A nano-encapsulated oil-control composition, preparation method and use

Abstract

The present invention belongs to the technical field of daily-use cosmetics, and specifically relates to the preparation and application of a nano-encapsulated oil-control composition. By weight percentage, the nano-encapsulated oil-control composition comprises the following components: 2%-6% of ginger root extract, 10%-20% of Platycladus orientalis leaf extract, 2%-6% of calendula extract, 1%-3% of niacinamide, 0.2%-0.7% of adenosine, 5%-10% of emulsifier, 0%-35% of co-emulsifier, 0.1%-3% of preservative, and the balance is water. The various components act synergistically in many aspects, can maintain the scalp physiological environment in many aspects, and at the same time regulate the microbial balance, oil secretion balance, and metabolic balance of the scalp environment, achieving a stronger oil-control effect.

Description

Technical Field

[0001] The present invention belongs to the technical field of daily-use cosmetics, and particularly relates to the preparation and application of a nano-encapsulated oil-control composition. Background Art

[0002] The oil on human skin is mainly secreted by sebaceous glands and has a certain function of protecting the skin. It can prevent direct damage from solar ultraviolet rays and resist the invasion of external allergenic factors. However, excessive sebum secretion will cause the accumulation of secretions around hair follicles, resulting in hair follicle blockage or atrophy. In severe cases, it may even lead to seborrheic dermatitis, seborrheic alopecia, etc. Scalp seborrheic dermatitis is common, and its main symptoms are itchy scalp, excessive dandruff, and excessive scalp oil. The ecological environment of the scalp is related to the balance of oil, flora, and metabolism. When any balance in the scalp ecological environment is disrupted, a chain reaction is likely to occur. For example, Malassezia is a normal parasitic flora on the surface of the human scalp and is a lipophilic fungus. When Malassezia multiplies excessively, it decomposes oil to generate excessive unsaturated fatty acids, which stimulate the scalp to cause inflammation and itching, and accelerate the metabolism of the scalp cutin layer, resulting in excessive exfoliation of cutin and dandruff. A large amount of dandruff blocks hair follicles, leading to oil accumulation, and this situation in turn promotes the proliferation of Malassezia, forming a vicious cycle. Therefore, adjusting any balance back to the normal level helps control sebum secretion.

[0003] In addition, sebum secretion is also related to androgen levels. Testosterone is an important androgen in the human body. Under the catalysis of 5α-reductase, it is irreversibly converted into dihydrotestosterone (DHT). Usually, only less than 10% of testosterone is converted. Dihydrotestosterone has higher biological activity and specifically binds to androgen receptors to form a complex. After entering the cell nucleus, it binds to nuclear chromatin to produce physiological effects, and then is reduced by dehydrogenase to 3α-androstanediol, which combines with glucuronic acid to form androstanediol glucuronide and is excreted from the body with urine produced by metabolism. The levels of testosterone and dihydrotestosterone in the human body are in a dynamic balance state. DHT plays a positive role in the appearance and maintenance of secondary sexual characteristics, and at the same time can inhibit hair follicle growth, causing hair follicle atrophy. An increase in its level will also lead to sebaceous gland hypertrophy and increased sebum secretion. Therefore, too high a content of dihydrotestosterone in the human body is likely to cause symptoms such as prostate hyperplasia, endocrine disorders, and hair loss. Inhibiting the activity of 5α-reductase can reduce the content level of dihydrotestosterone and decrease sebum secretion. Therefore, developing hair care products using raw materials that inhibit the activity of 5α-reductase has become a hot topic. In this era when hair loss is tending to be younger, oil-control and anti-hair loss products have become the most popular and concerned products among consumers.

[0004] At present, the oil-control hair care products on the market mainly remove the oil on the skin surface by adding chemical components with strong cleaning effects. However, excessive cleaning may cause water loss in the scalp, resulting in dryness and water shortage. This will prompt sebaceous gland cells to secrete more oil to protect the scalp, and instead fail to achieve the real oil-control effect. Moreover, chemical components have greater irritation to the scalp and are prone to cause inflammation.

[0005] With the gradual development of plant extraction technology, a variety of plant components have been applied to the washing and chemical industry. The extracts of natural plants are rich in various active ingredients, with multiple effects such as reducing oil accumulation, antibacterial and anti-inflammatory, and repairing the scalp barrier. Moreover, they have lower irritation than chemically synthesized components, are milder in action and more secure, and are more environmentally friendly. Currently, the commonly used methods for plant extraction include solvent extraction method, ultrasonic extraction method, enzyme extraction method, microwave-assisted extraction method, and supercritical fluid extraction method. Among them, the microwave-assisted extraction method and the supercritical fluid extraction method are being widely used as new extraction technologies.

[0006] For example, in the prior art 1: Chinese Patent No. 202110158512.0 discloses a composition, preparation and its preparation method for improving hair loss and promoting hair growth in humans. The composition includes the following components: biotin tripeptide-1 0.05-1 part, myristoyl pentapeptide-17 0.051 part, Ligustrum lucidum extract 0.01-1 part, Eclipta prostrata extract 0.01-1 part, Dictamnus dasycarpus extract 0.01-1 part, Sophora flavescens extract 0.01-1 part, Morus alba root bark extract 0.01-1 part, Platycladus orientalis extract 0.01-1 part, Polygonum multiflorum extract 0.01-1 part, Angelica sinensis extract 0.01-1 part, Aquilaria sinensis extract 0.01-1 part, Nigella sativa extract 0.01-1 part, and Lippia alba extract 0.01-1 part. This composition is a traditional Chinese medicine compound and a biological polypeptide composition, which can improve hair loss and promote hair to become black and thick, and can be used in anti-hair loss and hair growth products, including shampoos, conditioners, hair care essential oils, hair masks, eyebrow and eyelash growth liquids, etc.

[0007] The prior art 1 uses raw materials such as biotin tripeptide-1 and myristoyl pentapeptide-17 that can inhibit the activity of 5α-reductase as components of the composition for improving hair loss and promoting hair growth in humans, so as to achieve the purpose of inhibiting the activity of 5α-reductase. This shows that it is feasible to use raw materials that inhibit the activity of 5α-reductase to form an oil-control and anti-hair loss composition. However, it is not enough to have only one composition that inhibits the activity of 5α-reductase for washing and chemical daily necessities. In order to meet the diverse needs of the market, more oil-control compositions need to be developed to meet the needs of consumers.

[0008] Therefore, the technical problem to be solved by the present invention is: how to develop an oil-control composition that can inhibit the activity of 5α-reductase and meet the diverse needs of the market. Summary of the Invention

[0009] One of the objectives of the present invention is to provide a nano-encapsulated oil-control composition, which uses ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract as active ingredients to synergistically promote blood circulation in the scalp, control oil secretion, and inhibit the growth of microorganisms, and can simultaneously regulate the balance of the microbial community, oil secretion balance, and metabolic balance in the scalp environment, thereby improving the inhibitory effect on 5α-reductase activity.

[0010] Another objective of the present invention is to provide a preparation method of a nano-encapsulated oil-control composition, which obtains a stable oil-control composition by encapsulating the ginger root extract, avoiding the oxidation and decomposition of the ginger root extract in a high-temperature environment, and at the same time improving the solubility of the essential oil in the composition and avoiding loss.

[0011] Meanwhile, the present invention also provides a use of a nano-encapsulated oil-control composition, and the nano-encapsulated oil-control composition is used to prepare daily chemical products, and the prepared daily chemical products have excellent inhibitory efficacy on 5α-reductase activity and significant oil-control effect.

[0012] To achieve the above objectives, the present invention provides a nano-encapsulated oil-control composition. By weight percentage, the nano-encapsulated oil-control composition comprises the following components: 2%-6% of ginger root extract, 2%-6% of calendula extract, 10%-20% of Platycladus orientalis leaf extract, 1%-3% of niacinamide, 0.2%-0.7% of adenosine, 5%-10% of emulsifier, 0%-35% of co-emulsifier, 0.1%-3% of preservative, and the balance is water.

[0013] The ginger root extract is an essential oil extracted from ginger. Ginger has the effects of dissipating stasis, dredging meridians, and promoting blood circulation. Appropriate use of the ginger root extract can help enhance the moisture of the hair and improve the dry hair condition.

[0014] The Platycladus orientalis leaf extract can promote local vasodilation of the scalp, increase blood circulation, and improve cell nutrients to achieve the purpose of stimulating hair follicle growth; at the same time, it is rich in tannins, volatile oils, etc., and topical application can inhibit the growth of bacteria and play an anti-inflammatory and anti-dandruff role.

[0015] When niacinamide acts on the scalp, it can produce the following effects:

[0016] 1. Improve dandruff: Niacinamide can inhibit the oil secretion of the scalp and reduce the generation of dandruff.

[0017] 2. Repair hair quality: Niacinamide can combine with caffeine and panthenol to thicken hair strands, strengthen hair filaments, and play a role in promoting hair growth. It can also improve the anti-breakage tensile ability of hair strands and enhance the anti-torsion performance of hair.

[0018] 3. Improve scalp dryness: Niacinamide can promote blood circulation in the scalp, increase the oxygen supply to the scalp, and thus improve the problem of scalp dryness.

[0019] 4. Improve hair quality: Niacinamide can improve the dry and frizzy conditions of hair and can also assist in improving the frizzy situation of hair.

[0020] 5. Promote hair growth: Niacinamide can stimulate the proliferation of follicular cells, promote hair growth, and at the same time can regulate the secretion of sebaceous glands to keep the scalp moist.

[0021] Adenosine promotes hair growth by activating the vitality of hair cells; adenosine also has a certain anti-dandruff effect, can clean the scalp, and reduce the generation of dandruff.

[0022] Calendula officinalis extract has the following hair care effects:

[0023] 1. Soothe scalp itching: Calendula officinalis extract has the effect of soothing scalp itching and is especially suitable for people with dry, sensitive scalps and dandruff problems.

[0024] 2. Nourish hair strands: Calendula officinalis extract can nourish hair strands, reduce hair breakage and fragility, and make hair healthier and more shiny.

[0025] 3. Antioxidation: Calendula officinalis extract is rich in various antioxidants and can help hair resist the effects of pollution, ultraviolet rays, and other daily stresses.

[0026] 4. Anti-inflammation: Calendula officinalis extract can inhibit inflammation and keep the scalp and hair strands in a healthy state.

[0027] The present invention uses a compound of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and Calendula officinalis extract in a synergistic manner. While promoting blood circulation, controlling oil secretion, and inhibiting the growth of microorganisms, it regulates the balance of the flora, oil secretion, and metabolism in the scalp environment, thereby synergistically improving the inhibitory effect on 5α-reductase activity; among them, Platycladus orientalis leaf extract, ginger root extract, and niacinamide promote blood circulation from three directions: promoting local blood vessel dilation in the scalp, promoting the blood circulation speed by activating blood circulation, and increasing the oxygen supply to the scalp, and combined with the effects of adenosine and niacinamide in cleaning the scalp and regulating the secretion of sebaceous glands, effectively maintain the scalp environment. Then, through the soothing and anti-inflammatory effects of Calendula officinalis extract, it effectively inhibits the growth of bacteria, comprehensively regulates the balance of the scalp environment, and synergistically improves the oil control effect of the composition.

[0028] Preferably, the emulsifier includes at least one of Tween 80, Span 80, PEG-40 hydrogenated castor oil, polyglyceryl-10 myristate, and polyglyceryl-10 laurate.

[0029] Preferably, the co-emulsifier is at least one of glycerol, 1,3-butanediol, propylene glycol, and hexylene glycol.

[0030] Preferably, the co-emulsifier is at least one of p-hydroxyacetophenone, hexylene glycol, octanoyl hydroxamic acid, ethylhexylglycerin, phenoxyethanol, and sodium benzoate

[0031] The present invention also discloses a preparation method of a nano-encapsulated oil-control composition, comprising the following steps:

[0032] Step 1: Add the Platycladus orientalis extract, niacinamide, adenosine, calendula extract, co-emulsifier, preservative, and water into a reaction kettle, disperse evenly, and then heat to 75-85 °C until completely dissolved and transparent;

[0033] Step 2: Mix the ginger root extract and the emulsifier evenly, then add them to the reaction kettle in Step 1, disperse evenly, and then keep warm and homogenize for 8-15 min;

[0034] Step 3: Cool down, and filter to obtain a mixture when cooled to 40-45 °C;

[0035] Step 4: Homogenize the mixture under a pressure of 200-300 bar to obtain a nano-encapsulated oil-control composition.

[0036] Furthermore, the number of homogenization treatments in Step 4 is 2-4 times, and the homogenization time for each homogenization treatment is 10-30 min.

[0037] The present invention also discloses the use of a nano-encapsulated oil-control composition for preparing daily chemical products.

[0038] Beneficial effects

[0039] Compared with the prior art, the present invention has at least the following advantages:

[0040] (1) The present invention discloses a nano-encapsulated oil-control composition. Through the compound synergism of ginger root extract, Platycladus orientalis extract, niacinamide, adenosine, and calendula extract, the oil-control effect of the composition can be effectively improved, and the inhibitory effect of the composition on 5α-reductase is significant;

[0041] (2) The present invention discloses a preparation method of a nano-encapsulated oil-control composition. By encapsulating the ginger root extract, a stable oil-control composition is obtained, which avoids the oxidation and decomposition of the ginger root extract in a high-temperature environment, and at the same time improves the solubility of the essential oil in the composition and avoids loss;

[0042] (3) The present invention discloses the use of a nano-encapsulated oil-control composition. When applied to the preparation of daily chemical products for the scalp, it can comprehensively regulate the scalp environment, regulate the balance of the flora, oil secretion, and metabolism in the scalp environment, and at the same time has little irritation to the scalp, and is safe and mild. Brief Description of the Drawings

[0043] The present invention will be further described below in conjunction with the drawings and embodiments;

[0044] Figure 1 Observation diagram of chicken embryo before using the nano-encapsulated oil-control composition of Example 3 of the present invention;

[0045] Figure 2 Observation diagram of chicken embryo after using the nano-encapsulated oil-control composition of Example 3 of the present invention;

[0046] Figure 3 Particle size test result diagram of Example 3;

[0047] Figure 4 Schematic diagram of hair frizziness before using Example 3 in the nourishing efficacy test;

[0048] Figure 5 Schematic diagram of hair frizziness after using Example 3 in the nourishing efficacy test. Detailed Description of the Invention

[0049] The present invention will be further described below in conjunction with the embodiments, but it does not constitute any limitation to the present invention. Any limited modifications made within the scope of the claims of the present invention are still within the scope of the claims of the present invention.

[0050] In order to elaborate on the technical content of the present invention, the following further explanations are made in conjunction with the embodiments.

[0051] In the following examples and comparative examples, the ginger extract (ginger was purchased from the Australian company FICCECODE AUSTRALIA PTY LTD), the Platycladus orientalis leaf extract was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., nicotinamide was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., adenosine was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., calendula extract was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., PEG-40 hydrogenated castor oil was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., Tween 80 was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., Span 80 was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., polygonum multiflorum extract was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., ligusticum wallichii extract was purchased from Lanzhou Wateles Biotechnology Co., Ltd., betaine was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., colophony was purchased from Hubei Jianchu Biomedicine Co., Ltd., safflower extract was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., ginseng extract was purchased from Guangzhou Hemiao Biotechnology Co., Ltd., 1,2-Hexanediol and p-Hydroxyacetophenone were purchased from Guangzhou Hemiao Biotechnology Co., Ltd.

[0052] It should be noted that the technical solution of the present invention can be realized by other commercially available products, and is not limited to the raw material sources adopted above.

[0053] Unless otherwise specified, the percentages mentioned in the following examples and comparative examples are all weight percentages.

[0054] In the following examples and comparative examples, the compositions were all prepared by the following preparation method:

[0055] Step 1: Add Platycladus orientalis leaf extract or Polygonum multiflorum extract or Ligusticum chuanxiong extract, niacinamide or betaine, adenosine or cobiproxamol, Calendula officinalis extract or Carthamus tinctorius extract or Panax ginseng extract, glycerol, 1,2 - hexanediol, p - hydroxyacetophenone and water into a reaction kettle, disperse evenly and then heat to 80 °C until dissolved completely transparent;

[0056] Step 2: Mix ginger root extract and PEG - 40 hydrogenated castor oil evenly, then add them into the reaction kettle in Step 1 and disperse evenly, then keep warm and homogenize for 12 min;

[0057] Step 3: Cool down the temperature. When it is cooled to 45 °C, filter to obtain a mixture;

[0058] Step 4: Homogenize the mixture 4 times under the pressure of 200 bar, and the homogenization time for each time is 20 min to obtain the composition.

[0059] Example 1

[0060] A nano - encapsulated oil - control composition, comprising 5% ginger root extract, 12% Platycladus orientalis leaf extract, 1% niacinamide, 0.4% adenosine, 5% Calendula officinalis extract, 6% PEG - 40 hydrogenated castor oil, 13% glycerol, 0.8% 1,2 - hexanediol, 0.5% p - hydroxyacetophenone, 56.3% water.

[0061] Example 2

[0062] A nano - encapsulated oil - control composition, comprising 2% ginger root extract, 20% Platycladus orientalis leaf extract, 2% niacinamide, 0.5% adenosine, 15% Calendula officinalis extract, 5.5% PEG - 40 hydrogenated castor oil, 27% glycerol, 0.8% 1,2 - hexanediol, 0.5% p - hydroxyacetophenone, 26.7% water.

[0063] Example 3

[0064] A nano - encapsulated oil - control composition, comprising 5% ginger root extract, 15% Platycladus orientalis leaf extract, 2% niacinamide, 0.5% adenosine, 5% Calendula officinalis extract, 10% PEG - 40 hydrogenated castor oil, 33% glycerol, 0.8% 1,2 - hexanediol, 0.5% p - hydroxyacetophenone, 28.2% water.

[0065] Comparative Example 1

[0066] Substantially the same as Example 3, except that an oil-control composition includes 18% Platycladus orientalis leaf extract, 2% niacinamide, 0.6% adenosine, 6.9% calendula extract, 30% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 41.2% water; and the preparation method of the oil-control composition is as follows: Step 1: Add Platycladus orientalis leaf extract, niacinamide, adenosine, calendula extract, glycerol, hexylene glycol, p-hydroxyacetophenone, and water into a reaction kettle, disperse evenly, and then heat to 80°C until dissolved completely transparent;

[0067] Step 2: Lower the temperature. When cooled to 45°C, filter to obtain a mixture;

[0068] Step 3: Homogenize the mixture 4 times under a pressure of 200 bar, with each homogenization time being 20 min to obtain the composition.

[0069] Comparative Example 2

[0070] Substantially the same as Example 3, except that an oil-control composition includes 12% ginger root extract, 2% niacinamide, 1.1% adenosine, 12.4% calendula extract, 15% PEG-40 hydrogenated castor oil, 20% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 36.2% water.

[0071] Comparative Example 3

[0072] Substantially the same as Example 3, except that an oil-control composition includes 5.1% ginger root extract, 16.5% Platycladus orientalis leaf extract, 0.6% adenosine, 5.3% calendula extract, 6.13% PEG-40 hydrogenated castor oil, 20% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 45.07% water.

[0073] Comparative Example 4

[0074] Substantially the same as Example 3, except that an oil-control composition includes 5.1% ginger root extract, 15.3% Platycladus orientalis leaf extract, 2% niacinamide, 5.1% calendula extract, 7.6% PEG-40 hydrogenated castor oil, 11% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 52.6% water.

[0075] Comparative Example 5

[0076] Substantially the same as Example 3, except that an oil-control composition includes 6.9% ginger root extract, 18% Platycladus orientalis leaf extract, 2% niacinamide, 0.6% adenosine, 8.42% PEG-40 hydrogenated castor oil, 25% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 37.78% water.

[0077] Comparative Example 6

[0078] It is generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% fleece-flower root extract, 2% niacinamide, 0.5% adenosine, 5% calendula extract, 10% PEG-40 hydrogenated castor oil, 33% glycerin, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0079] Comparative Example 7

[0080] It is generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% chuanxiong rhizome extract, 2% niacinamide, 0.5% adenosine, 5% calendula extract, 10% PEG-40 hydrogenated castor oil, 33% glycerin, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0081] Comparative Example 8

[0082] It is generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% oriental arborvitae leaf extract, 2% betaine, 0.5% adenosine, 5% calendula extract, 10% PEG-40 hydrogenated castor oil, 33% glycerin, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0083] Comparative Example 9

[0084] It is generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% oriental arborvitae leaf extract, 2% niacinamide, 0.5% colchicine, 5% calendula extract, 10% PEG-40 hydrogenated castor oil, 33% glycerin, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0085] Comparative Example 10

[0086] It is generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% oriental arborvitae leaf extract, 2% niacinamide, 0.5% adenosine, 5% safflower extract, 10% PEG-40 hydrogenated castor oil, 33% glycerin, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0087] Comparative Example 11

[0088] Generally the same as Example 3, except that a nano-encapsulated oil-control composition includes 5% ginger root extract, 15% biota orientalis leaf extract, 2% niacinamide, 0.5% adenosine, 5% ginseng extract, 10% PEG-40 hydrogenated castor oil, 33% glycerol, 0.8% hexylene glycol, 0.5% p-hydroxyacetophenone, and 28.2% water.

[0089] Efficacy Test

[0090] 1. Irritation Test

[0091] 1.1 Instrument and Equipment

[0092] Fully automatic incubator, stereomicroscope, SPF chicken embryos;

[0093] 1.2 Reagents

[0094] Sodium chloride, sodium dodecyl sulfate (SDS);

[0095] 1.3 Incubation Conditions

[0096] Room temperature: 20°C - 25°C, relative humidity: 45% - 70%, incubation temperature: 37.5°C ± 0.5°C, relative humidity: 55% - 70%, turntable rotation: 3 times / h - 6 times / h. Chicken embryos at 9 days of age do not need to be rotated during incubation.

[0097] 1.4 Test Method

[0098] (1) Test Operation Steps

[0099] For this test, 6 embryos are selected for each group. The situation of the chorioallantoic membrane is recorded with a photographing device. A polytetrafluoroethylene resin ring is placed on the chorioallantoic membrane of the chicken embryo and photographed. The compositions prepared in Examples 1 - 3 and Comparative Examples 1 - 11 are respectively diluted with pure water to a solution with a composition mass fraction of 1% as the test samples. Subsequently, the test samples are added into the polytetrafluoroethylene resin ring, the time of adding the samples is recorded, and the air chamber is covered with a wet plastic wrap. The chicken embryos are transferred to a constant temperature and humidity incubator for cultivation, and the degree of change in each toxic effect is observed.

[0100] (2) Result Observation

[0101] Observe and record the manifestations of bleeding, blood coagulation, and vascular lysis, and score according to their severity

[0102] The scoring criteria for bleeding, blood coagulation, and vascular lysis are shown in Table 1:

[0103] Table 1

[0104]

[0105]

[0106] Scoring criteria: ES ≤ 12: no / mild irritation; 12 < ES < 16: moderate irritation; ES ≥ 16: strong irritation.

[0107] The compositions prepared in Examples 1 - 3 and Comparative Examples 1 - 11 were subjected to irritation tests according to the above method, and the results were all ES ≤ 4, indicating no irritation.

[0108] Among them, the ES of the negative control (0.9% normal saline) was 0.00, meeting the standard of the negative control sample; the ES of the positive control (1% SDS) was 18.00, meeting the standard of the positive control sample; the ES of Example 3 was 3.67. The pre - use chicken embryo diagram of Example 3 is shown in Figure 1 , and the post - use chicken embryo diagram of Example 3 is shown in Figure 2 .

[0109] 2. Particle size test

[0110] 2.1 Instrument and equipment

[0111] Winner802 photon - correlation nanoparticle size analyzer

[0112] 2.2 Test method

[0113] The sample is directly transported into the sample cell for testing; for opaque samples, dilution treatment is required (common dilution media include ethanol, water, isopropanol, glycerol, etc.) to ensure that the particles are evenly and representatively transported into the sample cell. Open the upper cover of the instrument and place the sample cell to be tested into it; fill in the test information of the sample to be measured, and select the name of the dispersion medium, refractive index, viscosity, and test temperature used; after placing the sample cell to be tested into the instrument, wait for 1 - 2 minutes to allow the sample to be in a completely static state and the sample temperature to reach the test temperature, and then enter the sample testing stage.

[0114] 2.3 Test results

[0115] The nano - encapsulated oil - controlling composition prepared in Example 3 was tested according to the above method, and the results are shown in Table 2 and Figure 3 as follows;

[0116] Table 2 Particle size results of the nano - encapsulated oil - controlling composition prepared in Example 3

[0117]

[0118] According to the results in Table 2, it can be seen that the average particle size of the nano - encapsulated oil - controlling composition prepared in Example 3 is 65.89 nm, indicating its good stability.

[0119] 3. Oil - controlling efficacy test

[0120] (1) Inhibition rate of intracellular lipid content in human sebaceous gland cells

[0121] Treatment and reagents for experimental groups

[0122] Samples: The compositions prepared in Examples 1-3 and Comparative Examples 1-11 were diluted with cell culture medium to a concentration of 0.08%.

[0123] Positive control: Isotretinoin

[0124] Negative control: Cell culture medium

[0125] Reagents: 0.25% Trypsin, cell culture medium, PBS buffer, 4% Paraformaldehyde, Oil Red O staining kit, Isopropanol, Isotretinoin

[0126] Experimental procedures

[0127] Determination of intracellular lipid content

[0128] Oil Red O staining: 3×10 SZ95 cells cultured to the exponential growth phase in DMEM medium containing 10% FBS and 1% double antibodies were inoculated into 96-well plates at 4 / well, and after 24 h of culture, samples or solvents with different mass fractions were added respectively, and incubation was continued at 37 °C for 24 h. Discard the DMEM medium, add 200 μL of 4% paraformaldehyde solution, fix at room temperature for 30 min, discard the excess solution, then add 0.5% Oil Red O solution, and stain at room temperature for 15 min. Determination of intracellular lipid content: Discard the excess staining solution, wash gently with PBS 2 times, discard the PBS in the 96-well plate, air dry at room temperature, add 150 μL of 100% isopropanol to completely dissolve the Oil Red O, then aspirate the dissolved Oil Red O into the 96-well plate, 50 μL / well, and set two replicates for each sample. Place it in an enzyme-linked immunosorbent assay (ELISA) reader to detect the absorbance value (A) at 490 nm. The inhibition rate of intracellular lipid content after drug intervention was calculated using the following formula with the A value:

[0129]

[0130] Data analysis

[0131] The statistical analysis software was SPSS, and an independent samples t-test was used to compare the inhibition rates of intracellular lipid content among the test samples, positive control substances, and negative control substances. The above statistical analyses were all two-tailed tests, and the significance level was a = 0.05. P≥0.05 indicates no significant difference between the two groups; P<0.05 indicates a significant difference between the two groups.

[0132] Result determination criteria

[0133] The test sample has a significant effect on inhibiting intracellular lipid content (P<0.05), that is, the test sample has an obvious ability to inhibit intracellular lipid content, indicating that the test sample has a certain oil control effect.

[0134] The results are shown in Table 3;

[0135] Table 3 Test results of the oil control efficacy of the compositions prepared in Examples 1-3 and Comparative Examples 1-11

[0136] Lipid content inhibition rate (%) P value Example 1 5.198 <0.05 Example 2 5.243 <0.05 Example 3 6.582 <0.05 Comparative Example 1 2.910 <0.05 Comparative Example 2 2.724 <0.05 Comparative Example 3 3.187 <0.05 Comparative Example 4 3.124 <0.05 Comparative Example 5 2.961 <0.05 Comparative Example 6 3.249 <0.05 Comparative Example 7 2.597 <0.05 Comparative Example 8 3.213 <0.05 Comparative Example 9 2.775 <0.05 Comparative Example 10 3.954 <0.05 Comparative Example 11 3.698 <0.05 Positive control 23.527 <0.05 Negative control / /

[0137] It can be seen from the results in Table 3 that:

[0138] From the comparison of the lipid content inhibition rate data of Example 3 and Comparative Examples 1-5, it can be seen that compared with Example 1, in the case of lacking any one of Zingiber officinale root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and Calendula officinalis flower extract in Comparative Examples 1-5, although the dosage of other components increased correspondingly, the lipid content inhibition rate shown was significantly decreased. This shows that the combination of Zingiber officinale root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and Calendula officinalis flower extract in the present invention has a synergistic effect and can synergistically inhibit the activity of human sebaceous gland cells.

[0139] From the comparison of the lipid content inhibition rate data of Example 3 and Comparative Examples 6 and 7, it can be seen that using Polygonum multiflorum Thunb. extract and Ligusticum chuanxiong Hort. extract with similar effects to replace Platycladus orientalis leaf extract cannot produce a synergistic effect of inhibiting lipid production in human sebaceous gland cells with Zingiber officinale root extract, niacinamide, adenosine, and Calendula officinalis flower extract. Since the inhibitory effect of Polygonum multiflorum Thunb. extract on the activity of human sebaceous gland cells is greater than that of Platycladus orientalis leaf extract and Ligusticum chuanxiong Hort. extract, the lipid content inhibition rate of Comparative Example 6 is correspondingly higher than that of Comparative Example 7, further verifying that the combination of Polygonum multiflorum Thunb. extract and Ligusticum chuanxiong Hort. extract with Zingiber officinale root extract, niacinamide, adenosine, and Calendula officinalis flower extract only produces a simple additive effect of efficacy and does not produce a synergistic effect.

[0140] From the comparison of the lipid content inhibition rate data of Example 3 and Comparative Example 8, it can be seen that the technical solution using betaine, which has a similar effect to niacinamide, to replace niacinamide shows a significant decrease in the lipid content inhibition rate. This shows that the combination of Zingiber officinale root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and Calendula officinalis flower extract in the present invention has a synergistic effect and can synergistically inhibit the synthesis of lipids in human sebaceous gland cells; while betaine only produces a simple additive effect of efficacy with Zingiber officinale root extract, Platycladus orientalis leaf extract, adenosine, and Calendula officinalis flower extract, etc.

[0141] From the comparison of the lipid content inhibition rate data of Example 3 and Comparative Example 9, it can be seen that the technical solution of replacing adenosine with comparablecide, which has a similar effect to adenosine, shows a significant decrease in the lipid content inhibition rate. This indicates that the combination of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in the present invention produces a synergistic effect and has a synergistic effect on inhibiting lipid production in human sebaceous gland cells; while comparablecide only produces a simple additive effect with ginger root extract, Platycladus orientalis leaf extract, niacinamide, calendula extract, etc.

[0142] From the comparison of the lipid content inhibition rate data of Example 3 and Comparative Examples 10 and 11, it can be seen that using safflower extract and ginseng extract with similar effects to replace calendula extract cannot produce a synergistic effect on inhibiting human sebaceous gland cells with ginger root extract, Platycladus orientalis leaf extract, niacinamide, and adenosine. Since the inhibitory effect of safflower extract itself on the activity of human sebaceous gland cells is greater than that of calendula extract and ginseng extract, the lipid content inhibition rate of Comparative Example 10 is correspondingly higher than that of Comparative Example 11, further verifying that the combination of safflower extract and ginseng extract with ginger root extract, Platycladus orientalis leaf extract, niacinamide, and adenosine only produces a simple additive effect of efficacy and does not produce a synergistic effect.

[0143] (2) 5α - reductase inhibition rate test

[0144] Treatment and reagents for each test group

[0145] Samples: The compositions prepared in Examples 1 - 3 and Comparative Examples 1 - 11 diluted to a concentration of 5% with Tris - HCl buffer.

[0146] Positive control: Finasteride

[0147] Negative control: Tris - HCl buffer

[0148] Reagents: Testosterone, reduced coenzyme II - tetrasodium salt, 1M Tris - HCl buffer, methanol, ethanol, finasteride

[0149] Test steps

[0150] 1. Extraction of 5α - reductase crude enzyme

[0151] Prepare crushed ice in advance and pre-cool the homogenization equipment in advance. Take 10 male SD rats, decapitate them after fasting for 24 hours without water deprivation, take out the prostate or epididymis and weigh them. Place the tissues in the homogenization equipment and make a 1:5 homogenate (g / mL) with pre-cooled PBS in a glass homogenizer. After thorough grinding, aliquot it into centrifuge tubes and centrifuge at 4°C and 10,000 rpm for 30 minutes to remove the floating fat. Take the supernatant as the crude extract. Make the volume up to 10 - 20 mL, aliquot and store it in 1.5 mL centrifuge tubes. It can be stored at -80°C for 3 months.

[0152] 2. Protein content determination

[0153] Determine by BCA protein quantification kit or Coomassie Brilliant Blue method.

[0154] 3. 5α - reductase inhibition rate test

[0155] Set up four groups: sample group, finasteride group, complete reaction group and control group.

[0156] Sample group: Add 0.25 mL of Tris-HCl, 0.7 mL of enzyme extract, 0.6 mL of sample solution, 0.1 mL of testosterone solution and 0.35 mL of NADPH. React the test tube at 37°C for 30 minutes. After the reaction is completed, add 2 mL of dichloromethane to stop the reaction. Shake for 1 minute and then centrifuge at 3000 r / min for 10 minutes. Remove the upper aqueous phase and take 1 mL of the lower organic phase (in the "dichloromethane - water" system, the white gel-like layer will separate the two phases in the middle). Evaporate the organic phase to dryness, and there will be a white powdery residue dissolved in 1 mL of methanol.

[0157] Complete reaction group: Add 0.25 mL of Tris-HCl, 0.7 mL of enzyme extract, 0.6 mL of 10% ethanol solution, 0.1 mL of testosterone solution and 0.35 mL of NADPH. React the test tube at 37°C for 30 minutes. After the reaction is completed, add 2 mL of dichloromethane to stop the reaction. Shake for 1 minute and then centrifuge at 3000 r / min for 10 minutes. Remove the upper aqueous phase and take 1 mL of the lower organic phase. Evaporate the organic phase to dryness, and there will be a white powdery residue dissolved in 1 mL of methanol.

[0158] Negative group: Add 0.25 mL of Tris-HCl, 0.7 mL of enzyme extract, 0.6 mL of Tris-HCl solution, 0.1 mL of testosterone solution and 0.35 mL of NADPH. Directly add 2 mL of dichloromethane to stop the reaction. Shake for 1 minute and then centrifuge at 3000 r / min for 10 minutes.

[0159] Finasteride (positive) group: Add 0.25 mL of Tris-HCl, 0.7 mL of enzyme extract, 0.6 mL of finasteride solution, 0.1 mL of testosterone solution, and 0.35 mL of NADPH. React the test tube at 37 °C for 30 min. After the reaction, add 2 mL of dichloromethane to stop the reaction. Shake for 1 min and then centrifuge at 3000 r / min for 10 min. Remove the upper aqueous phase, take 1 mL of the lower organic phase, evaporate the organic phase to dryness, and dissolve the white powdery residue in 1 mL of methanol.

[0160] Remove the upper aqueous phase, take 1 mL of the lower organic phase, evaporate the organic phase to dryness, and dissolve the white powdery residue in 1 mL of methanol. Perform HPLC analysis on each group under the following conditions: C18 (250 mm × 4.6 mm, 5 μm), column temperature 40 °C, mobile phase methanol:water = 70:30 (v / v), flow rate 1 mL / min, photodiode array detector, detection wavelength 242 nm.

[0161] Result calculation

[0162] Testosterone standard curve: Perform HPLC analysis on different concentrations of testosterone standard solutions respectively. Take the concentration (X) as the abscissa and the peak area (Y) as the ordinate to make the standard curve.

[0163] Under the above chromatographic conditions, determine the content of testosterone in the reaction solution. The strength of the inhibitory activity is characterized by the inhibition rate, as shown in the following formula:

[0164]

[0165] Result determination criteria

[0166] The inhibition rate of 5α-reductase in the positive control > 50%, and the reaction system is effective. When the inhibition rate of 5α-reductase in the sample dilution is significantly different from that of the negative control (P < 0.05), it indicates that the sample has a certain oil control effect.

[0167] Test the compositions prepared in Examples 1-3 and Comparative Examples 1-11 according to the above method, and the results are shown in Table 4;

[0168] Table 4 Results of the inhibition rate of 5α-reductase of the compositions prepared in Examples 1-3 and Comparative Examples 1-11

[0169]

[0170]

[0171] According to the results in Table 4, it can be seen that:

[0172] From the comparison of the 5α-reductase inhibition rate data of Example 3 and Comparative Examples 1-5, it can be seen that compared with Example 1, in the case of lacking any one of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in Comparative Examples 1-5, although the dosages of other components increased correspondingly, the 5α-reductase inhibition rate showed a significant decrease. This shows that the combination of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in the present invention has a synergistic effect and can synergistically inhibit the activity of 5α-reductase.

[0173] From the comparison of the 5α-reductase inhibition rate data of Example 3 and Comparative Examples 6 and 7, it can be seen that using polygonum multiflorum extract and chuanxiong rhizome extract with similar efficacy to replace Platycladus orientalis leaf extract cannot produce a synergistic effect of inhibiting the activity of 5α-reductase with ginger root extract, niacinamide, adenosine, and calendula extract. Since the inhibitory effect of polygonum multiflorum extract itself on 5α-reductase is greater than that of Platycladus orientalis leaf extract and chuanxiong rhizome extract, the 5α-reductase inhibition rate of Comparative Example 6 is correspondingly higher than that of Comparative Example 7, further verifying that the combination of polygonum multiflorum extract and chuanxiong rhizome extract with ginger root extract, niacinamide, adenosine, and calendula extract only produces a simple additive effect of efficacy and does not produce a synergistic effect.

[0174] From the comparison of the 5α-reductase inhibition rate data of Example 3 and Comparative Example 8, it can be seen that the technical solution of using betaine similar to niacinamide to replace niacinamide shows a significant decrease in the 5α-reductase inhibition rate, indicating that the combination of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in the present invention has a synergistic effect and can synergistically inhibit the activity of 5α-reductase; while betaine only produces a simple additive effect of efficacy with ginger root extract, Platycladus orientalis leaf extract, adenosine, calendula extract, etc.

[0175] From the comparison of the 5α-reductase inhibition rate data of Example 3 and Comparative Example 9, it can be seen that the technical solution of using coloprostenol similar to adenosine to replace adenosine shows a significant decrease in the 5α-reductase inhibition rate, indicating that the combination of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in the present invention has a synergistic effect and can synergistically inhibit the activity of 5α-reductase; while coloprostenol only produces a simple additive effect of efficacy with ginger root extract, Platycladus orientalis leaf extract, niacinamide, calendula extract, etc.

[0176] According to the comparison of the 5α-reductase inhibition rate data of Example 3, Comparative Example 10, and Comparative Example 11, it can be seen that replacing the calendula extract with safflower extract and ginseng extract with similar efficacy cannot produce a synergistic effect of inhibiting 5α-reductase activity with ginger root extract, Platycladus orientalis leaf extract, niacinamide, and adenosine. Since the inhibitory effect of safflower extract itself on 5α-reductase is greater than that of calendula extract and ginseng extract, the 5α-reductase inhibition rate of Comparative Example 10 is correspondingly higher than that of Comparative Example 11, further verifying that the compounding of safflower extract and ginseng extract with ginger root extract, Platycladus orientalis leaf extract, niacinamide, and adenosine only produces a simple additive effect of efficacy and does not produce a synergistic effect.

[0177] 4. Nourishing Efficacy Test

[0178] Treatment and Reagents for Test Groups

[0179] Samples: The nano-encapsulated oil-control compositions prepared in Examples 1 to 3 and Comparative Examples 1 to 11.

[0180] Reagents: 10% sodium dodecyl sulfate (K12) aqueous solution

[0181] Test Procedures

[0182] 1. Instrument Testing

[0183] Frizziness (proportion of small hair area) test: Select 5 bundles of healthy ex vivo human hair bundles, use VISIA7 to record the images of the hair bundles before and after using the samples, and use IPP to analyze the frizziness (proportion of small hair area) of the photos of the hair bundles before and after using the products.

[0184] Baseline Dry Hair Test

[0185] The hair bundles to be tested are fully wetted with flowing constant-temperature water (38 ± 1°C), and used evenly on the hair bundle surface at a dosage of 0.2 g of cleaning solution per gram of hair bundle for about 30 seconds, left standing for about 1 minute, and then rinsed for about 30 seconds. The hair bundles are placed in a constant-temperature and humidity chamber for more than 4 hours, taken out and fixed at the test position for frizziness testing.

[0186] Sample Dry Hair Test

[0187] The hair bundles to be tested are fully wetted with flowing constant-temperature water (38 ± 1°C), and used evenly on the hair bundle surface at a dosage of 0.2 g of the sample or in accordance with the usage method of the sample for about 30 seconds, left standing for about 1 minute, and then rinsed for about 30 seconds or rinsing is omitted. The hair bundles after the wet hair test are placed in a constant-temperature and humidity chamber for more than 4 hours, taken out and fixed at the test position for frizziness testing.

[0188] Data Analysis

[0189] Descriptive statistics were performed on the measurement parameters, including mean, standard deviation, median, etc. The values of the initial value / blank group of the measurement parameters and other measurement time points / other groups were calculated and analyzed using professional statistical software. If the data was normally distributed, t-tests or analysis of variance methods were used for data analysis and statistics; if the data was non-normally distributed, the rank sum test method was used for statistics. All statistical methods used two-tailed tests, and the significance level α = 0.05.

[0190] Result judgment criteria

[0191] Compared with the control group or before sample application, the hair frizziness after sample application was significantly reduced, indicating that the sample had the effect of improving hair frizziness.

[0192] The compositions prepared in Examples 1-3 and Comparative Examples 1-11 were tested according to the above method, and the results are shown in Table 5, where Figure 4 、 Figure 5 are schematic diagrams of hair frizziness before using Example 3 and after using Example 3, respectively;

[0193] Table 5 Test results of the nourishing effects of the compositions prepared in Examples 1-3 and Comparative Examples 1-11

[0194]

[0195]

[0196] According to the results in Table 5, it can be seen that:

[0197] Different from the oil control effect performances in Table 3 and Table 4, the nourishing effect performances of Examples 1-3 and Comparative Examples 1-11 were mostly based on the nourishing effects brought by the components. Although the synergistic effect shown by the technical solution of the present invention could still synergistically improve the nourishing effect of the composition to a certain extent, its synergistic effect was weaker than that of the oil control effect performance.

[0198] According to the data comparison of Example 3 and Comparative Examples 1-5, it can be seen that compared with Example 1, in the case of lacking any one of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in Comparative Examples 1-5, although the dosages of other components increased correspondingly, the change rate of hair frizziness also decreased to a certain extent; among them, Comparative Example 1 showed a significant decrease. The reason is that in the performance of the nourishing effect of the composition, ginger root extract plays the most important role; while the difference in the change rate of hair frizziness between Comparative Example 2 and Example 3 is relatively small. Since the dosages of ginger root extract, niacinamide, adenosine, and calendula extract in Comparative Example 2 increased correspondingly, especially the dosage of ginger root extract increased significantly, the change rate of hair frizziness in Comparative Example 2 also increased significantly and was close to that of Example 3, but it was still lower than that of Example 3. This shows that the combination of ginger root extract, Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract in Example 3 produced a synergistic effect in enhancing the hair nourishing effect of the composition, which has a better effect than the simple effect superposition of Comparative Examples 1-5.

[0199] And according to the data comparison of Example 3 and Comparative Examples 1-11, it can be seen that the technical solutions using other raw materials to replace Platycladus orientalis leaf extract, niacinamide, adenosine, and calendula extract respectively did not show a synergistic effect in enhancing the hair nourishing effect of the composition similar to the technical solution of the present invention.

[0200] Application Example

[0201] An oil-control shampoo, and the formulation ratio is shown in Table 6.

[0202] Table 6

[0203]

[0204]

[0205] The embodiments presented herein are only implementation manners selected according to combinations of all possible embodiments. The appended claims should not be limited by the embodiments illustrating the present invention. Some numerical ranges used in the claims include sub-ranges within them, and variations within these ranges should also be covered by the appended claims.

Claims

1. A nano-encapsulated oil control composition, characterized in that: The nano-encapsulated oil-control composition is composed of the following ingredients by weight percentage: 2%-6% ginger root extract, 2%-6% calendula extract, 10%-20% orientalis leaf extract, 1%-3% niacinamide, 0.2%-0.7% adenosine, 5%-10% emulsifier, 0%-35% co-emulsifier, 0.1-3% preservative, and the balance is water; The preservative is at least one of p-hydroxyacetophenone, hexylene glycol, ethylhexylglycerin, phenoxyethanol, and sodium benzoate; The nano-encapsulated oil control composition is prepared by the following steps: Step 1: Add Platycladus orientalis leaf extract, niacinamide, adenosine, calendula officinalis extract, emulsifier, preservative and water into a reaction pot, disperse evenly, heat to 75-85°C, and dissolve until completely transparent; Step 2: Mix the ginger root extract and the emulsifier evenly, then add them into the reaction pot in step 1 and disperse them evenly, then keep warm and homogenize for 8-15 minutes; Step 3: Cooling down to 40-45°C and filtering to obtain a mixture; Step 4: homogenize the mixture at a pressure of 200-300 bar to obtain a nano-encapsulated oil-control composition.

2. The nano-encapsulated oil control composition according to claim 1, characterized in that: The emulsifier includes at least one of Tween 80, Span 80, PEG-40 hydrogenated castor oil, polyglyceryl-10 myristate, and polyglyceryl-10 laurate.

3. The nano-encapsulated oil control composition according to claim 1, characterized in that: The auxiliary emulsifier is at least one of glycerol, 1,3-butylene glycol, propylene glycol and hexylene glycol.

4. The nano-encapsulated oil control composition according to claim 1, characterized in that: The homogenization process in step 4 is performed 2-4 times, and the homogenization time for each homogenization process is 10-30 minutes.

5. Use of the nano-encapsulated oil-control composition according to any one of claims 1 to 4 for preparing daily chemical products.

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