature for 15 min;
(3) adding 20 times volume of water into dried Ulva lactuca, heating to boil, stirring, leaching, filtering under reduced pressure to obtain filtrate, rotary evaporating and concentrating to obtain concentrated solution
Centrifuging at 8000r/min for 10min to remove part of fine solid impurities, collecting supernatant, and rotary evaporating to obtain the final product
Adding ethanol according to the volume of 1: 2, centrifuging at high speed to obtain precipitate, deproteinizing by a Sevage reagent method, and freeze-drying to obtain seaweed extract dry powder, weighing 15.0g of a mixture of glycerol and propylene glycol (the mass ratio is 1: 1) and 2.0g of the seaweed extract prepared by the method, dissolving in 46m L deionized water, heating to 55 ℃, stirring to obtain a uniform water phase, and keeping the temperature for 15 min;
(4) pumping the oil phase prepared in the step (2) into the water phase prepared in the step (3) for premixing, shearing for 30min by using an IKA ultra-high-speed high-shear emulsification dispersion machine (DRS2000), and preserving heat for 15min at 55 ℃ to prepare a primary emulsion;
(5) introducing the primary emulsion into an APV1000 type ultrahigh pressure micro-jet nano dispersion homogenizer, and homogenizing under 900bar pressure. Extruding the dispersion liquid through a 100nm film, and naturally cooling to room temperature to obtain the nano liposome emulsion.
Example 2:
(1) pulverizing fresh dried flos Sophorae Immaturus into powder with average particle size of 60 mesh, adding 20 times of ethanol, heating and reflux extracting for 2 hr, filtering to remove solid impurities to obtain filtrate, and concentrating the filtrate to original volume by rotary evaporator
Cooling and crystallizing to obtain a crude product. Re-dissolving the crude product in 5 times (w/v) hot ethanol (50 deg.C), centrifuging at 8000r/min for 10min, collecting supernatant, rotary evaporating, concentrating, crystallizing, and repeating for 3 times to obtain refined flos Sophorae Immaturus extract. Pulverizing radix Scutellariae to average particle size of 30 mesh, adding 0.05 wt% neutral cellulase (15 wu/g, Ningxia and Kyobi Biotechnology Co., Ltd.) and 10 times of water, heating to 50 deg.C, and performing enzymolysis for 1.5 hr. Filtering, extracting the filter cake with 10 times of ethanol at 70 + -0.5 deg.C under reflux for 2 hr, repeating twice, mixing extractive solutions, filtering, distilling under reduced pressure to obtain powder, and drying to obtain Scutellariae radix extract. According to the mass ratio of 2:1 weighing and mixing the sophora flower bud extract and the scutellaria baicalensis extract to obtain the sophora flower bud/scutellaria baicalensis composite extract.
(2) Weighing 2.0g of cetearyl alcohol, 20.0g of a mixture of soybean lecithin and cholesterol (the mass ratio is 4: 1), 3.0g of sophora flower bud/scutellaria baicalensis composite extract, 10.0g of propylene glycol dicaprylate/dicaprate, 2.0g of caprylic/capric triglyceride and 0.1g of tocopheryl acetate, mixing at the temperature of 60 ℃, fully stirring until an oil phase is uniform, and preserving heat for 15 min;
(3) adding 20 times volume of water into dried Ulva lactuca, heating to boil, stirring, leaching, filtering under reduced pressure to obtain filtrate, rotary evaporating and concentrating to obtain concentrated solution
Centrifuging at 8000r/min for 10min to remove part of fine solid impurities, collecting supernatant, and rotary evaporating to obtain the final product
Adding ethanol according to the volume of 1: 2, centrifuging at high speed to obtain precipitate, deproteinizing by a Sevage reagent method, and freeze-drying to obtain seaweed extract dry powder, weighing 20.0g of a mixture of glycerol and propylene glycol (in a mass ratio of 1: 1) and 3.0g of the seaweed hot water extract prepared by the method, dissolving in 40m L deionized water, heating to 60 ℃, stirring to obtain a uniform water phase, and keeping the temperature for 15 min;
(4) pumping the oil phase prepared in the step (2) into the water phase prepared in the step (3) for premixing, shearing for 30min by using an IKA ultra-high-speed high-shear emulsification dispersion machine (DRS2000), and preserving heat for 15min at 60 ℃ to prepare a primary emulsion;
(5) introducing the primary emulsion into an APV2000 type ultrahigh pressure micro-jet nano dispersion homogenizer, and homogenizing under 1200bar pressure. Extruding the dispersion liquid through a 100nm film, and naturally cooling to room temperature to obtain the nano liposome emulsion.
The liposome emulsion obtained in example 2 was subjected to preliminary examination using a Mastersizer 20 laser particle size analyzer. As shown in fig. 2.
Comparative example 1: blank emulsion without sophora flower bud/scutellaria baicalensis composite extract
(1) Weighing 2.0g of cetearyl alcohol, 20.0g of a mixture of soybean lecithin and cholesterol (the mass ratio is 4: 1), 10.0g of propylene glycol dicaprylate/dicaprate, 2.0g of caprylic/capric triglyceride and 0.1g of tocopheryl acetate, mixing and fully stirring at the temperature of 60 ℃ until an oil phase is uniform, and keeping the temperature for 15 min;
(2) adding 20 times volume of water into dried Ulva lactuca, heating to boil, stirring, leaching, filtering under reduced pressure to obtain filtrate, rotary evaporating and concentrating to obtain concentrated solution
Centrifuging at 8000r/min for 10min to remove part of fine solid impurities, collecting supernatant, and rotary evaporating to obtain the final product
Adding ethanol according to the volume of 1: 2, centrifuging at high speed to obtain precipitate, deproteinizing by a Sevage reagent method, and freeze-drying to obtain seaweed extract dry powder, weighing 20.0g of a mixture of glycerol and propylene glycol (in a mass ratio of 1: 1) and 3.0g of the seaweed hot water extract prepared by the method, dissolving in 43m L deionized water, heating to 60 ℃, stirring to obtain a uniform water phase, and keeping the temperature for 15 min;
(3) pumping the oil phase prepared in the step (1) into the water phase prepared in the step (2) for premixing, shearing for 30min by using an IKA ultra-high-speed high-shear emulsification dispersion machine (DRS2000), and preserving heat for 15min at 60 ℃ to prepare a primary emulsion;
(4) introducing the primary emulsion into an APV2000 type ultrahigh pressure micro-jet nano dispersion homogenizer, and homogenizing under 1200bar pressure. Extruding the dispersion liquid through a 100nm film, and naturally cooling to room temperature to obtain the nano liposome emulsion.
Comparative example 2: blank emulsion without seaweed extract
(1) Pulverizing fresh dried flos Sophorae Immaturus into powder with average particle size of 60 mesh, adding 20 times of ethanol, heating and reflux extracting for 2 hr, filtering to remove solid impurities to obtain filtrate, and concentrating the filtrate to original volume by rotary evaporator
Cooling and crystallizing to obtain a crude product. Re-dissolving the crude product in 5 times (w/v) hot ethanol (50 deg.C), centrifuging at 8000r/min for 10min, collecting supernatant, rotary evaporating, concentrating, crystallizing, and repeating for 3 times to obtain refined flos Sophorae Immaturus extract. Pulverizing Scutellariae radix to average particle size of 30 mesh, adding 0.05 wt% neutral cellulase (15 ten thousand u/g, Ningxia) according to the raw material weightHeishi wall biotechnology Co., Ltd.) and 10 times volume of water, heating to 50 deg.C, and performing enzymolysis for 1.5 hr. Filtering, extracting the filter cake with 10 times of ethanol at 70 + -0.5 deg.C under reflux for 2 hr, repeating twice, mixing extractive solutions, filtering, distilling under reduced pressure to obtain powder, and drying to obtain Scutellariae radix extract. According to the mass ratio of 2:1 weighing and mixing the sophora flower bud extract and the scutellaria baicalensis extract to obtain the sophora flower bud/scutellaria baicalensis composite extract.
(2) Weighing 2.0g of cetearyl alcohol, 20.0g of a mixture of soybean lecithin and cholesterol (the mass ratio is 4: 1), 3.0g of sophora flower bud/scutellaria baicalensis composite extract, 10.0g of propylene glycol dicaprylate/dicaprate, 2.0g of caprylic/capric triglyceride and 0.1g of tocopheryl acetate, mixing at the temperature of 60 ℃, fully stirring until an oil phase is uniform, and preserving heat for 15 min;
(3) weighing 20.0g of a mixture of glycerol and propylene glycol (mass ratio is 1: 1), dissolving in 43m L deionized water, heating to 60 ℃, stirring to obtain a uniform water phase, and keeping the temperature for 15 min;
(4) pumping the oil phase prepared in the step (2) into the water phase prepared in the step (3) for premixing, shearing for 30min by using an IKA ultra-high-speed high-shear emulsification dispersion machine (DRS2000), and preserving heat for 15min at 60 ℃ to prepare a primary emulsion;
(5) introducing the primary emulsion into an APV2000 type ultrahigh pressure micro-jet nano dispersion homogenizer, and homogenizing under 1200bar pressure. Extruding the dispersion liquid through a 100nm film, and naturally cooling to room temperature to obtain the nano liposome emulsion.
And (3) performance testing:
1. antioxidant effect of flos Sophorae Immaturus/Scutellariae radix extract
The antioxidant effect of the sophora flower bud/scutellaria baicalensis extract on skin is evaluated by measuring the antioxidant index of the sophora flower bud/scutellaria baicalensis extract in vitro by using a free radical reagent. The specific test method comprises the following steps:
① Hydroxyl radical elimination ratio by ultraviolet-visible spectrophotometry (Hydroxyl radical radiation by UV spectrophotometry, 2014)
② superoxide radical eliminating rate ESR Spectroscopy (Free-radial active and active effective impact of greenk organic isolated by SFE, 2014)
③ singlet oxygen radical elimination rate spectrophotometry (Steinbeck M J, et al. J Biol Chem,1993)
④ lipid peroxidation inhibition Thiobabital acid reaction method (Nakashima et al,2001)
The results are shown in table 1, which shows that the sophora flower bud/scutellaria baicalensis extract has good antioxidation, can reduce the damage of ultraviolet rays to human skin, and has far better effect than ascorbic acid.
TABLE 1
2. Ultraviolet absorption spectrum of emulsion
The results are shown in FIG. 5, which is a UV absorption spectrum for each of the emulsions prepared in examples 1 and 2 and comparative example 1. The results show that the sunscreen emulsions containing the sophora flower bud/scutellaria baicalensis complex extract prepared in examples 1 and 2 have better ultraviolet absorption in UVA to UVB, while the blank emulsion containing no sophora flower bud/scutellaria baicalensis complex extract prepared in comparative example 1 has weaker ultraviolet absorption.
3. SPF (Sun protection factor) test
SPF (Sun protection factor) is defined as the ratio of the MED (minimum amount of erythema) required to cause erythema on skin protected by sunscreen cosmetics to the MED required to cause erythema on unprotected skin2The SPF value of the sample is calculated by the instrument detection and is shown in the following table. The SPFs of examples 1, 2 both exceed 20, indicating that the sunscreen emulsions prepared according to examples 1, 2 are capable of absorbing more than 95% of the UV radiation, and are significantly more effective compared to the reference.
4. Emulsion stability
FIG. 6 is a graph showing the change of the average particle size of the emulsions prepared in examples 1 and 2 and comparative example 2 in 0-30 days at room temperature (20 ℃) and the ξ potential measurement data, wherein the average particle size and ξ potential of the emulsions reflect the relative stability of the emulsions, and the smaller the particle size, the higher the ξ potential (positive or negative), the better the emulsion stability, as can be seen from the results in FIG. 6, the particle size of the emulsions in the blank control group is significantly increased compared with those in examples 1 and 2 during storage, and similarly, the absolute value of the ξ potential of the emulsions in the blank control group is significantly reduced, and the difference between the particle size and the ξ potential of examples 1 and 2 is not significant, which indicates that the storage stability of the liposome emulsions is better after the algal polysaccharide extract is.
Claims (6)
1. A nanoliposome sunscreen emulsion is prepared from a raw material composition containing the following components in percentage by weight, wherein the content of each component is represented by the following weight percentage based on 100 percent of the total weight of the raw material composition:
wherein the cosmetic matrix is cetostearyl alcohol, the moisturizing factor base material is caprylic/capric triglyceride, the humectant is one or more of glycerol, propylene glycol and butanediol, the lipid is a mixture of soybean lecithin and cholesterol, the antioxidant is tocopherol acetate, and the solubilizer is one or more of tween-80 and propylene glycol dicaprylate/dicaprate;
the sophora flower bud/scutellaria baicalensis root composite extract is obtained by mixing a sophora flower bud extract and a scutellaria baicalensis extract according to the mass ratio of 2:1, wherein the sophora flower bud extract is obtained by extracting sophora flower buds with ethanol, cooling, crystallizing and refining, and the scutellaria baicalensis extract is obtained by performing enzymolysis on scutellaria baicalensis roots with cellulase, extracting with ethanol, filtering, removing a solvent and drying;
the preparation method of the seaweed extract comprises the following steps: water extracting and alcohol precipitating the ulva fasciata, and removing impurities, deproteinizing, purifying and separating by using a Sevage reagent method to obtain a seaweed extract;
the preparation method of the nano-liposome sunscreen emulsion comprises the following steps:
(1) weighing cetearyl alcohol, a mixture of soybean lecithin and cholesterol, a sophora flower bud/scutellaria baicalensis composite extract, a solubilizer, a moisturizing factor base material and an antioxidant according to the formula ratio, mixing and fully stirring at the temperature of 55-60 ℃ until an oil phase is uniform, and keeping the temperature for 5-15 min;
(2) weighing the humectant and the seaweed extract according to the formula ratio, dissolving in deionized water, heating to 55-60 ℃, stirring to form a uniform water phase, and keeping the temperature for 5-15 min;
(3) pumping the oil phase prepared in the step (1) into the water phase prepared in the step (2) for premixing, shearing at a high speed for 15-30 min by using a high-speed shearing machine, and preserving heat at 55-60 ℃ for 5-15 min to prepare a primary emulsion;
(4) and introducing the primary emulsion into an ultrahigh-pressure micro-jet nano dispersion homogenizer, homogenizing under the pressure of 68.9-137.9 MPa, extruding the homogenized dispersion liquid through a filter membrane with the average pore diameter of 100nm, and naturally cooling to room temperature to obtain the nano-liposome sunscreen emulsion.
2. The nanoliposome sunscreen emulsion according to claim 1 wherein: in the preparation process of the sophora flower bud extract, the refining is to recrystallize by ethanol.
3. The nanoliposome sunscreen emulsion according to claim 1 wherein: the cellulase is neutral cellulase.
4. The nanoliposome sunscreen emulsion according to claim 1 wherein: the mass ratio of the soybean lecithin to the cholesterol in the lipid is 10-5: 1.
5. the nanoliposome sunscreen emulsion according to claim 1 wherein: in the preparation of the seaweed extract, Sevage reagent method is used for removing impurities, deproteinizing, purifying and separating.
6. The nanoliposome sunscreen emulsion according to any one of claims 1 to 5 wherein: the raw materials of the nano-liposome sunscreen emulsion comprise a cosmetic matrix, a moisturizing factor base material, a humectant, a sophora flower bud/scutellaria baicalensis composite extract, lipid, a seaweed extract, an antioxidant, a solubilizer and deionized water.
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| CN109771339B (en) * | 2019-03-13 | 2021-07-30 | 中国热带农业科学院椰子研究所 | Preparation method of coconut oil nano-emulsion with whitening and moisturizing effects |
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