Abelmoschus manihot extract, preparation method thereof and application of abelmoschus manihot extract in hair care products

Abstract

The invention belongs to the technical field of hair care, and particularly relates to an abelmoschus manihot extract, a preparation method thereof and application of the abelmoschus manihot extract in hair care products. The abelmoschus manihot, the biological enzyme and the water are mixed for ultrasonic extraction, the obtained abelmoschus manihot crude extracting solution and the Sevage reagent are mixed for deproteinization and freeze drying, the obtained abelmoschus manihot extract contains rich active substances such as flavone, oligosaccharide and polysaccharide and is directly used as a hair care product raw material, an anti-dandruff agent and a humectant do not need to be additionally added, and the anti-dandruff effect is good. The anti-dandruff hair conditioner is free of heavy metal ions and organic aromatic ring components, the production process is safe and environmentally friendly, and the problems that a traditional hair conditioner needs to be added with an artificially synthesized anti-dandruff agent and a humectant, heavy metal salt and organic aromatic compounds are possibly introduced, scalp irritation and allergy are caused, and environmental pollution is likely to be caused are solved. In-vitro hair care experiments show that the abelmoschus manihot extract has the effects of preventing hair breakage, protecting hair, removing dandruff and the like, and can be widely applied to the field of hair care products as a new generation of natural plant environment-friendly hair care agents.

Description

Technical Field

[0001] The invention belongs to the technical field of hair care, and particularly relates to a hibiscus hibiscus extract and a preparation method thereof and application of the extract in hair care products. Background Art

[0002] The main component of hair is keratinized protein, and the remaining components are water, lipids, pigments and trace elements. The outer structure of hair is mainly composed of flat keratin cells arranged in fish scales, also known as hair scales. Hair scales can not only protect the hair core and resist damage to hair from ultraviolet rays, pollutants, etc., but also protect sebum, prevent water evaporation, and make hair soft and shiny. The hair scales of healthy hair are arranged neatly, smooth, and covered with oil on the surface, making the hair easy to comb. However, with the development of modern cities, behaviors such as hair dyeing and perming, as well as ultraviolet radiation, pollutant particles and other substances in the air can damage the hair scales, causing them to curl up and destroy the original arrangement structure, which in turn makes the hair lose its luster, feel rough, and difficult to comb. Finally, the hair becomes dry, easy to break, and even falls off.

[0003] Abelmoschus manihot (L.) Medicus is an annual or perennial herbaceous plant of the genus Abelmoschus in the Malvaceae family. Abelmoschus manihot contains rich plant polysaccharides and plant gums. Abelmoschus manihot extract has been used as a "paper medicine" in papermaking since the Han Dynasty. Paper treated with Abelmoschus manihot extract is easy to separate during papermaking because the surface is covered with a thin film and has smooth, lint-free and unbreakable properties.

[0004] Research on natural plant extract hair conditioners is a trend and hotspot in the current hair care industry. Chinese patent CN117562842A discloses a hair care composition containing Rosa centifolia flower extract, which is mixed with 0.5% to 20% Rosa centifolia flower extract and high-grade fatty alcohol, cationic conditioning agent, moisturizer, water and other components to obtain a hair conditioner that can protect against smog, smoke and ultraviolet rays. Chinese patent CN 107184418A discloses a pullulan hair conditioner, which is mixed with cationic conditioning agent, thickener, anti-dandruff agent, preservative and water to obtain a hair conditioner that can repair dry, split and easily broken hair and make hair smoother and glossier.

[0005] The above-mentioned hair care products are based on natural extracts. However, to achieve the effects of anti-dandruff, hair care, and anti-hair breakage, additional ingredients such as anti-dandruff agents and moisturizers need to be added. Common anti-dandruff agents are antibacterial drugs such as zinc pyrithione and oxiconazole, and common moisturizers are polyols, sodium hyaluronate, etc. These anti-dandruff agents and moisturizers are industrially synthesized components, which can also cause environmental pollution during the industrial synthesis process and do not conform to the current environmental protection trend. Moreover, these industrially synthesized components may cause skin irritation, allergies, and other problems. Summary of the Invention

[0006] In view of this, the purpose of the present invention is to provide an Abelmoschus manihot extract, its preparation method, and its application in hair care products. The present invention applies the Abelmoschus manihot extract to hair care. The Abelmoschus manihot extract is a natural extract, and at the same time has the effects of anti-dandruff, hair care, and anti-hair breakage, without the need to additionally add anti-dandruff agents and moisturizers, solving the problems that industrially synthesized components may cause skin irritation and allergies.

[0007] To achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0008] The present invention provides a preparation method of an Abelmoschus manihot extract, including the following steps:

[0009] Mix Abelmoschus manihot, biological enzyme, and water, and perform ultrasonic extraction to obtain an Abelmoschus manihot crude extract;

[0010] Mix the Abelmoschus manihot crude extract with Sevage reagent for protein removal treatment to obtain a purified solution;

[0011] Lyophilize the purified solution to obtain an Abelmoschus manihot extract.

[0012] Preferably, the biological enzyme includes one or more of cellulase, pectinase, and papain.

[0013] Preferably, the addition amount of the biological enzyme is 0-20% of the mass fraction of Abelmoschus manihot, and not 0.

[0014] Preferably, the temperature of the ultrasonic extraction is 30-60°C, and the time is 10-90 min.

[0015] Preferably, the dosage ratio of Abelmoschus manihot to water is 1 g:(5-30) mL.

[0016] Preferably, the ratio of the mass of Abelmoschus manihot to the volume of Sevage reagent is 1 g:(1-3) mL.

[0017] The present invention also provides an Abelmoschus manihot extract obtained by the preparation method described in the above technical solution, which comprises oligosaccharides, polysaccharides and flavonoids. The mass content of oligosaccharides in the Abelmoschus manihot extract is 0.5% - 3%, the mass content of polysaccharides is > 85%, and the mass content of flavonoids is 0.1% - 1%.

[0018] The present invention also provides the application of the Abelmoschus manihot extract described in the above technical solution in hair care products.

[0019] Preferably, the Abelmoschus manihot extract is used in the form of an aqueous solution of the Abelmoschus manihot extract, and the mass concentration of the Abelmoschus manihot extract in the aqueous solution of the Abelmoschus manihot extract is 1% - 5%.

[0020] The present invention also provides a hair care product, which comprises an Abelmoschus manihot extract, a preservative and water. The mass concentration of the Abelmoschus manihot extract in the hair care product is 1% - 5%.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The present invention provides a preparation method of an Abelmoschus manihot extract, which comprises the following steps: mixing Abelmoschus manihot, a biological enzyme and water for ultrasonic extraction to obtain a crude Abelmoschus manihot extract; mixing the crude Abelmoschus manihot extract and Sevage reagent for protein removal treatment to obtain a purified solution; freeze-drying the purified solution to obtain the Abelmoschus manihot extract.

[0023] The present invention uses a biological enzyme to destroy the cell wall tissue of Abelmoschus manihot and release plant secondary metabolites. The Abelmoschus manihot extract obtained with the assistance of ultrasonic waves contains rich active substances such as flavonoids, oligosaccharides and polysaccharides. As a natural antibacterial and fungicidal agent, flavonoids have a certain inhibitory effect on Malassezia that causes dandruff; while oligosaccharides, as non-ionic surfactants, can balance the oil of the scalp and hair, nourish the hair core and enhance the tensile strength of the hair; polysaccharides, as a natural moisturizer and macromolecular substance, can effectively lock the moisture of the hair and form a protective film to isolate the hair from the air, so as to reduce the damage to the hair caused by harmful substances in the environment. The hair treated with the Abelmoschus manihot extract shows the characteristics of being smooth, soft and non-fuzzy. The present invention directly uses the Abelmoschus manihot extract as a raw material for hair care products, without the need to additionally add anti-dandruff agents and moisturizers, and there are no heavy metal ions and organic aromatic ring components. The production process is safe and environmentally friendly, solving the disadvantages that traditional hair care agents need to add artificial synthetic anti-dandruff agents and moisturizers, which may introduce heavy metal salts and organic aromatic compounds to cause scalp irritation and allergies, as well as the problem of environmental pollution easily caused during the whole production process. In vitro hair care experiments show that the Abelmoschus manihot extract of the present invention has the effects of preventing hair breakage, hair care and anti-dandruff, and can be widely used in the hair care product field as a new generation of natural plant environmental protection hair care agent.

[0024] The present invention uses bioenzymes to prepare Abelmoschus manihot extract with the assistance of ultrasonic waves. Compared with the extraction of Abelmoschus manihot polysaccharide only using ultrasonic waves, the present invention adds bioenzymes to degrade the cellulose in the plant cell wall, thereby destroying the cell wall tissue of the roots of Abelmoschus manihot, promoting the release and dissolution of plant secondary metabolites, and improving the extraction efficiency. At the same time, the bioenzymes have a degradation effect on plant fibers and polysaccharides, generating oligosaccharides with a molecular weight of 1000 - 3000 Da (average molecular weight about 2000). Compared with macromolecular polysaccharides, oligosaccharides have a low molecular weight and a small molecular volume, and are more easily absorbed by hair. Therefore, oligosaccharides can quickly penetrate into the hair shaft, improve the internal structure of the hair, repair the split hair ends, and nourish the hair. In addition, compared with polysaccharides with a higher molecular weight, oligosaccharides do not form a thick film on the hair surface. While nourishing the hair core and enhancing the toughness of the hair, they can effectively improve the smoothness of the hair, making the hair easier to comb, more suitable for hair care, and enhancing the reprocessing and utilization value of the roots and rhizomes of Abelmoschus manihot. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required in the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0026] Figure 1 It is a comparison chart of the tensile strength and the work of rupture for Application Example 1;

[0027] Figure 2 It is a comparison chart of the wet combing force and the dry combing force before and after using Application Example 1;

[0028] Figure 3 It is a comparison chart of the wet combing work and the dry combing work before and after using Application Example 1;

[0029] Figure 4 It is a comparison chart of the inhibitory rate of Malassezia for the sample in Application Example 1. The left figure is the comparison chart of the inhibitory rate of Malassezia furfur after diluting the sample 100 times, and the right figure is the comparison chart of the inhibitory rate of Malassezia furfur after diluting the sample 1000 times;

[0030] Figure 5 It is a comparison chart of the tensile strength and the work of rupture for Application Example 2;

[0031] Figure 6 It is a comparison chart of the wet combing force and the dry combing force before and after using Application Example 2;

[0032] Figure 7 It is a comparison chart of the wet combing work and the dry combing work before and after using Application Example 2;

[0033] Figure 8It is a comparison chart of the antibacterial rate of Malassezia for the sample in Application Example 2. The left figure is the comparison chart of the antibacterial rate of Malassezia furfur after diluting the sample 100 times, and the right figure is the comparison chart of the antibacterial rate of Malassezia furfur after diluting the sample 1000 times;

[0034] Figure 9 It is the gel permeation chromatogram of the extract of Abelmoschus manihot under the condition of enzyme promotion;

[0035] Figure 10 It is the gel permeation chromatogram of the extract of Abelmoschus manihot under the condition without enzyme. Detailed implementation manners

[0036] The present invention provides a preparation method of an extract of Abelmoschus manihot, comprising the following steps:

[0037] Mix Abelmoschus manihot, biological enzyme and water and perform ultrasonic extraction to obtain a crude extract of Abelmoschus manihot;

[0038] Mix the crude extract of Abelmoschus manihot and Sevage reagent and perform protein removal treatment to obtain a purified solution;

[0039] Freeze-dry the purified solution to obtain an extract of Abelmoschus manihot.

[0040] In the present invention, unless otherwise specified, the materials and equipment used are all commercially available products in the art.

[0041] The present invention mixes Abelmoschus manihot, biological enzyme and water and performs ultrasonic extraction to obtain a crude extract of Abelmoschus manihot.

[0042] In the present invention, the Abelmoschus manihot preferably includes the root of Abelmoschus manihot, the flower of Abelmoschus manihot or the leaf of Abelmoschus manihot, and more preferably the root of Abelmoschus manihot.

[0043] In the present invention, the Abelmoschus manihot is preferably used in the form of Abelmoschus manihot powder. The moisture content of the Abelmoschus manihot powder is preferably less than 10 wt%, and the particle size is preferably less than 0.63 mm.

[0044] In the present invention, the water is preferably ultrapure water.

[0045] In the present invention, the dosage ratio of the Abelmoschus manihot to the water is preferably 1 g:(5 - 30) mL, and more preferably 1 g:15 mL or 1 g:20 mL.

[0046] The present invention preferably mixes Abelmoschus manihot and water first and stands for a period of time, and then adds a biological enzyme; the standing time is preferably 3 - 24 h, and specifically can be 12 h or overnight.

[0047] In the present invention, the biological enzyme preferably includes one or more of cellulase, pectinase and papain, and more preferably cellulase.

[0048] In the present invention, the addition amount of the bio-enzyme is preferably 0-20% of the mass fraction of Abelmoschus manihot, and not 0, more preferably 1%-6%.

[0049] In the present invention, preferably before the ultrasonic extraction, it further includes: adjusting the pH value of the obtained mixed solution to 2-6, more preferably 4-6, and specifically can be 4, 4.5, 5, 5.5 or 6. The pH value regulator is preferably dilute hydrochloric acid, and the mass fraction of the dilute hydrochloric acid is preferably 14.4%.

[0050] In the present invention, the temperature of the ultrasonic extraction is preferably 30-60 °C, specifically can be 40 °C or 50 °C, the time is preferably 10-90 min, more preferably 40 min; the power of the ultrasonic extraction is preferably 300 W.

[0051] In the present invention, preferably after the ultrasonic extraction, it further includes: inactivating the enzyme, separating the solid and liquid, and the obtained supernatant is the crude extract of Abelmoschus manihot. The temperature for inactivating the enzyme is preferably 0 °C, the time is preferably 15 min, and specifically can be inactivating the enzyme with ice water. The solid-liquid separation preferably includes centrifugation and filtration; the rotation speed of the centrifugation is preferably 6000 r / min, the time is preferably 5 min; the filtration is preferably vacuum filtration.

[0052] After obtaining the crude extract of Abelmoschus manihot, the present invention mixes the crude extract of Abelmoschus manihot and Sevage reagent for protein removal treatment to obtain a purified solution.

[0053] In the present invention, the ratio of the mass of Abelmoschus manihot to the volume of Sevage reagent is preferably 1 g:(1-3) mL, more preferably 1 g:2 mL. The Sevage reagent includes chloroform and n-butanol, and the volume ratio of chloroform to n-butanol is preferably 4:1.

[0054] In the present invention, the number of times of the protein removal treatment is preferably 3 times. The present invention allows the aqueous phase obtained in the last time to stand overnight, and centrifuges to remove the precipitate to obtain a purified solution.

[0055] After obtaining the purified solution, the present invention freeze-dries the purified solution to obtain an Abelmoschus manihot extract.

[0056] In the present invention, the freeze-drying preferably includes: pre-freezing the purified solution until it is completely frozen into ice, and performing vacuum freeze-drying; the time of the vacuum freeze-drying is preferably 65 h.

[0057] The present invention also provides an Abelmoschus manihot extract obtained by the preparation method described in the above technical solution. The main components of the Abelmoschus manihot extract include oligosaccharides, polysaccharides and flavonoids. The mass content of oligosaccharides in the Abelmoschus manihot extract is 0.5%-3%, the mass content of polysaccharides > 85%, and the mass content of flavonoids is 0.1%-1%.

[0058] The present invention also provides the application of the Abelmoschus manihot extract described in the above technical solution in hair care products.

[0059] In the present invention, the Abelmoschus manihot extract is preferably used in the form of an aqueous solution of Abelmoschus manihot extract. The mass concentration of the Abelmoschus manihot extract in the aqueous solution of Abelmoschus manihot extract is preferably 1% - 5%, more preferably 2% - 4%, and still more preferably 3%.

[0060] In the present invention, based on 1 g of hair, the dosage of the aqueous solution of Abelmoschus manihot extract is preferably 0.2 - 0.3 g.

[0061] In the present invention, the water in the aqueous solution of Abelmoschus manihot extract is preferably deionized water after sterilization.

[0062] The present invention also provides a hair care product, which includes Abelmoschus manihot extract, a preservative, and water. The mass concentration of the Abelmoschus manihot extract in the hair care product is 1% - 5%.

[0063] In the present invention, the preservative preferably includes potassium sorbate. The mass concentration of the preservative in the hair care product is preferably 0.5% - 3%. The preservative can prevent the Abelmoschus manihot extract solution from spoiling.

[0064] In the present invention, the hair care product preferably further includes a thickener. The thickener preferably includes one or more of glyceryl stearate, sodium carboxymethyl cellulose, propylene glycol, and glycerol. The mass concentration of the thickener in the hair care product is preferably 0.5% - 2%.

[0065] Using the Abelmoschus manihot extract obtained by the present invention as a hair conditioner, there is no need to additionally add an anti-dandruff agent and a moisturizer, solving the problem that traditional natural hair conditioners still need to additionally add anti-dandruff agents, moisturizers, nourishing agents, etc. to achieve the hair care effect. The results of in vitro hair care experiments show that the Abelmoschus manihot extract has the effects of preventing hair breakage, hair care, and anti-dandruff, laying a foundation for the application of the Abelmoschus manihot extract in the hair care field.

[0066] For the hair samples treated with the Abelmoschus manihot extract, both the tensile strength and the work at break are improved, indicating that using the Abelmoschus manihot extract as a hair care raw material has the effect of preventing hair breakage. For the hair samples treated with the Abelmoschus manihot extract, both the dry / wet combing force and the combing work are reduced, indicating that the Abelmoschus manihot extract as a hair care raw material has the effect of hair care. The Abelmoschus manihot extract has antibacterial activity against Malassezia, indicating that the Abelmoschus manihot extract as a hair care raw material has the effect of anti-dandruff.

[0067] To further illustrate the present invention, the Abelmoschus manihot extract provided by the present invention, its preparation method, and its application in hair care products will be described in detail below with reference to the accompanying drawings and examples, but they should not be construed as limiting the protection scope of the present invention.

[0068] Example 1

[0069] Dry the root of Hibiscus hibiscus to make its moisture content <10%, crush and sieve (aperture 0.630mm, 30 mesh) to obtain Hibiscus hibiscus root powder. Weigh 5g of Hibiscus hibiscus root powder, mix it with ultrapure water according to the solid-liquid ratio of 1:20 (g / mL), and let it stand overnight. Use 14.4% hydrochloric acid to adjust pH=6.0, set the ultrasonic power to 300W, the time to 40min, the ultrasonic temperature to 40℃, and the amount of cellulase added (based on the mass of Hibiscus hibiscus root powder) to 1%. After the end, take out the ice water to kill the enzyme for 15min, centrifuge at 6000r / min for 5min, and filter under reduced pressure. The supernatant is the crude extract of Hibiscus hibiscus root.

[0070] Subsequently, Sevage reagent was added in a volume ratio of 1:2 (g / mL) of hibiscus root powder to Sevage reagent (chloroform-n-butanol volume ratio 4:1), mixed thoroughly, allowed to stand to separate layers, and the aqueous phase was retained using a separatory funnel. This operation was repeated three times. After the organic layer was removed for the third time, it was allowed to stand overnight, centrifuged to remove protein precipitation, the liquid was pre-frozen until it was completely solidified into ice, and vacuum freeze-dried for 65 hours. The weight of the hibiscus extract was weighed, and the yield was calculated to be 15.33%.

[0071] Example 2

[0072] Dry the root of Hibiscus hibiscus to make its moisture content <10%, crush and sieve (aperture 0.630mm, 30 mesh) to obtain Hibiscus hibiscus root powder. Weigh 5g of Hibiscus hibiscus root powder, mix it with ultrapure water according to the solid-liquid ratio of 1:15 (g / mL), and let it stand overnight. Use 14.4% hydrochloric acid to adjust pH=4.0, set the ultrasonic power to 300W, the time to 40min, the ultrasonic temperature to 40℃, the amount of cellulase added (based on the mass of Hibiscus hibiscus root powder) to 1%, take out ice water to kill enzyme for 15min after the end, centrifuge at 6000r / min for 5min, and filter under reduced pressure. The supernatant is the crude extract of Hibiscus hibiscus root.

[0073] Subsequently, Sevage reagent was added in a volume ratio of 1:2 (g / mL) of hibiscus root powder to Sevage reagent (chloroform-n-butanol volume ratio 4:1), mixed thoroughly, allowed to stand to separate layers, and the aqueous phase was retained using a separatory funnel. This operation was repeated three times. After the organic layer was removed for the third time, it was allowed to stand overnight, centrifuged to remove protein precipitates, the liquid was pre-frozen until it was completely solidified into ice, and vacuum freeze-dried for 65 hours. The weight of the hibiscus extract was weighed, and the yield was calculated to be 14.79%.

[0074] Embodiments 3 to 8

[0075] The difference from Example 1 is that the cellulase is replaced by pectinase, papain or a mixed enzyme thereof (the total amount of enzyme added is 1% based on the mass of hibiscus root powder, and the enzyme types and their mass ratios are shown in Table 1), and the other conditions are the same.

[0076] The yield results of Example 1 and Examples 3 to 8 are shown in Table 1:

[0077] Table 1 Yield of hibiscus tiliaceus extract under different enzymes

[0078] Example Enzyme types and their mass ratios Yield (%) 1 Cellulase 15.33 3 Pectinase 13.52 4 Papain 12.81 5 Cellulase:Pectinase = 1:1 13.32 6 Cellulase:Papain = 1:1 10.98 7 Papain:Pectinase = 1:1 11.78 8 Cellulase:Pectinase:Papain = 1:1:1 11.76

[0079] In Examples 5 to 8, mixed enzymes were used, and the yield of hibiscus hibiscus extract was reduced. The reason may be the antagonism between enzymes, resulting in reduced catalytic activity; or the enzyme concentration dilution effect.

[0080] Examples 9 to 12

[0081] The difference from Example 2 is that the pH values ​​are adjusted to 4.5, 5.0, 5.5 and 6.0 respectively, and the other conditions are the same.

[0082] The yield results of Example 2 and Examples 9 to 12 are shown in Table 2:

[0083] Table 2 Yield of hibiscus tiliaceus extract under different enzymatic hydrolysis pH values

[0084]

[0085]

[0086] Application Example 1

[0087] Preparation of hibiscus hibiscus extract solution: 3.01 g of the hibiscus hibiscus extract prepared in Example 1 was dissolved in 100 mL of sterilized deionized water to prepare a hibiscus hibiscus extract solution with a mass concentration of 3%.

[0088] (1) Anti-hair breakage efficacy test: The anti-hair breakage efficacy is mainly characterized by the tensile strength and work to break of the sample before and after use. Abelmoschus hibiscus extract solution is used as the sample, and clean water is used as the control. Damaged in vitro hair bundles are selected, and the diameter of the damaged hair bundles is measured using a micrometer, which is reserved for calculating the tensile strength. The test is divided into a control group and a sample group, and the effective number of each group is greater than 30 hairs.

[0089] The hair samples to be tested are rinsed with flowing constant-temperature (37°C) water. According to the dosage of 0.2 grams of the sample (Abelmoschus manihot extract solution) per gram of hair bundle, it is evenly applied on the hair surface (simulating the actual process of using shampoo, wearing gloves and repeatedly and evenly applying the sample on the hair surface by hand), with a usage time of about 30 seconds, and then rinsed and the hair surface is blotted dry with a soft and clean paper towel. The hair samples are placed in a constant-temperature and constant-humidity [(26±2)°C, (60±10)%RH] environment and naturally dried for 24 hours, and then single-fiber tensile tests are carried out.

[0090] The tensile strength before and after using the sample is calculated by the following formula:

[0091]

[0092] The results are statistically analyzed using SPSS software, and an independent-samples t-test is used for comparison between the test sample and the control sample. The significance level α = 0.05. If P>0.05, it indicates that there is no significant difference between the two groups; if P<0.05, it indicates that there is a significant difference between the two groups. Table 3 shows the test results of tensile strength and work at break. Figure 1 It is a comparison chart of tensile strength and work at break for Application Example 1.

[0093] Table 3 Test results of tensile strength and work at break

[0094]

[0095] The test results show that: the average tensile strength and work at break of the sample group are both better than those of the control group, and the P value of the statistical difference <0.05, indicating a significant difference, proving that the test sample has the efficacy of preventing hair breakage.

[0096] (2) Hair care efficacy test: The hair care efficacy is mainly characterized by the combing force and combing work before and after using the sample. Using the Abelmoschus manihot extract solution as the sample and pure water as the control.

[0097] Take 10 clean hair pieces and randomly divide them into two groups, with 5 pieces in each group. One group is the sample group and the other group is the control group. Number the hair pieces, turn on the hair function tester, set the instrument displacement to 12 cm and the speed to 1 cm / s, and measure the combing work of each hair piece, ensuring that the starting point of each hair piece test is the same and the hair tail completely passes through the comb to end.

[0098] Baseline group setting: Thoroughly moisten the hairpiece with flowing constant-temperature clear water. Apply evenly on the surface of the hairpiece at a dosage of 0.2 g of cleaning solution per gram of hair bundle (the cleaning solution is a 10% mass fraction sodium dodecyl sulfate solution). (Wear gloves and evenly coat the sample on the hair surface by hand repeatedly). The application time is 30 seconds, let it stand for about 1 minute, and then rinse for 30 seconds. Fix the treated hairpiece at the test position, conduct the baseline wet hair combing test to obtain the wet combing force data of the W0-1 baseline group and the W'0-1 baseline group. Put the hairpiece after the wet hair test into a thermostatic and humidified chamber to balance for more than 4 hours, take it out and fix it at the test position, conduct the baseline dry hair combing test, and obtain the dry combing force data of the D0-1 baseline group and the D'0-1 baseline group. Integrate the combing force with respect to the displacement length to obtain the corresponding combing work.

[0099] Determination of the combing force and combing work of the sample and the control: Thoroughly moisten the hair bundles of the sample group that have completed the baseline combing test with constant-temperature flowing clear water. Apply evenly on the surface of the hairpiece at a dosage of 0.2 g of the sample or pure water without the sample per gram of hairpiece. The application time is 30 seconds, let it stand for 1 minute, and then rinse for 30 seconds. Fix the treated hairpiece at the test position, conduct the sample wet hair combing test, and obtain the wet combing force data of the W1-1 sample group and the W'1-1 control group. Put the hairpiece after the wet hair test into a thermostatic and humidified chamber to balance for more than 4 hours, take it out and fix it at the test position, conduct the sample dry hair combing test, and obtain the dry combing force data of the D1-1 sample group and the D'1-1 control group. Integrate the combing force with respect to the displacement length to obtain the corresponding combing work.

[0100] Data processing: Use SPSS software to statistically analyze the results. The independent samples t-test is used for comparison between the test sample and the control sample. The significance level α = 0.05. If P > 0.05, it indicates that there is no significant difference between the two groups; if P < 0.05, it indicates that there is a significant difference between the two groups. Table 4 shows the test results of the combing force and combing work. Figure 2 It is a comparison chart of the wet combing force before and after the use of Application Example 1. Figure 3 It is a comparison chart of the wet combing work and dry combing work before and after the use of Application Example 1. In the figure, NS indicates no significant relationship.

[0101] Table 4 Test results of the combing force and combing work

[0102]

[0103]

[0104] The test results showed that after using the sample, both the average wet combing force (W1-1) and wet combing work (W11-1) of the test sample group were better than the average wet combing force (W0-1) and wet combing work (W10-1) of the baseline group, and both the average dry combing force (D1-1) and dry combing work (D11-1) of the test sample group were better than the average dry combing force (D0-1) and dry combing work (D10-1) of the baseline group; after using the sample, both the average wet combing force (W1-1) and wet combing work (W11-1) of the test sample group were better than the average wet combing force (W'1-1) and wet combing work (W1'1-1) of the blank control group, and both the average dry combing force (D1-1) and dry combing work (D11-1) of the test sample group were better than the average dry combing force (D'1-1) and dry combing work (D1'1-1) of the blank control group. The P value of the statistical difference was <0.05, indicating a significant difference, proving that the test sample had the ability to improve hair combability and had a hair care effect.

[0105] (3) Dandruff removal efficacy test: The dandruff removal efficacy test was achieved by using the Malassezia furfur antibacterial test. The solution of Abelmoschus manihot extract was used as the sample, while phosphate buffer was used as the blank control and the suspension of Malassezia furfur + phosphate buffer was used as the control sample respectively. The sample group, blank control group and control sample group were set up.

[0106] Take the suspension of Malassezia furfur, add it to each test sample solution and control sample solution respectively and mix evenly. Start timing. When the specified action time is reached, dilute the samples 100 times and 1000 times respectively. Absorb 1 ml of each test sample solution and control sample solution and place them in two petri dishes respectively. Pour the Malassezia furfur culture medium and mix evenly. After it solidifies, turn the petri dish over and put it in the incubator for 7 days for viable count.

[0107] Calculate the Malassezia furfur antibacterial rate through the following formula:

[0108]

[0109] Where: A is the average colony count of the control sample; B is the average colony count of the test sample.

[0110] Table 5 shows the test results of the Malassezia furfur antibacterial rate. Figure 4 It is a comparison chart of the Malassezia furfur antibacterial rate for the sample in Application Example 1. The left figure is the comparison chart of the Malassezia furfur antibacterial rate when the sample is diluted 100 times, and the right figure is the comparison chart of the Malassezia furfur antibacterial rate when the sample is diluted 1000 times.

[0111] Table 5 Test results of the Malassezia furfur antibacterial rate

[0112] Name Unit Test results Bacteriostatic rate Bacteriostatic time Sample CFU / mL <![CDATA[5.0×10 3 > 94％ 10 min Blank control CFU / mL <10 / 10 min Control sample group CFU / mL <![CDATA[9.0×10 4 > / 10 min

[0113] The test results show that: the blank control is < 10 CFU / mL, and the Malassezia furfur in the control sample group is 9.0×10 4 CFU / mL, the system is effective. When the original sample solution is added, the Malassezia furfur is 5.0×10 3 CFU / mL, and the inhibition rate is 94%, indicating that the sample has an anti-dandruff effect.

[0114] Application Example 2

[0115] Preparation of the Abelmoschus manihot extract solution: Take 2.01 g of the Abelmoschus manihot extract prepared in Example 2 and dissolve it in 100 mL of sterilized deionized water to prepare an Abelmoschus manihot extract solution with a mass concentration of 2%.

[0116] The test method for the following tests is the same as that in Application Example 1

[0117] (1) Anti-hair breakage efficacy test: Table 6 shows the test results of tensile strength and work to break, Figure 5 which is a comparison chart of tensile strength and work to break in Application Example 2.

[0118] Table 6 Test results of tensile strength and work to break

[0119]

[0120] The test results show that: the average tensile strength and work to break of the sample group are better than those of the control group, and the P value of the statistical difference is < 0.05, indicating a significant difference, proving that the test sample has an anti-hair breakage effect.

[0121] (2) Hair care efficacy test: Table 7 shows the test results of tensile strength and work to break, Figure 6 which is a comparison chart of wet combing force and dry combing force before and after using Application Example 2, Figure 7 which is a comparison chart of wet combing work and dry combing work before and after using Application Example 2. In the figure, NS indicates no significant relationship.

[0122] Table 7 Test results of combing force and combing work

[0123]

[0124] The test results show that: after using the sample, both the average wet combing force (W1-2) and wet combing work (W11-2) of the test sample group are better than the average wet combing force (W0-2) and wet combing work (W10-2) of the baseline group, and both the average dry combing force (D1-2) and dry combing work (D11-2) of the test sample group are better than the average dry combing force (D0-2) and dry combing work (D10-2) of the baseline group; after using the sample, both the average wet combing force (W1-2) and wet combing work (W11-2) of the test sample group are better than the average wet combing force (W'1-2) and wet combing work (W1'1-2) of the blank control group, and both the average dry combing force (D1-2) and dry combing work (D11-2) of the test sample group are better than the average dry combing force (D'1-2) and dry combing work (D1'1-2) of the blank control group. The P value of the statistical difference is <0.05, indicating a significant difference, which proves that the test sample has the ability to improve hair combability and has a hair care effect.

[0125] (3) Dandruff removal efficacy test: Table 8 shows the test results of the inhibitory rate of Malassezia furfur. Figure 8 It is a comparison chart of the inhibitory rate of Malassezia furfur for the sample in Application Example 2. The left chart is the comparison chart of the inhibitory rate of Malassezia furfur when the sample is diluted 100 times, and the right chart is the comparison chart of the inhibitory rate of Malassezia furfur when the sample is diluted 1000 times.

[0126] Table 8 Test results of the inhibitory rate of Malassezia furfur

[0127] Name Unit Test results Bacteriostatic rate Bacteriostatic time Sample CFU / mL <![CDATA[1.4×10 4 > 84％ 10 min Blank control CFU / mL <10 / 10 min Control sample group CFU / mL <![CDATA[9.0×10 4 > / 10 min

[0128] The test results show that: the blank control is <10 CFU / mL, the Malassezia furfur in the control sample group is 9.0×10 4 CFU / mL, the system is effective. When the original sample solution is added, the Malassezia furfur is 1.4×10 4 CFU / mL, and the inhibition rate is 84%, indicating that the sample has a dandruff removal effect.

[0129] Figure 9 It is the gel permeation chromatogram of the extract of Abelmoschus manihot (Example 1) under enzyme-promoted conditions. Figure 10 It is the gel permeation chromatogram of the extract of Abelmoschus manihot (only different from Example 1 in that cellulase is not added) under enzyme-free conditions. Under the same extraction conditions, the gel permeation chromatographic analysis results of the enzyme-promoted extract of Abelmoschus manihot and the enzyme-free extract of Abelmoschus manihot show that the chromatographic peak (retention time about 24 minutes) corresponding to the extract with a larger molecular weight (greater than 2000000 Da) in the enzyme-promoted extract of Abelmoschus manihot is below the detection limit. It shows that under the action of the enzyme, the average molecular weight of the extract can be effectively reduced.

[0130] Compared with the sapindus mukorossi extract in the authorized patent CN 109666549 B, a hair cleansing soap containing sapindus mukorossi extract, the dry combing and wet combing functions of the abelmoschus manihot extract are both less than those of the sapindus mukorossi extract, indicating that the abelmoschus manihot extract has more excellent hair care and softening properties. Compared with the published patent CN 118415912A, the application of hibiscus flower polysaccharide in the preparation of anti-malassezia furfur hair care products, the abelmoschus manihot extract shows stronger anti-malassezia furfur antibacterial ability at a lower concentration than the hibiscus flower polysaccharide extract (the antibacterial rate of 300 μg / mL abelmoschus manihot extract is 94%, which is better than the antibacterial rate of 60% of 390 μg / mL hibiscus flower polysaccharide extract). Therefore, the anti-dandruff effect of the abelmoschus manihot extract of the present invention is better.

[0131] In the present invention, the abelmoschus manihot extract is used as a raw material for hair care products. The results of in vitro hair care experiments show that the abelmoschus manihot extract solution has the effects of preventing hair breakage, hair care, and anti-dandruff, and is a potential excellent raw material for hair care products.

[0132] Although the above embodiments have described the present invention in detail, they are only a part of the embodiments of the present invention, not all of them. People can also obtain other embodiments according to the embodiments of the present invention without creative work, and these embodiments all belong to the protection scope of the present invention.

Claims

1. A method for preparing an Abelmoschus manihot extract, characterized in that, It includes the following steps: Mix Abelmoschus manihot, biological enzyme and water and perform ultrasonic extraction to obtain a crude extract of Abelmoschus manihot; Mix the crude extract of Abelmoschus manihot and Sevage reagent for protein removal treatment to obtain a purified solution; Freeze-dry the purified solution to obtain an Abelmoschus manihot extract.

2. The preparation method according to claim 1, characterized in that, The biological enzyme includes one or more of cellulase, pectinase and papain.

3. The preparation method according to claim 1 or 2, characterized in that, The addition amount of the biological enzyme is 0-20% of the mass fraction of Abelmoschus manihot and is not 0.

4. The preparation method according to claim 1, characterized in that, The temperature of the ultrasonic extraction is 30-60°C and the time is 10-90 min.

5. The preparation method according to claim 1, characterized in that The dosage ratio of Abelmoschus manihot to water is 1 g:(5-30) mL.

6. The preparation method according to claim 1, characterized in that, The ratio of the mass of Abelmoschus manihot to the volume of Sevage reagent is 1 g:(1-3) mL.

7. The Abelmoschus manihot extract obtained by the preparation method according to any one of claims 1 to 6, characterized in that, It includes oligosaccharides, polysaccharides and flavonoids. The mass content of oligosaccharides in the Abelmoschus manihot extract is 0.5%-3%, the mass content of polysaccharides is >85%, and the mass content of flavonoids is 0.1%-1%.

8. Application of the Abelmoschus manihot extract according to claim 7 in hair care products.

9. The application according to claim 8, wherein The Abelmoschus manihot extract is used in the form of an aqueous solution of Abelmoschus manihot extract, and the mass concentration of the Abelmoschus manihot extract in the aqueous solution of Abelmoschus manihot extract is 1%-5%.

10. A hair care product, characterized in that, It includes Abelmoschus manihot extract, preservative and water. The mass concentration of Abelmoschus manihot extract in the hair care product is 1%-5%.

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