A hair care composition having long-lasting detangling benefits

Abstract

This invention belongs to the field of daily chemical products, specifically relating to a hair care composition with a long-lasting smoothing effect on hair, comprising the following components by weight percentage: 1.05-5.1% linear asparagine plant exosome-silicone oil combination; 1-10% higher fatty alcohols; 0.5-10% cationic conditioning agent; 0.5-10% moisturizer; and the balance being purified water; wherein the linear asparagine plant exosome-silicone oil combination comprises 0.05-0.1% linear asparagine plant exosomes and 1-5% silicone oil; the viscosity of the silicone oil is 10-300 cSt. The composition of this invention exhibits a significant long-lasting smoothing effect. By constructing a deep repair mechanism using linear asparagine plant exosomes and surface protection using silicone oil, and further combining it with the synergistic compounding system of the remaining components, it achieves comprehensive care that improves hair quality from the root and provides long-lasting smoothness.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical products, and specifically relates to a hair care composition that has a long-lasting effect of making hair smooth. Background Technology

[0002] As living standards improve, consumers' demands for hair care products are also constantly increasing. Consequently, a variety of products with different functions have emerged on the market to specifically improve problems such as dry, frizzy, and flat hair.

[0003] Most common hair care products achieve their desired effects through a combination of active ingredients, and many of these ingredients contain silicone oil. Silicone oil forms a film on the surface of the hair to improve its smoothness. However, regular silicone oil only physically coats the surface of the hair, resulting in a short-lived repair effect and failing to provide lasting smoothness. It often leads to smoothness after use, but the hair becomes rough the next day. Furthermore, it cannot balance gentle scalp care with long-lasting smoothness, making it unsuitable for stubborn, damaged hair types such as naturally curly or frizzy hair. In addition, existing hair care products often use high-viscosity modified silicone oil in pursuit of long-lasting smoothness, which not only easily leads to flat, heavy hair but also has poor biodegradability and tends to accumulate in the environment. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a hair care composition with a long-lasting smooth hair effect. By constructing a deep repairing method of linear asparagine plant exosomes and surface protection of silicone oil, and then rationally combining the other components into a synergistic compound system, it can achieve comprehensive care that improves hair quality from the root and provides long-lasting smoothness.

[0005] The technical solution adopted by the present invention to solve the above problems is as follows: A hair care composition with a long-lasting smoothing effect on hair, comprising the following components by weight percentage: 1.05-5.1% linear asparagine plant exosome-silicone oil combination; 1-10% higher fatty alcohols; 0.5-10% cationic conditioning agent; 0.5-10% moisturizer; balance: purified water; The linear asparagine plant exosome-silicone oil combination comprises 0.05-0.1% linear asparagine plant exosomes and 1-5% silicone oil; the viscosity of the silicone oil is 10-300 cSt.

[0006] Through the above technical solution, the linear asparagine plant exosomes of the present invention are extracellular vesicles with a diameter of nanometers, containing effective components such as a lipid bilayer, tea polyphenols, tetraspan membrane proteins (CD9, CD63), amino acids, flavonoids, SOD enzymes, aspartame, and nucleic acids. Amino acids are keratin precursors, which can repair broken keratin fibers and enhance hair toughness; flavonoids and SOD enzymes can scavenge free radicals, reducing oxidation-induced hair breakage and yellowing; aspartame can regulate the moisture balance of the cortex, reducing hair dryness; tetraspan membrane proteins can slightly regulate the metabolism of hair cuticle cells, promoting the autonomous closure of hair cuticles, laying the foundation for silicone oil's protective effect. The nano-sized linear asparagine plant exosomes can penetrate the hair cuticle, carrying amino acids, proteins, and other biomolecules deep into the hair shaft to replenish hair nutrition, while simultaneously regulating the scalp microenvironment, achieving deep repair and root-cause nourishment. In the composition of the present invention, the concentration of the finished linear asparagine plant exosome is consistently maintained at 1×10⁻⁶. 10 ~1×10 12 When this exosome product is added at a weight percentage of 0.05–0.1%, the exosome concentration in the composition can be maintained at the effective threshold for significant cortical repair, ensuring that the exosomes can carry active ingredients and fully penetrate into the hair shaft. Linear asparagine plant exosomes can form a synergistic system with silicone oil for deep penetration and surface protection. The linear asparagine plant exosomes are responsible for deep repair, while the silicone oil forms a water-locking film to reduce the loss of active ingredients.

[0007] Furthermore, the method for preparing the linear asparagus plant exosomes includes the following steps: S1. Select the leaves and stems of linear asparagus plants and wash them with water. Then soak them in 70-75% anhydrous ethanol for 10-20 seconds. After soaking, rinse them several times with sterile deionized water and drain the surface water to obtain the treated leaves and stems. S2. Transfer the treated leaves and stems to a sterile mortar that has been pre-cooled at 2-6°C, and add liquid nitrogen to freeze them until they harden. Keep the mortar at the pre-cooled temperature and grind the treated leaves and stems into powder. Add liquid nitrogen several times during grinding to keep the powder temperature at 2-6°C to obtain linear asparagus powder. S3. Prepare a homogenization buffer pre-cooled to 2-6℃. Use sterile phosphate buffer. Add 0.05-0.15 mL of disodium ethylenediaminetetraacetate, 0.5-2 mL of protease inhibitor cocktail, and 10-50 U of RNase inhibitor to every 100 mL of sterile phosphate buffer. Mix well and cool to 2-6℃ to obtain the homogenization buffer. S4. Mix the linear astragalus powder with 1g of the powder in a sterile environment at a ratio of 6-10mL homogenization buffer. Stir at 2-6℃ and 8000-12000rpm for 4-6 minutes, pausing 2-3 times during the stirring process, each pause for 30 seconds. After stirring until homogenized, a homogenate is obtained. S5. The homogenate was centrifuged for the first time in a sterile environment at a temperature of 2–6°C and a relative centrifugal force of 500–1000 xg for 10–20 min. The supernatant was collected and centrifuged for the second time at a temperature of 2–6°C and a relative centrifugal force of 2000–5000 xg for 30–50 min. The supernatant obtained from the second centrifugation was then subjected to ultracentrifugation at a temperature of 4°C and a relative centrifugal force of 10000–15000 xg for 30–40 min. The supernatant obtained from the ultracentrifugation was collected to obtain the extract. The extract was transferred to an ultracentrifuge tube, and sterile phosphate buffer pre-cooled at 2–6°C was added to 2 / 3 of the volume. The temperature was adjusted to 2–6°C, and the tube was centrifuged at a relative centrifugal force of 100000–150000 xg for 2–4 h. After centrifugation, the supernatant was discarded, and the bottom precipitate was collected to obtain the crude exosome precipitate. S6. Take 1-2 mL of pre-cooled sterile phosphate buffer at 2-6℃ and filter it through a 0.22 μm filter membrane. Then, slowly add the filtered sterile phosphate buffer to an ultracentrifuge tube containing crude exosomes. Gently pipette the crude exosomes while avoiding violent shaking to resuspend them. Transfer the resuspended exosomes to another ultracentrifuge tube and add sterile phosphate buffer to 2 / 3 of the tube's capacity. Adjust the temperature to 2-6℃ and centrifuge at a relative centrifugal force of 100,000-150,000 x g for 1.5-2.5 h. Retain the precipitate at the bottom of the tube and analyze it. Electron microscopy shows a typical cup-shaped or spherical vesicle structure. Nanoparticle tracking analysis shows a particle size of 30-150 nm. Western blotting detects specific exosome marker proteins. After the exosome protein concentration is ≥0.5 mg / mL using the BCA protein quantification method, a high-purity linear asparagine plant exosome precipitate is obtained. S7. Take the high-purity linear asparagine plant exosome precipitate, add an appropriate amount of sterile deionized water, and gently pipette several times until the precipitate is completely dissolved, avoiding the generation of air bubbles. Add sterile deionized water to adjust the concentration of the high-purity linear asparagine plant exosome solution to 1×10⁻⁶. 10 ~1×10 12 The product was obtained by extracting linear asparagus plant exosomes at a concentration of 1 / mL.

[0008] Using the above technical solution, high-purity linear asparagine plant exosomes can be prepared. The obtained linear asparagine plant exosomes have cup-shaped or spherical vesicle structures, with particle sizes concentrated in the range of 30–150 nm, and the concentration can be stably maintained at 1 × 10⁻⁶. 10 ~1×10 12 It contains cells / mL and specifically expresses exosome marker proteins. This nanoscale size ensures its effective penetration into the hair cuticle gaps, laying the foundation for deep repair efficacy in hair care compositions.

[0009] Furthermore, the silicone oil includes at least one of polydimethylsiloxane, cyclodimethylsiloxane, cyclopentadimethylsiloxane, and polymethylphenylsiloxane.

[0010] Preferably, the viscosity of the silicone oil is 100 cSt.

[0011] Through the above technical solution, the silicone oil used in the composition of the present invention has both good extensibility and film-forming properties, which can form a hydrophobic film on the surface of hair without causing the hair to flatten due to excessive film thickness.

[0012] Furthermore, the polydimethylsiloxane is XIAMETER™ PMX-200 Silicone Fluid 100cSt.

[0013] Through the above technical solution, the polydimethylsiloxane uses the chemical-grade XIAMETER™ PMX-200 Silicone Fluid 100 cSt, which has better environmental compatibility and can reduce the risk of environmental accumulation. At the same time, the hydrophobic properties of XIAMETER™ PMX-200 Silicone Fluid 100 cSt can effectively block external moisture from penetrating to the hair surface, reducing the risk of linear asparagine plant exosomes that have penetrated into the cortex being lost with moisture. This, in turn, increases the retention rate of effective active ingredients in linear asparagine plant exosomes, laying the foundation for subsequent long-lasting repair.

[0014] Furthermore, the higher fatty alcohols include at least one of lauryl alcohol, tetradecyl alcohol, hexadecyl alcohol, hexadecyl / octadecyl alcohol, and stearyl alcohol.

[0015] The aforementioned technical solution utilizes advanced fatty alcohols that possess excellent spreadability and a certain thickening effect, improving the appearance and feel of the composition and reducing the possibility of system stratification. Among these, hexadecyl alcohol and hexadecyl / octadecyl alcohol exhibit even better spreadability, allowing for even coverage of the hair surface and reducing the greasy feeling caused by localized accumulation. Furthermore, the molecular structures of hexadecyl alcohol and hexadecyl / octadecyl alcohol are highly compatible with hair surface lipids, making them easier for the hair to absorb. This enhances hair shine and smoothness, and also forms an auxiliary nourishing film on the hair cuticle surface, synergistically enhancing hair smoothness in conjunction with silicone oil.

[0016] Furthermore, the cationic conditioner includes at least one of behenamidopropyl dimethylamine, stearamidopropyl dimethylamine, behenyltrimethylammonium chloride, and cetearyltrimethylammonium chloride.

[0017] Through the above technical solutions, cationic conditioning agents can impart softness, antistatic properties, moisturizing properties, and conditioning effects to hair. However, different hair types have conflicting needs for conditioning agents. Damaged and frizzy hair requires strong cationic adsorption to provide significant smoothness and repair, but this often results in heavy and flat hair. On the other hand, fine and oily hair seeks a refreshing and voluminous feel and is extremely sensitive to excessive adsorption and a heavy feeling. This invention utilizes the synergistic effect of stearamide-propyl dimethylamine and cetearyltrimethylammonium chloride to meet the needs of damaged and frizzy hair for smoothness and repair while simultaneously satisfying the needs of fine and oily hair for a refreshing and voluminous feel. On one hand, stearamide-propyl dimethylamine has excellent adsorption and moisturizing properties, forming a breathable moisturizing film on the hair surface to lock in moisture for a long time and alleviate problems such as dryness and frizz. On the other hand, cetearyltrimethylammonium chloride has higher cationic activity, resulting in more prominent antistatic properties and a smoothing effect, quickly reducing hair tangling during combing and minimizing friction damage. Meanwhile, the combination of stearamide propyl dimethylamine and cetearyl trimethylammonium chloride can reduce the heaviness of hair caused by high concentration of single cationic components, reduce the weight and flatness of hair strands, keep hair soft and smooth while maintaining a light texture, adapt to the care needs of different hair types, and further enhance the comprehensive conditioning ability of the composition of the present invention.

[0018] Furthermore, the moisturizer includes at least one of glycerin, sorbitol, and propylene glycol.

[0019] Through the above technical solution, the moisturizer possesses excellent hygroscopic properties, providing long-lasting hydration to the hair, making it nourished and smooth, and significantly improving dryness and frizz. Increasing the hair's moisture content enhances its resistance to environmental stimuli and protects its overall health.

[0020] Furthermore, the hair care composition may also include at least one of the following components: 0.05-2.5% thickener; 0.01-2% fragrance agent; 0.01-1.5% preservative; and 0.001-2% pH adjuster.

[0021] Furthermore, the thickener includes at least one of hydroxyethyl cellulose, carbomer, acrylic / C10-30 alkanol acrylate crosspolymer, and acrylate / C10-30 alkanol acrylate crosspolymer.

[0022] Furthermore, the fragrance agent includes at least one of fragrance and plant essential oil.

[0023] Furthermore, the preservative includes at least one of phenoxyethanol, sodium benzoate, benzyl alcohol, benzoic acid, and potassium sorbate.

[0024] Furthermore, the pH adjuster includes at least one of lactic acid, citric acid, arginine, sodium hydroxide, potassium hydroxide, and triethanolamine.

[0025] The present invention has the following beneficial effects: 1. The composition of this invention provides a significant and long-lasting smoothing effect. By constructing a deep-repairing linear asparagine plant exosome and a surface-locking silicone oil, combined with a synergistic system of other components, it achieves comprehensive care that improves hair quality from the root and provides long-lasting smoothness. Furthermore, the naturally derived linear asparagine plant exosomes have good biocompatibility, minimizing the risk of irritation or pore blockage, making long-term use safer.

[0026] 2. The composition of the present invention can meet the needs of fine and soft hair for lightness and volume, and can also meet the needs of damaged and coarse hair for strong repair and smoothness, and is widely suitable for various hair types.

[0027] 3. The preparation method of linear asparagine plant exosomes adopts liquid nitrogen grinding and ultracentrifugation process, which does not require complicated chemical reactions and is simple to operate; the overall production process of the composition has no high pollution and high energy consumption steps, the raw material cost is low, and the compounding of each component of the composition does not require special process, which can be integrated into the production line of existing products, which is conducive to large-scale promotion and easy production. Detailed Implementation

[0028] To make the technical problems, solutions, and advantages of this invention clearer, a detailed description will be provided below with reference to specific examples. However, the scope of protection of this invention is not limited to the following specific embodiments. The described embodiments are merely some, not all, of the embodiments of this invention, and are not intended to limit the invention. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0029] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0030] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.

[0031] In the quantitative experiments in the following examples, three replicate experiments were set up, and the data are the average of the three replicate experiments or the average ± standard deviation.

[0032] The present invention includes Examples 1 to 3 and Comparative Examples 1 to 5, and the specific components and contents are shown in Table 1, in units of weight percentage.

[0033] Table 1

[0034] Specifically, the method for preparing the linear asparagus plant exosomes includes the following steps: S1. Select the leaves and stems of linear asparagus plants and wash them with water. Then soak them in 75% anhydrous ethanol for 10-20 seconds. After soaking, rinse them several times with sterile deionized water and drain the surface water to obtain the treated leaves and stems. S2. Transfer the treated leaves and stems to a sterile mortar that has been pre-cooled at 4°C, add liquid nitrogen to quickly freeze until the treated leaves and stems harden, keep the mortar pre-cooled, grind the treated leaves and stems into powder, add liquid nitrogen several times during grinding, keep the powder temperature at 4°C, and obtain linear asparagus powder. S3. Prepare a homogenization buffer pre-cooled to 4℃. Use sterile phosphate buffer. Add 0.1 mL of disodium ethylenediaminetetraacetate, 1 mL of protease inhibitor cocktail, and 10 U of RNase inhibitor to every 100 mL of sterile phosphate buffer. Mix well and cool to 4℃ to obtain the homogenization buffer. S4. Mix the linear astragalus powder at a ratio of 1g to 8mL homogenization buffer in a sterile environment, stir at 4℃ and 10000rpm for 5min, pause twice during the stirring process, each pause for 30s, and stir until homogenized to obtain a homogenate. S5. The homogenate was centrifuged for the first time in a sterile environment at 4°C with a relative centrifugal force of 800xg for 15 min. The supernatant was then collected for a second centrifugation. The second centrifugation was performed at 4°C with a relative centrifugal force of 3500xg for 40 min. The supernatant from the second centrifugation was then subjected to ultracentrifugation. The ultracentrifugation was performed at 4°C with a relative centrifugal force of 12500xg for 35 min. The supernatant from the ultracentrifugation was collected to obtain the extract. The extract was transferred to an ultracentrifuge tube, and sterile phosphate buffer pre-cooled at 4°C was added to 2 / 3 of the tube's capacity. A fixed-angle rotor or a horizontal rotor was used for centrifugation. The temperature was set to 4°C, and the tube was centrifuged at a relative centrifugal force of 125000xg for 2 h. After centrifugation, the supernatant was discarded, and the loose white to pale yellow precipitate at the bottom was collected to obtain the coarse exosome precipitate. S6. Take 2 mL of 4℃ pre-cooled sterile phosphate buffer and filter it through a 0.22 μm filter membrane. Then, slowly add the filtered sterile phosphate buffer to an ultracentrifuge tube containing crude exosomes. Gently pipette the crude exosomes while avoiding violent shaking to resuspend them. Transfer the resuspended exosomes to another ultracentrifuge tube and add sterile phosphate buffer to 2 / 3 of the tube's capacity. Adjust the temperature to 4℃ and centrifuge at a relative centrifugal force of 125000xg for 2 hours. Retain the precipitate at the bottom of the tube and analyze it. Electron microscopy shows that it has a typical cup-shaped or spherical vesicle structure. Nanoparticle tracking analysis shows that the particle size is 30-150 nm. Western blotting detects the specific expression of exosome marker proteins. After the exosome protein concentration is ≥0.5 mg / mL by BCA protein quantification method, high-purity linear asparagine plant exosome precipitate is obtained. S7. Take the high-purity linear asparagine plant exosome precipitate, add an appropriate amount of sterile deionized water, and gently pipette several times until the precipitate is completely dissolved, avoiding the generation of air bubbles. Add sterile deionized water to adjust the concentration of the high-purity linear asparagine plant exosome solution to 1×10⁻⁶. 11 The product was obtained by extracting linear asparagus plant exosomes at a concentration of 1 / mL.

[0035] The preparation methods of the above embodiments and comparative examples are conventional mixing techniques in the art, and will not be described in detail here.

[0036] Experimental testing Comparative Examples 4 and 5 differed from Examples 1-3 in their non-core components. To verify the effects of these non-core components—lecithin and argan kernel oil in Comparative Example 4, and octadecyltrimethylammonium chloride in Comparative Example 5—on the core indicators, preliminary experiments were conducted: normal damaged hair strands were taken, and experimental concentrations of lecithin (0.28%), argan kernel oil (0.28%), and octadecyltrimethylammonium chloride (0.2%) were added respectively. Changes in cuticle closure rate and combing force were measured after 24 hours. The results showed that the preliminary experiments indicated that the above non-core components, when acting alone, had a negligible impact on the 24-hour cuticle closure rate and combing force. Furthermore, the experiments strictly controlled other irrelevant variables (such as reaction conditions and detection methods) and fixed the core verification indicators to ensure that the differences in these non-core components did not violate the principle of single variable analysis or interfere with the derivation of conclusions.

[0037] 1. Penetration test of plant exosomes from linear asparagus Experimental grouping: 24 strands of normal damaged hair were taken and divided into 8 groups, with three strands in each group.

[0038] Processing method: The hair strands were completely immersed in the corresponding examples and comparative samples, left to stand at a constant temperature of 25°C for 10 minutes to simulate the time the hair care products stayed on the surface, then gently rinsed with deionized water for 10 seconds, and then dried at 37°C to constant weight.

[0039] Detection method: Frozen sections were prepared to form 5 μm thick hair cross sections. CD63 protein of linear asparagine plant exosomes was labeled with FITC and its distribution in the hair cross section was observed using laser confocal microscopy. The proportion of linear asparagine plant exosomes reaching the cortex was determined. Ten sections were used in each group, and the average value was calculated.

[0040] Judgment criteria: When the proportion of linear asparagus plant exosomes reaching the cortex is ≥50%, it is determined that it has effective penetration ability. The test results are shown in Table 2.

[0041] Table 2

[0042] As shown in Table 2, the linear asparagine plant exosomes of Examples 1-3 and Comparative Example 2 all reached ≥50% of the cortex, with Example 2 reaching the highest at 79.6%, demonstrating effective penetration ability. In contrast, the penetration rates of Comparative Examples 1, 3, 4, and 5 were all 0, proving that the linear asparagine plant exosomes are the only component that can penetrate the cuticle to reach the cortex, overcoming the limitations of surface care and providing a foundation for deep repair.

[0043] 2. Detection of cortical cavity filling and keratin repair Experimental grouping: 24 bundles of normal damaged hair were taken and divided into 8 groups, with 3 bundles in each group.

[0044] Treatment method: The hair strands were completely immersed in the corresponding examples and comparative samples, left to stand at a constant temperature of 25°C for 5 minutes to simulate the time the hair care products stayed on the surface, then gently rinsed with deionized water for 10 seconds, and then dried at 37°C to constant weight. An untreated normal damaged hair strands were set up as a blank control.

[0045] Detection method: Cortical void ratio: The longitudinal section of the hair strands was observed using SEM, and the proportion of void area in the cortex was analyzed using ImageJ software (10 hair strands were counted in each group, and 3 fields of view were selected for each hair strand, and the average value was calculated). Using the average void ratio of the blank control group (untreated hair strands) as a benchmark, the reduction value (%) of the cortical void ratio in each experimental group was calculated using the following formula: Cortical void ratio reduction rate (%) = (Void ratio of blank control group - Void ratio of experimental group) / Void ratio of blank control group × 100%.

[0046] Keratin Repair: FTIR was used to determine the characteristic peak of keratin in hair strands (1650 cm⁻¹). -1 Amide I band, 1540cm -1 The absorbance change of the amide II band was compared with the absorbance difference ΔA before and after treatment. The larger the ΔA, the better the keratin repair effect.

[0047] Data recording: The reduction in cortical void ratio and keratin characteristic peak ΔA of the hair strands after treatment of 8 groups of samples were recorded. The specific results are shown in Table 3.

[0048] Table 3

[0049] Comparison of experimental data from Example 2 with Comparative Examples 1, 2, 4, and 5 shows that the reduction in cortical void rate and the keratin characteristic peak ΔA in Example 2 are significantly higher than those in Comparative Examples 1, 4, and 5, and also higher than those in Comparative Example 2. This indicates that linear asparagine plant exosomes can effectively fill cortical voids and replenish keratin precursors; when combined with silicone oil, the synergistic effect further enhances the repair effect, improving hair damage from the root and resolving the short-term drawback of immediate smoothness followed by frizz the next day.

[0050] 3. Short-term and long-term flexibility testing Experimental grouping: 48 hair bundles were taken from each of the three types of hair: normal damaged, naturally curly and sandy, and fine and soft. Each type of hair was divided into 8 groups, with 6 bundles in each group.

[0051] Simulated hair care process: Using a standard hair care simulation device, first use silicone-free shampoo to wash the hair strands at 38°C water temperature, rub and wash for 1 minute, rinse for 30 seconds, then apply the corresponding example and comparative sample at a dosage of 1g / strand, rub for 2 minutes, leave for 3 minutes, rinse for 30 seconds after using the sample, and dry at 37°C to constant weight, which is considered as one complete hair care cycle.

[0052] Testing time points: Smoothness-related indicators were measured at 0h, 24h, 48h, and 72h after washing and conditioning.

[0053] Detection indicators and methods: Hair cuticle closure rate: SEM was used to observe the surface of hair strands and the percentage of hair strands with completely closed cuticles was counted. Ten hair strands were counted in each group, and five fields of view were selected for each hair strand. The average value was calculated.

[0054] Contact angle: The contact angle of deionized water on the hair surface is measured using a contact angle meter. The larger the contact angle, the smoother the surface. Each group is measured 10 times and the average value is taken.

[0055] Combing force: The maximum resistance when combing hair strands with a comb (1mm tooth spacing) is measured using a hair combing force tester. The lower the combing force, the better the smoothness. Each group is measured 5 times and the average value is taken.

[0056] The specific test results are shown in Table 4.

[0057] Table 4

[0058] 4. Anti-leaking performance test Experimental grouping: 24 strands of normal damaged hair were taken and divided into 8 groups, with 3 strands in each group.

[0059] Treatment method: After completing the simulated washing and care process described in Experiment 3 once, the hair bundle was placed in a constant temperature and humidity chamber at 25℃ and 50% humidity. After 24h and 48h, it was gently rinsed with deionized water for 30s to simulate a small amount of moisture contact in the daily environment. After drying, the hair was tested.

[0060] Detection indicators: The retention rate of active ingredients (aspartate and flavonoids) of linear asparagine plant exosomes in hair strands was detected by HPLC. The changes in component content before and after rinsing were compared. The hydrophobic film formed by silicone oil can reduce water penetration and thus reduce the dissolution of active ingredients. Therefore, the higher the retention rate, the better the anti-loss effect.

[0061] The specific test results are shown in Table 5.

[0062] Table 5

[0063] Referring to Tables 4 and 5, a comparison of the experimental data from Examples 1-3 with Comparative Examples 2, 4, and 5 shows that Examples 1-3 exhibited higher retention rates of active ingredients after rinsing at 24h and 48h, with Example 2 showing a significantly higher retention rate than Comparative Example 2. Furthermore, at 24h, Example 2 demonstrated significantly better cuticle closure rate, contact angle, and combing power compared to Comparative Examples 4 and 5 in terms of normal damaged hair. Considering the hydrophobic film-forming properties of silicone oil, the core reason for this result is the continuous hydrophobic film formed by silicone oil on the hair surface. This film not only reduces the contact between water and hair in the daily environment but also prevents adsorbed exosomes from dissolving with water, thereby significantly improving the retention rate of active ingredients such as aspartame and flavonoids. Ultimately, this forms a complete closed loop of deep exosome penetration, repair of damaged hair, and silicone oil's hydrophobic locking and anti-loss mechanism, addressing the core pain points of easy loss of repairing ingredients and short-lived smoothing effects. Comparative Example 4 contains hydrolyzed wheat protein, which has a large molecular weight and is easily detached. Comparative Example 5 contains repair proteins, but they are easily lost during washing, resulting in a 0% retention rate of active ingredients in both samples after 24 hours. In contrast, this invention uses silicone oil to lock in exosomes, achieving a retention rate of 58.5% to 82.1%, further validating the effectiveness of existing technologies in addressing short-term pain points.

[0064] 5. Compatibility test for stubbornly damaged hair Experimental grouping: 48 strands of naturally curly hair and 48 strands of sandy hair were taken and divided into 8 groups, with 6 strands in each group.

[0065] Treatment method: After completing the simulated washing and care process described in Experiment 3 once, place it in a constant temperature and humidity chamber at 25℃ and 50% humidity for 24 hours.

[0066] Testing indicators: Hair cuticle closure rate: SEM was used to observe the surface of hair strands and the percentage of hair strands with completely closed cuticles was counted. Ten hair strands were counted in each group, and five fields of view were selected for each hair strand. The average value was calculated.

[0067] Hair elasticity recovery rate: The elasticity recovery rate of hair under 1% strain was determined by DMA. The higher the elasticity recovery rate, the better the hair toughness. Each group was measured 5 times and the average value was taken.

[0068] Judgment criteria: Hair cuticle closure rate ≥40% and elasticity recovery rate ≥70% are considered suitable for stubborn and damaged hair.

[0069] The specific test results are shown in Table 6.

[0070] Table 6

[0071] Referring to Table 6, a comparison of experimental data from Examples 1-3 and Comparative Examples 1-5 shows that Examples 1-3 meet the standards for adapting to stubborn hair types in terms of 24-hour cuticle closure rate and elasticity recovery rate for naturally curly and sandy hair. Examples 2-3 show significant advantages, while Example 1's indicators are close to the standard. However, Comparative Examples 1-5 do not meet the standards, indicating the difficulty of adapting traditional silicone oils to stubborn and damaged hair types in the prior art. This invention, through the synergy of exosomes and silicone oil, enables the cuticle closure rate of naturally curly and sandy hair types to meet the adaptation standards, thus improving the adaptability of this invention.

[0072] 6. Compatibility test for fine and soft hair Experimental grouping: 48 strands of fine and soft hair were taken and divided into 8 groups, with 6 strands in each group.

[0073] Treatment method: After completing one simulated washing and care process as in Experiment 3, place it in a constant temperature and humidity chamber at 25℃ and 50% humidity for 24 hours.

[0074] Testing indicators: Hair volume: The volume of hair strands in a naturally hanging state was measured using the volume method. Each group was measured 3 times and the average value was taken. Volume reduction rate = (volume before treatment - volume after treatment) / volume before treatment * 100%.

[0075] Single hair breakage strength: The breakage strength of a single hair is measured using a hair breakage strength meter. A breakage strength improvement rate of ≥10% is considered to have a repair effect.

[0076] Judgment criteria: A decrease in fluffiness of ≤15% and an increase in breaking strength of ≥10% are considered suitable for fine and soft hair. Specific test results are shown in Table 7.

[0077] Table 7

[0078] According to Table 7, Examples 1-3 meet the criteria for being suitable for fine and soft hair, while only Comparative Example 2 meets the criteria for being suitable for fine and soft hair. This is because the linear asparagustrine plant exosomes are nanoscale vesicles with a density close to that of the hair cortex. After application, only a small amount adheres to the hair surface, unlike traditional silicone oils which form a thick film that causes flatness. Simultaneously, the amino acids carried by the linear asparagustrine plant exosomes can replenish the keratin lost from fine and soft hair, improving its breaking strength. This is fundamentally different from plant extracts in existing technologies: small molecule extracts are easily washed away and cannot provide continuous repair; large molecule extracts tend to accumulate on the hair surface, causing fine and soft hair to flatten. Therefore, the nanoscale characteristics of the linear asparagustrine plant exosomes make them suitable for fine and soft hair.

[0079] Based on the test results of Example 2 and Comparative Example 2, and referring to the data in Table 7, Comparative Example 2 is suitable for fine and soft hair in terms of volume and breaking strength. However, due to the lack of silicone oil surface protection, as shown in Table 5, the 24-hour retention rate of active ingredients in Comparative Example 2 is lower, significantly different from Example 2. Furthermore, in the 72-hour follow-up test, as shown in Table 4, the combing strength of the fine and soft hair treated in Comparative Example 2 recovers to 390mN, and the smoothing effect decays significantly over time, failing to meet consumers' needs for long-lasting care. Therefore, it needs to be used in combination with silicone oil. Through the synergistic mechanism of exosome repair and silicone oil protection, both compatibility and durability can be achieved. The above experiments demonstrate that this invention achieves multi-hair type compatibility through the universal repair of exosomes and the flexible film formation of silicone oil, overcoming the shortcomings of the narrow compatibility of existing technologies.

[0080] 7. Screening experiment for optimal compound ratio Variable design: The silicone oil was fixed at XIAMETER™ PMX-200 Silicone Fluid 100 cSt, with five addition gradients: 1%, 2%, 3%, 4%, and 5%. The concentration of the linear asparagus plant exosome stock solution was fixed at 1×10⁻⁶. 11 Five addition gradients were set: 0.02%, 0.05%, 0.075%, 0.1%, and 0.15%. An orthogonal experimental design was used, with a total of 25 compound samples. The auxiliary components (higher fatty alcohols, cationic conditioners, etc.) were fixed according to the ratio in Example 3.

[0081] Testing indicators: 24h cuticle closure rate, 24h combing power, and active ingredient retention rate.

[0082] Screening criteria: 24-hour cuticle closure rate ≥ 50%, 24-hour combing force ≤ 300mN, and active ingredient retention rate ≥ 60% were used as screening conditions. In 25 orthogonal experiments, 17 samples failed to meet the core screening conditions of "24-hour cuticle closure rate ≥ 50%, 24-hour combing force ≤ 300mN, and active ingredient retention rate ≥ 60%", therefore only 8 samples meeting the basic screening conditions are presented.

[0083] The specific test results are shown in Table 8.

[0084] Table 8

[0085] The substandard samples mainly had the following problems: First, insufficient silicone oil addition led to inadequate protection, or insufficient exosome addition led to insufficient repair, ultimately resulting in a 24-hour cuticle closure rate of less than 50%. Second, when the exosome addition was too high, the retention rate of active ingredients did not improve significantly, but the cost increased, which did not meet the cost-effectiveness requirements, further confirming the necessity of the optimal ratio of core components for synergistic compounding.

[0086] As shown in Table 8, the orthogonal experimental data revealed that a total of 8 groups of samples met the screening criteria. Among them, the group with 3% silicone oil and 0.075% exosome mother liquor exhibited the best 24-hour cuticle closure rate, 24-hour combing power, and active ingredient retention rate. Furthermore, the core indicators under this ratio all met the screening criteria. Therefore, it was determined to be the preferred compound ratio of the core components, verifying the rationality of the core component allocation ratio.

[0087] 8. Skin irritation test Experimental method: EpiSkin skin model was used. TM In vitro irritation test: The samples of the examples and comparative examples were applied to the surface of the skin model at a dosage of 0.1 g / tablet, and cultured at 37°C for 48 h. The cell viability of the skin model was then measured.

[0088] Judgment criteria: Cell viability ≥ 50% is considered non-irritating.

[0089] The specific test results are shown in Table 9.

[0090] Table 9

[0091] 9. Long-term safety testing (animal experiments) Experimental subjects: 24 SPF-grade SD rats were divided into 8 groups of 3 rats each.

[0092] Treatment method: Apply the sample at a dose of 100 mg / kg body weight to the hair-removed area on the back of the rat (area 5cm*5cm), apply 3 times a week for 28 consecutive days.

[0093] Detection indicators: Appearance observation: Daily observation of rat skin for abnormalities such as redness, swelling, itching, and desquamation. Pathological sections: After the experiment, skin tissue from the back was taken for HE staining to observe whether the skin tissue morphology was normal.

[0094] Judgment criteria: If there is no abnormal skin reaction and the tissue morphology is normal, it is considered safe for long-term use.

[0095] The specific test results are shown in Table 10.

[0096] Table 10

[0097] Referring to Tables 9 and 10, the cell survival rate of the skin models in Examples 1-3 and Comparative Examples 1-5 was ≥50%, and the rats showed no abnormalities such as redness, swelling, or desquamation after 28 days of long-term application, with normal tissue morphology. This proves that the natural plant exosomes selected in this invention have good biocompatibility with conventional silicone oil, with no risk of irritation or pore blockage, meeting the safety requirements for long-term use. However, the test results of Examples 1-3 and Comparative Example 5 show that although the network-modified amino silicone oil used in Comparative Example 5 has no strongly irritating groups in its molecular structure, and its short-term in vitro irritation and long-term safety meet the standards, its skin model cell survival rate is significantly lower than that of Examples 1-3. This further confirms that the natural plant exosomes selected in this invention have a greater advantage in biocompatibility with conventional silicone oil.

[0098] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0099] It should also be noted that the various specific technical features described in the above embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0100] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A hair care composition with a long-lasting hair-smoothing effect, characterized in that, It comprises the following components by weight percentage: linear asparagine plant exosomes-silicone oil combination 1.05-5.1%; higher fatty alcohols 1-10%; cationic conditioner 0.5-10%; humectant 0.5-10%; balance: purified water; The linear asparagine plant exosome-silicone oil combination comprises 0.05-0.1% linear asparagine plant exosomes and 1-5% silicone oil; the viscosity of the silicone oil is 10-300 cSt.

2. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, The method for preparing the linear asparagus plant exosomes includes the following steps: S1. Select the leaves and stems of linear asparagus plants and wash them with water. Then soak them in 70-75% anhydrous ethanol for 10-20 seconds. After soaking, rinse them several times with sterile deionized water and drain the surface water to obtain the treated leaves and stems. S2. Transfer the treated leaves and stems to a sterile mortar that has been pre-cooled at 2-6°C, and add liquid nitrogen to freeze them until they harden. Keep the mortar at the pre-cooled temperature and grind the treated leaves and stems into powder. Add liquid nitrogen several times during grinding to keep the powder temperature at 2-6°C to obtain linear asparagus powder. S3. Prepare a homogenization buffer pre-cooled to 2-6℃. Use sterile phosphate buffer. Add 0.05-0.15 mL of disodium ethylenediaminetetraacetate, 0.5-2 mL of protease inhibitor cocktail, and 10-50 U of RNase inhibitor to every 100 mL of sterile phosphate buffer. Mix well and cool to 2-6℃ to obtain the homogenization buffer. S4. Mix the linear astragalus powder with 1g of the powder in a sterile environment at a ratio of 6-10mL homogenization buffer. Stir at 2-6℃ and 8000-12000rpm for 4-6 minutes, pausing 2-3 times during the stirring process, each pause for 30 seconds. After stirring until homogenized, a homogenate is obtained. S5. The homogenate was centrifuged for the first time in a sterile environment at a temperature of 2–6°C and a relative centrifugal force of 500–1000 xg for 10–20 min. The supernatant was collected and centrifuged for the second time at a temperature of 2–6°C and a relative centrifugal force of 2000–5000 xg for 30–50 min. The supernatant obtained from the second centrifugation was then subjected to ultracentrifugation at a temperature of 4°C and a relative centrifugal force of 10000–15000 xg for 30–40 min. The supernatant obtained from the ultracentrifugation was collected to obtain the extract. The extract was transferred to an ultracentrifuge tube, and sterile phosphate buffer pre-cooled at 2–6°C was added to 2 / 3 of the volume. The temperature was adjusted to 2–6°C, and the tube was centrifuged at a relative centrifugal force of 100000–150000 xg for 2–4 h. After centrifugation, the supernatant was discarded, and the bottom precipitate was collected to obtain the crude exosome precipitate. S6. Take 1-2 mL of pre-cooled sterile phosphate buffer at 2-6℃ and filter it through a 0.22 μm filter membrane. Then, slowly add the filtered sterile phosphate buffer to an ultracentrifuge tube containing crude exosomes. Gently pipette the crude exosomes while avoiding violent shaking to resuspend them. Transfer the resuspended exosomes to another ultracentrifuge tube and add sterile phosphate buffer to 2 / 3 of the tube's capacity. Adjust the temperature to 2-6℃ and centrifuge at a relative centrifugal force of 100,000-150,000 x g for 1.5-2.5 h. Retain the precipitate at the bottom of the tube and analyze it. Electron microscopy shows a typical cup-shaped or spherical vesicle structure. Nanoparticle tracking analysis shows a particle size of 30-150 nm. Western blotting detects specific exosome marker proteins. After the exosome protein concentration is ≥0.5 mg / mL using the BCA protein quantification method, a high-purity linear asparagine plant exosome precipitate is obtained. S7. Take the high-purity linear asparagine plant exosome precipitate, add an appropriate amount of sterile deionized water, and gently pipette several times until the precipitate is completely dissolved, avoiding the generation of air bubbles. Add sterile deionized water to adjust the concentration of the high-purity linear asparagine plant exosome solution to 1×10⁻⁶. 10 ~1×10 12 The product was obtained by extracting linear asparagus plant exosomes at a concentration of 1 / mL.

3. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, The silicone oil includes at least one of polydimethylsiloxane, cyclodimethylsiloxane, cyclopentadimethylsiloxane, and polymethylphenylsiloxane.

4. The hair care composition with a long-lasting hair-smoothing effect according to claim 3, characterized in that, The polydimethylsiloxane is XIAMETER™ PMX-200 Silicone Fluid 100 cSt.

5. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, The higher fatty alcohols include at least one of lauryl alcohol, tetradecyl alcohol, hexadecyl alcohol, hexadecyl / octadecyl alcohol, and stearyl alcohol.

6. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, The cationic conditioner includes at least one of behenamidopropyl dimethylamine, stearamidopropyl dimethylamine, behenyltrimethylammonium chloride, and cetearyltrimethylammonium chloride.

7. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, The moisturizer includes at least one of glycerin, sorbitol, and propylene glycol.

8. The hair care composition with a long-lasting hair-smoothing effect according to claim 1, characterized in that, It may also include at least one of the following components: 0.05-2.5% thickener; 0.01-2% flavoring agent; 0.01-1.5% preservative; and 0.001-2% pH adjuster.

9. The hair care composition with a long-lasting hair-smoothing effect according to claim 8, characterized in that, The thickener includes at least one of hydroxyethyl cellulose, carbomer, acrylic / C10-30 alkanol acrylate crosspolymer, and acrylate / C10-30 alkanol acrylate crosspolymer.

10. The hair care composition with a long-lasting hair-smoothing effect according to claim 8, characterized in that, The preservative includes at least one of phenoxyethanol, sodium benzoate, benzyl alcohol, benzoic acid, and potassium sorbate.

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