Sensitive skin face moisturizing essence and preparation method thereof

Abstract

This invention discloses a facial moisturizing essence for sensitive skin and its preparation method, belonging to the field of essence technology. It includes: Phase A: lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, and sea buckthorn fruit extract, deionized water, thickener, moisturizer, allantoin, and butylene glycol; Phase B: squalane, silicone oil, emulsifier, skin moisturizer, and vetiver extract; Phase C: antioxidant, preservative, and (daily) fragrance. By adding lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract during the preparation of the essence, the synergistic effect of each component results in excellent moisturizing effects, achieving hydrated skin and improving and repairing sensitive skin problems.

Description

Technical Field

[0001] This invention belongs to the field of serum technology, specifically relating to a facial moisturizing serum for sensitive skin and its preparation method. Background Technology

[0002] As a highly effective skincare product, serums have seen significant advancements in formulation design and preparation technology in recent years. Currently, the main types of serums on the market include lotion and water-based products. These products play an important role in moisturizing, anti-oxidation, and anti-aging, greatly satisfying users with different skin types and needs.

[0003] Sensitive skin is a sub-healthy state in which the skin's natural barrier is damaged, its self-defense ability is reduced, allowing external irritants to easily penetrate, increasing the transmission of sensory nerve signals and lowering the tolerance threshold. This leads to an overreaction to even mild external stimuli, activating the skin's immune response, causing vasodilation and the release of inflammatory factors. Subjective symptoms such as burning, stinging, itching, and tightness may occur, accompanied by objective signs such as erythema, scaling, and telangiectasia, or without these symptoms. In recent years, to improve the efficacy of skincare products, serums often contain various chemical additives, such as emollients, moisturizers, and skin conditioning agents. These irritating additives can further burden the skin of people with sensitive skin, exacerbating symptoms. Therefore, the development of skincare products specifically designed for sensitive skin has become an urgent technical challenge. Summary of the Invention

[0004] The purpose of this invention is to provide a facial moisturizing essence for sensitive skin and its preparation method, which can improve the skin conditioning effect for people with sensitive skin.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A facial moisturizing serum for sensitive skin, comprising:

[0007] Phase A: Litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol;

[0008] Phase B: Squalane, silicone oil, emulsifiers, emollients, and vetiver extract;

[0009] Phase C: Antioxidants, preservatives, and (daily) fragrances.

[0010] As a preferred embodiment of the present invention, in phase A, the mass ratio of the litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, humectant, allantoin, and butylene glycol is 1.2-2.4:1.8-3.6:1.4-1.8:1.2-1.4:1.8-2.2:1.8-2.6:74.7-81.9:0.3-0.4:0.4-0.6:0.2-0.3:8-10.

[0011] As a preferred embodiment of the present invention, in phase B, the mass ratio of squalane, silicone oil, emulsifier, emollient and vetiver extract is 0.7-0.9:0.4-0.5:0.02-0.04:0.04-0.06:1.2-1.4.

[0012] As a preferred embodiment of the present invention, in phase C, the mass ratio of the antioxidant, preservative and (daily) fragrance is 3-7:1-3:2-4.

[0013] As a preferred embodiment of the present invention, the method for preparing the litchi seed extract includes the following steps:

[0014] Peel and remove the pulp from fresh lychees to obtain lychee seeds. After cleaning, crush the seeds and pass them through an 80-mesh sieve to obtain seed powder. Add the powder to deionized water and adjust the pH to 4.5 with an acid solution. Add surfactant and cellulase, stir at 45℃ for 40-80 minutes, and then reflux at 80℃ for 2 hours with stirring. Concentrate the powder to 10 mL using a rotary evaporator. Add 80 mL of 75% ethanol solution, seal and let stand for 24 hours. Filter the powder, wash the filter cake three times with 75% ethanol solution, and evaporate the ethanol in a 65℃ water bath to obtain the lychee seed extract.

[0015] The surfactant is selected from any one of Tween-80, sodium lauryl sulfate, and glyceryl monostearate.

[0016] The ratio of nuclear powder, deionized water, surfactant and cellulase is 15g:200mL:0.4g:300000U;

[0017] As a preferred embodiment of the present invention, the method for preparing the giant salamander collagen freeze-dried powder includes the following steps:

[0018] Healthy, artificially bred giant salamanders were selected, and skin tissue was obtained. Excess muscle tissue and pigment were removed. The tissue was then washed with deionized water, air-dried, and weighed. Next, it was cut into 2×2cm pieces. The air-dried pieces were added to a clean 2L beaker, and anhydrous diethyl ether was added to achieve a material-to-liquid ratio of 1:10 (g / mL). The beaker was sealed with plastic wrap and magnetically stirred for 24 hours for the first defatting. After this initial defatting, the mixture was filtered, and the solid phase was retained. After the residual solvent had evaporated completely, 10% n-butanol was added to achieve a material-to-liquid ratio of 1:10 (g / mL). The beaker was then sealed with plastic wrap and magnetically stirred for 24 hours for the second defatting. After this second defatting, the mixture was filtered, and the solid phase was retained. Wash with deionized water until neutral, air dry, then add 0.1 mol / L sodium hydroxide solution to make the solid-liquid ratio 1:20 (g / mL). Remove impurities and proteins by sealing the beaker with plastic wrap and magnetically stirring for 24 hours, changing the solvent every 8 hours. Separate the solid phase, wash with deionized water until neutral, drain, and air dry. Once the surface is dry, perform initial acid extraction by adding 0.5 mol / L acetic acid solution to make the solid-liquid ratio 1:60 (g / mL), magnetically stirring for 24 hours. Filter, add sodium chloride to the filtrate until the sodium chloride concentration is 2.5 mol / L, and salt out for 12 hours. Filter, retain the precipitate, and... The obtained precipitate was dissolved in 0.1 mol / L acetic acid, and the solution was then filled into dialysis bags and placed in large beakers for dialysis. Dialysis was first performed with 0.1 mol / L acetic acid, with the solvent changed every 8 hours until chloride ions were removed (tested with AgNO3 solution). Then, dialysis was performed with ultrapure water, with the solvent changed every 8 hours, until the dialysate was neutral (tested with pH paper). The dialyzed collagen was poured into a petri dish, sealed with plastic wrap, and several small holes were poked. It was pre-frozen at -18°C for 24 hours. The pre-frozen collagen was then freeze-dried at -45°C for 20 hours. The freeze-dried crude extract was then... The collagen was dissolved in 0.2 mol / L acetic acid solution to prepare a 0.5% collagen solution. Neutral protease was added to the collagen solution for enzymatic hydrolysis. The hydrolysis conditions were: hydrolysis time 5 h, temperature 45 °C, pH 6.8, enzyme dosage 5000 U / g, and material-to-liquid ratio 1:10 (g / mL). After hydrolysis, the reaction solution was heated in a 90 °C water bath for 10 min to inactivate the enzyme activity. The hydrolysate after enzyme inactivation was centrifuged, the supernatant was collected, and filtered through a 0.45 μm filter membrane. The filtered solution was purified by dialyzing for 10 h and then transferred to a freeze dryer and freeze-dried at -45 °C to obtain the giant salamander collagen freeze-dried powder.

[0019] As a preferred embodiment of the present invention, the preparation method of the black chokeberry extract includes the following steps:

[0020] Take fresh black chokeberry fruit, rinse it three times with deionized water, drain the surface water and cut it into 1-2cm small pieces. Place it in a freeze dryer (-50℃, vacuum degree 10Pa) and freeze dry for 24 hours until completely dry (moisture content ≤5%). Crush the dried fruit, pass it through a 40-mesh sieve, collect the sieved powder, put it into a sealed bag and place it in a desiccator for later use.

[0021] Take a qualitative filter paper (12cm in diameter), weigh 10g of dried black chokeberry powder and place it in the center. Fold it into a cylindrical filter paper packet (the height should be less than 2 / 3 of the height of the Soxhlet extractor tube). Tie the open end tightly with cotton thread, mark the sample information, add 100mL of diethyl ether (analytical grade) to a 250mL round-bottom flask, place the filter paper packet into the extraction tube, ensuring that the filter paper packet is completely immersed in the diethyl ether, connect the extraction tube and the spherical condenser in sequence, and circulate cooling water through the condenser. Place the apparatus in a constant temperature water bath, set the temperature to 54℃, and extract for 5 hours. After extraction, remove the filter paper packet and let it air dry naturally until there is no ether odor. Place the dried filter paper packet into a 500mL three-necked flask, and add the liquid to the solid at a ratio of 1:40 (g / mL). Add 400 mL of deionized water preheated to 77 °C and extract for 60 min. After extraction, pour the hot mixture into a funnel and filter using a vacuum pump. Collect the filtrate into a 500 mL beaker. Rinse the inner wall of the three-necked flask and the filter paper pack with 50 mL of 77 °C hot water. Add the washings to the filtrate. Put the filter residue (along with the filter paper pack) back into the three-necked flask. Add 400 mL of 77 °C hot water at the same liquid-to-solid ratio and repeat the extraction and filtration steps. Collect the second filtrate. Combine the two filtrates and transfer them to a 1 L beaker. Stir well with a glass rod. Transfer the combined filtrate to a 500 mL evaporation flask of a rotary evaporator. Set the parameters as follows: water bath temperature 55 °C, rotation speed 60 r / min, vacuum degree 0.0.09 MPa, concentrate to a volume of 200 mL. After concentration, transfer the concentrate to a 250 mL beaker, rinse the evaporating flask with a small amount of deionized water, and add the washings to the beaker (total 210 mL). Measure 630 mL of 93% ethanol solution (3 times the volume of the concentrate), pre-cool it in a 4°C refrigerator for 30 min, and slowly add the pre-cooled 93% ethanol solution dropwise to the concentrate while magnetically stirring. After the addition is complete, continue stirring for 10 min to ensure the solution is thoroughly mixed. Transfer the mixture to a 500 mL beaker. Seal the mouth of a stoppered conical flask and place it in a 4°C refrigerator overnight to allow the polysaccharides to fully precipitate. Aliquot the mixture into 50mL centrifuge tubes and centrifuge, retaining the precipitate at the bottom of the tube. Add 20mL of 93% ethanol solution to each centrifuge tube and gently stir with a glass rod to disperse the precipitate. Sonicate for 2 minutes (300W). Repeat the centrifugation process 2-3 times until the supernatant is colorless. Replace the ethanol with 20mL of diethyl ether (analytical grade) and repeat the dispersion-sonication-centrifugation steps 2-3 times to remove residual lipids. After centrifugation for the last time, transfer the precipitate to a petri dish and air-dry it in a fume hood for 30 minutes until no ether odor remains. Weigh the dried precipitate and add it to 80℃ deionized water at a solid-liquid ratio of 1:20 (g / mL). Stir magnetically for 30 minutes to obtain a polysaccharide solution. Transfer the solution to a 250mL separatory funnel and add a mixture of chloroform and n-butanol at a volume ratio of 4:1 (1 / 5 the volume of the polysaccharide solution). Tighten the stopper of the separatory funnel and invert it for 5 minutes. Then place it on a reciprocating shaker and set the speed to 180 rpm. Shake for 30 minutes, remove the separatory funnel, and let stand for 30 minutes until the layers are clearly separated (upper layer is aqueous phase containing polysaccharides; middle layer is protein layer; lower layer is organic phase). Slowly open the stopcock, retaining the upper aqueous phase. Repeat the above operation (adding the mixture - shaking - standing - separating) 5 times until the middle protein layer disappears. Transfer the deproteinized aqueous phase to a pre-treated dialysis bag (MD44-10000 dialysis bag, molecular weight cutoff 10000 Da, cut into 20 cm long segments, and add 0.5 mol / L EDTA solution (pH 10.5). Boil the polysaccharide solution in water (8.0) for 10 minutes, then boil it in deionized water for another 10 minutes. After cooling, soak it in deionized water for later use. Tie both ends tightly with cotton thread (leaving 1 / 3 space to prevent expansion and breakage). Place it in a 5L beaker, add 4L of deionized water (the liquid level should cover the dialysis bag), and stir slowly with a magnetic stirrer (50 rpm). Dialyze in a 4℃ refrigerator for 12 hours, changing the deionized water every 4 hours. After dialysis, transfer the polysaccharide solution in the dialysis bag to a lyophilization bottle and pre-freeze it in an ultra-low temperature freezer at -80℃ for 4 hours until completely frozen. Transfer it to a freeze dryer and set the parameters: vacuum degree 10Pa, cold trap temperature -55℃. Freeze-dry for 24 hours until the sample is in a loose powder state. Take out the freeze-dried powder, grind it gently with a mortar and pestle, and pass it through an 80-mesh sieve to obtain the black chokeberry extract.

[0022] As a preferred embodiment of the present invention, the preparation method of the lentil seed extract includes the following steps:

[0023] Take the cleaned and dried lentil seeds, crush them, pass them through an 80-mesh sieve, collect 10g of the sieved powder, place it in a 250mL round-bottom flask, add 70% ethanol solution at a material-to-liquid ratio of 1:15 (g / mL), reflux extract three times in a water bath at 78℃, with each extraction lasting 2 hours. After extraction, cool to room temperature, pre-filter with double-layer gauze, and then filter through a 0.45μm microporous membrane. Collect the filtrate, concentrate it to 1 / 5 of the original volume in a rotary evaporator, and freeze-dry at -45℃ for 24 hours to obtain the lentil seed extract.

[0024] As a preferred embodiment of the present invention, the preparation method of the short-petaled golden lotus extract includes the following steps:

[0025] Take short-petaled golden lotus (retaining complete petals and sepals), wash, dry, and crush. Sieve through an 80-mesh sieve, collect 10g of the sieved powder, and place it in a 2L stoppered conical flask. Add 60% ethanol solution at a material-to-liquid ratio of 1:30 (g / mL), stir well, and place in a constant temperature water bath shaker (set temperature 60℃, rotation speed 180r / min, extraction time 140min) for extraction. After extraction, filter under normal pressure using double-layer qualitative filter paper, collect the filtrate into a 500mL beaker, and rinse the inner wall of the conical flask and the filter residue with 20mL of 60% ethanol solution. Add the washing liquid to the filtrate, start a rotary evaporator to concentrate under reduced pressure (water bath temperature 45℃, vacuum degree 0.09MPa, rotation speed 50r / min), concentrate to 1 / 5 of the original volume, stop concentration, and transfer the concentrate to a vacuum drying oven (set temperature 50℃, vacuum degree 0.09MPa) to dry for 6h to obtain crude extract of short-petaled golden lotus.

[0026] Take 50g of macroporous adsorption resin AB-8, put it into a 500mL beaker, add 200mL of 95% ethanol solution, and soak for 24h; then wash three times with 95% ethanol solution under reduced pressure until the eluent is clear after dilution with deionized water; then soak in 5% hydrochloric acid solution for 2h, filter, and wash with deionized water until pH neutral; finally soak in 5% sodium hydroxide solution for 2h, filter, and wash with deionized water until pH neutral to obtain the pretreated macroporous adsorption resin for later use;

[0027] The pretreated AB-8 resin was packed into a glass chromatography column (2.5 cm in diameter and 30 cm in height) using a wet packing method, with the column height controlled at 20 cm. The resin column was then flushed with an acetate-sodium acetate buffer solution at pH 4.0 (prepared by mixing 0.1 mol / L acetic acid solution and 0.1 mol / L sodium acetate solution at a volume ratio of 15:1 and calibrating with a pH meter) at a flow rate of 5 mL / min until the pH of the effluent stabilized at 4.0, thus completing the equilibration process.

[0028] Weigh 1g of crude extract from *Trollius chinensis* (short-petaled lotus) and add it to 100mL of acetate-sodium acetate buffer solution (pH 4.0). Stir magnetically for 30min to obtain the loading solution. Pump the loading solution into the chromatography column at a constant flow rate of 10mL / min using a constant flow pump. During the loading process, collect 5mL of eluent every 10min. When the target spot (consistent with the reference standard) appears in the eluent using thin-layer chromatography (TLC), stop the loading. After loading, rinse the chromatography column with deionized water at a flow rate of 10mL / min until the eluent is colorless and transparent to remove unadsorbed water-soluble impurities. Discard this portion of the eluent and elute with 50% ethanol solution at a flow rate of 8mL / min, collecting the eluent in fractions. Collect 1 portion of each 20 mL eluent, combine the effective eluents, and transfer the combined effective eluents to a 500 mL rotary evaporator. Start the rotary evaporator and set the parameters: water bath temperature 45℃, vacuum degree 0.08 MPa, rotation speed 55 r / min. Concentrate to a volume of 30 mL. After concentration, rinse the inner wall of the evaporator with a small amount of deionized water (5 mL). Combine the concentrates to a 50 mL lyophilization bottle and place it in an ultra-low temperature freezer at -80℃. Let it stand for 5 hours until the concentrate is completely frozen. Transfer the pre-frozen lyophilization bottle to a freeze dryer and freeze-dry for 24 hours at a cold trap temperature of -55℃ and a vacuum degree of 10 Pa. Take out the lyophilized powder, grind it, and pass it through an 80-mesh sieve to obtain the short-petaled golden lotus extract.

[0029] As a preferred embodiment of the present invention, the preparation method of the *Prickly pear* fruit extract includes the following steps:

[0030] Collect the residue after pressing oil from the prickly pear fruit, remove the shells, impurities, and unpressed kernel lumps, retaining the loose seed meal fragments. Dry the residue in a 50℃ forced-air drying oven for 5 hours (moisture content reduced to ≤8%), pulverize, pass through an 80-mesh sieve, collect 100g of the sieved powder, and pour it into a 2L microwave extraction beaker. Add deionized water at a material-to-liquid ratio of 1:10 (g / mL), and microwave treat (set microwave power to 250W, magnetic stirring speed to 200r / min, total microwave time to 60min). Transfer the microwave-treated mixture to a 2L round-bottom flask. Connect the reflux condenser, and connect the upper end of the condenser to the vacuum line (connected to the vacuum pump) and the thermometer interface. Place the flask in a constant temperature water bath, adjust the vacuum to 0.05 MPa and the water bath temperature to 40℃, and extract for 90 min. After extraction, filter the flask while it is still hot through a 200-mesh filter cloth, collect the filtrate into a 1L beaker, wash the filter residue twice with 50 mL of 40℃ distilled water, and add the washing liquid to the filtrate. Start the rotary evaporator (water bath temperature 45℃, vacuum 0.08 MPa, rotation speed 60 r / min), and stop when the volume is concentrated to 1 / 4 of the original volume to obtain the concentrated solution.

[0031] The concentrate was placed in a 5L beaker. Under magnetic stirring, a 95% ethanol solution was added dropwise to the concentrate at a rate of 140 mL / min using a constant flow pump. After the addition was complete, stirring was continued for 10 min. The solution was then placed in a 4℃ refrigerator and allowed to stand for 2 h. The solution was then filtered under reduced pressure (0.06 MPa) using a 200-mesh filter cloth. The filter cake was collected, transferred to a freeze-drying bottle, and pre-frozen in an ultra-low temperature freezer at -80℃ for 4 h. The solution was then transferred to a freeze dryer and freeze-dried for 24 h at a cold trap temperature of -55℃ and a vacuum of 10 Pa. The solution was then ground and passed through an 80-mesh sieve to obtain the *Cyprinus coccinea* extract.

[0032] As a preferred embodiment of the present invention, the method for preparing the vetiver extract includes the following steps:

[0033] Select fresh vetiver roots, wash, dry, crush, pass through a 20-mesh sieve, and collect the powder that passes through the sieve.

[0034] Add 500 mL of deionized water to a 1000 mL round-bottom flask, connect a distillation stand with a sieve plate (5 mm aperture), and evenly spread 300 g of vetiver root powder on the sieve plate. Cover the top with a layer of absorbent cotton. Connect the condenser and the tail tube in sequence, inserting the end of the tail tube into a separatory funnel. Ensure the entire apparatus is sealed. After the water in the flask boils and produces stable steam, adjust the heating power to stabilize the steam generation rate (the distillate dripping rate at the condenser outlet should be 1-2 drops / second). Distill for 5 hours, then stop distillation and transfer the distillate to a container. The oil was transferred to a separatory funnel and allowed to stand for 30 minutes until the oil-water interface became clear. The lower layer of crude essential oil was then slowly released. The crude essential oil was transferred to an Erlenmeyer flask, and anhydrous sodium sulfate (10% of the essential oil mass) was added. The flask was sealed and placed on a shaker for 30 minutes. The dehydrated essential oil was filtered through qualitative filter paper to remove the anhydrous sodium sulfate particles, resulting in a pre-purified essential oil. The pre-purified essential oil was then placed in a -5°C freezer for 24 hours to allow the wax crystals to precipitate. The filtrate was then collected using a Buchner funnel pre-cooled to 0°C to obtain the vetiver extract.

[0035] As a preferred embodiment of the present invention, the thickener is selected from at least one of xanthan gum, carbomer, and hydroxyethyl cellulose.

[0036] As a preferred embodiment of the present invention, the moisturizer is selected from at least one of sodium hyaluronate and 1,2-hexanediol.

[0037] As a preferred embodiment of the present invention, the emulsifier is selected from at least one of PEG-10 polydimethylsiloxane and PEG-3 polydimethylsiloxane.

[0038] As a preferred embodiment of the present invention, the emollient is selected from at least one of ethylhexylglycerin, cetearyl stearate, and cetearyl palmitate.

[0039] The preparation method of the above-mentioned facial moisturizing serum for sensitive skin includes the following steps:

[0040] S1. Take lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol, heat to 40-50℃, stir for 8-10 minutes to obtain phase A.

[0041] S2. Mix squalane, silicone oil, emulsifier, emollient, and vetiver extract, heat to 70-80℃, and stir for 5-10 minutes to obtain phase B;

[0042] S3. Add phase B to phase A, and homogenize and stir at 8000-12000 r / min for 5-10 min at 45°C. Add phase C and homogenize and stir at 8000 r / min for 3-5 min to obtain the sensitive skin facial moisturizing essence.

[0043] As a preferred embodiment of the present invention, the mass ratio of phase A, phase B, and phase C is 73-79:21-27:0.3-0.5.

[0044] As a preferred embodiment of the present invention, the antioxidant is selected from at least one of tocopherol acetate and 3-o-ethyl ascorbic acid.

[0045] As a preferred embodiment of the present invention, the preservative is potassium sorbate.

[0046] The beneficial effects of this invention are:

[0047] This invention incorporates lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract into the preparation of the essence. Through the synergistic effect of these components, it achieves excellent moisturizing effects, resulting in hydrated skin. It also reduces the content of chemical additives and introduces a variety of natural extracts that are more compatible with human skin to improve and repair sensitive skin problems. Detailed Implementation

[0048] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0049] Preparation Example 1

[0050] The preparation method of litchi seed extract includes the following steps:

[0051] Peel and remove the pulp from fresh lychees to obtain lychee seeds. After cleaning, crush the seeds and pass them through an 80-mesh sieve to obtain seed powder. Add the powder to deionized water and adjust the pH to 4.5 with an acid solution. Add surfactant and cellulase, stir at 45℃ for 60 min, and then reflux at 80℃ for 2 h with stirring. Concentrate the powder to 10 mL using a rotary evaporator. Add 80 mL of 75% ethanol solution, seal and let stand for 24 h. Filter the powder, wash the filter cake three times with 75% ethanol solution, and evaporate the ethanol in a 65℃ water bath to obtain the lychee seed extract.

[0052] The surfactant is sodium dodecyl sulfate;

[0053] The ratio of nuclear powder, deionized water, surfactant and cellulase is 15g:200mL:0.4g:300000U.

[0054] Preparation Example 2

[0055] The preparation method of giant salamander collagen freeze-dried powder includes the following steps:

[0056] Healthy, artificially bred giant salamanders were selected, and skin tissue was obtained. Excess muscle tissue and pigment were removed. The tissue was then washed with deionized water, air-dried, and weighed. Next, it was cut into 2×2cm pieces. The air-dried pieces were added to a clean 2L beaker, and anhydrous diethyl ether was added to achieve a material-to-liquid ratio of 1:10 (g / mL). The beaker was sealed with plastic wrap and magnetically stirred for 24 hours for the first defatting. After this initial defatting, the mixture was filtered, and the solid phase was retained. After the residual solvent had evaporated completely, 10% n-butanol was added to achieve a material-to-liquid ratio of 1:10 (g / mL). The beaker was then sealed with plastic wrap and magnetically stirred for 24 hours for the second defatting. After this second defatting, the mixture was filtered, and the solid phase was retained. Wash with deionized water until neutral, air dry, then add 0.1 mol / L sodium hydroxide solution to make the solid-liquid ratio 1:20 (g / mL). Remove impurities and proteins by sealing the beaker with plastic wrap and magnetically stirring for 24 hours, changing the solvent every 8 hours. Separate the solid phase, wash with deionized water until neutral, drain, and air dry. Once the surface is dry, perform initial acid extraction by adding 0.5 mol / L acetic acid solution to make the solid-liquid ratio 1:60 (g / mL), magnetically stirring for 24 hours. Filter, add sodium chloride to the filtrate until the sodium chloride concentration is 2.5 mol / L, and salt out for 12 hours. Filter, retain the precipitate, and... The obtained precipitate was dissolved in 0.1 mol / L acetic acid, and the solution was then filled into dialysis bags and placed in large beakers for dialysis. Dialysis was first performed with 0.1 mol / L acetic acid, with the solvent changed every 8 hours until chloride ions were removed (tested with AgNO3 solution). Then, dialysis was performed with ultrapure water, with the solvent changed every 8 hours, until the dialysate was neutral (tested with pH paper). The dialyzed collagen was poured into a petri dish, sealed with plastic wrap, and several small holes were poked. It was pre-frozen at -18°C for 24 hours. The pre-frozen collagen was then freeze-dried at -45°C for 20 hours. The freeze-dried crude extract was then... The collagen was dissolved in 0.2 mol / L acetic acid solution to prepare a 0.5% collagen solution. Neutral protease was added to the collagen solution for enzymatic hydrolysis under the following conditions: hydrolysis time 5 h, temperature 45 °C, pH 6.8, enzyme dosage 5000 U / g, and material-to-liquid ratio 1:10 (g / mL). After hydrolysis, the reaction solution was heated in a 90 °C water bath for 10 min to inactivate the enzyme activity. The hydrolysate was centrifuged, the supernatant was collected, and filtered through a 0.45 μm filter membrane. The filtered solution was purified by dialyzing for 10 h and then transferred to a freeze dryer for freeze drying at -45 °C to obtain the giant salamander collagen freeze-dried powder.

[0057] Preparation Example 3

[0058] The preparation method of black chokeberry extract includes the following steps:

[0059] Take fresh black chokeberry fruit, rinse it three times with deionized water, drain the surface water and cut it into 1-2cm small pieces. Place it in a freeze dryer (-50℃, vacuum degree 10Pa) and freeze dry for 24 hours until completely dry (moisture content ≤5%). Crush the dried fruit, pass it through a 40-mesh sieve, collect the sieved powder, put it into a sealed bag and place it in a desiccator for later use.

[0060] Take a qualitative filter paper (12cm in diameter), weigh 10g of dried black chokeberry powder and place it in the center. Fold it into a cylindrical filter paper packet (the height should be less than 2 / 3 of the height of the Soxhlet extractor tube). Tie the open end tightly with cotton thread, mark the sample information, add 100mL of diethyl ether (analytical grade) to a 250mL round-bottom flask, place the filter paper packet into the extraction tube, ensuring that the filter paper packet is completely immersed in the diethyl ether, connect the extraction tube and the spherical condenser in sequence, and circulate cooling water through the condenser. Place the apparatus in a constant temperature water bath, set the temperature to 54℃, and extract for 5 hours. After extraction, remove the filter paper packet and let it air dry naturally until there is no ether odor. Place the dried filter paper packet into a 500mL three-necked flask, and add the liquid to the solid at a ratio of 1:40 (g / mL). Add 400 mL of deionized water preheated to 77 °C and extract for 60 min. After extraction, pour the hot mixture into a funnel and filter using a vacuum pump. Collect the filtrate into a 500 mL beaker. Rinse the inner wall of the three-necked flask and the filter paper pack with 50 mL of 77 °C hot water. Add the washings to the filtrate. Put the filter residue (along with the filter paper pack) back into the three-necked flask. Add 400 mL of 77 °C hot water at the same liquid-to-solid ratio and repeat the extraction and filtration steps. Collect the second filtrate. Combine the two filtrates and transfer them to a 1 L beaker. Stir well with a glass rod. Transfer the combined filtrate to a 500 mL evaporation flask of a rotary evaporator. Set the parameters as follows: water bath temperature 55 °C, rotation speed 60 r / min, vacuum degree 0.0.09 MPa, concentrate to a volume of 200 mL. After concentration, transfer the concentrate to a 250 mL beaker, rinse the evaporating flask with a small amount of deionized water, and add the washings to the beaker (total 210 mL). Measure 630 mL of 93% ethanol solution (3 times the volume of the concentrate), pre-cool it in a 4°C refrigerator for 30 min, and slowly add the pre-cooled 93% ethanol solution dropwise to the concentrate while magnetically stirring. After the addition is complete, continue stirring for 10 min to ensure the solution is thoroughly mixed. Transfer the mixture to a 500 mL beaker. Seal the mouth of a stoppered conical flask and place it in a refrigerator at 4°C overnight to allow the polysaccharides to fully precipitate. Aliquot the mixture into 50mL centrifuge tubes, centrifuge, and retain the precipitate at the bottom of the tube. Add 20mL of 93% ethanol solution to each centrifuge tube, gently stir with a glass rod to disperse the precipitate, and sonicate for 2 minutes (300W). Repeat the centrifugation process 3 times until the supernatant is colorless. Replace the ethanol with 20mL of diethyl ether (analytical grade), and repeat the dispersion-sonication-centrifugation steps 2-3 times to remove residual lipids. To remove impurities, after the final centrifugation, transfer the precipitate to a petri dish and air-dry it in a fume hood for 30 minutes until no ether odor remains. Weigh the dried precipitate and add it to 80℃ deionized water at a solid-liquid ratio of 1:20 (g / mL). Stir magnetically for 30 minutes to obtain a polysaccharide solution. Transfer the solution to a 250mL separatory funnel and add a mixture of chloroform and n-butanol at a volume ratio of 4:1 (1 / 5 the volume of the polysaccharide solution). Tighten the stopper of the separatory funnel and invert it for 5 minutes. Then place it on a reciprocating shaker and set the speed to 180 rpm. Shake for 30 minutes, remove the separatory funnel, and let stand for 30 minutes until the layers are clearly separated (upper layer is aqueous phase containing polysaccharides; middle layer is protein layer; lower layer is organic phase). Slowly open the stopcock, retaining the upper aqueous phase. Repeat the above operation (adding the mixture - shaking - standing - separating) 5 times until the middle protein layer disappears. Transfer the deproteinized aqueous phase to a pre-treated dialysis bag (MD44-10000 dialysis bag, molecular weight cutoff 10000 Da, cut into 20 cm long segments, and add 0.5 mol / L EDTA solution (pH 10.5). Boil the polysaccharide solution in water (8.0) for 10 minutes, then boil it in deionized water for another 10 minutes. After cooling, soak it in deionized water for later use. Tie both ends tightly with cotton thread (leaving 1 / 3 space to prevent expansion and breakage). Place it in a 5L beaker, add 4L of deionized water (the liquid level should cover the dialysis bag), and stir slowly with a magnetic stirrer (50 rpm). Dialyze in a 4℃ freezer for 12 hours, changing the deionized water every 4 hours. After dialysis, transfer the polysaccharide solution from the dialysis bag to a lyophilization bottle and pre-freeze it in a -80℃ ultra-low temperature freezer for 4 hours until completely frozen. Transfer it to a freeze dryer and set the parameters: vacuum degree 10Pa, cold trap temperature -55℃. Freeze-dry for 24 hours until the sample is a loose powder. Take out the freeze-dried powder, grind it gently with a mortar and pestle, and pass it through an 80-mesh sieve to obtain the black chokeberry extract.

[0061] Preparation Example 4

[0062] The preparation method of lentil seed extract includes the following steps:

[0063] Take the cleaned and dried lentil seeds, crush them, pass them through an 80-mesh sieve, collect 10g of the sieved powder, place it in a 250mL round-bottom flask, add 70% ethanol solution at a material-to-liquid ratio of 1:15 (g / mL), reflux extract three times in a water bath at 78℃, with each extraction lasting 2 hours. After extraction, cool to room temperature, pre-filter with double-layer gauze, and then filter through a 0.45μm microporous membrane. Collect the filtrate, concentrate it to 1 / 5 of its original volume in a rotary evaporator, and freeze-dry at -45℃ for 24 hours to obtain the lentil seed extract.

[0064] Preparation Example 5

[0065] The preparation method of the extract of short-petaled golden lotus includes the following steps:

[0066] Take short-petaled golden lotus (retaining complete petals and sepals), wash, dry, and crush. Sieve through an 80-mesh sieve, collect 10g of the sieved powder, and place it in a 2L stoppered conical flask. Add 60% ethanol solution at a material-to-liquid ratio of 1:30 (g / mL), stir well, and place in a constant temperature water bath shaker (set temperature 60℃, rotation speed 180r / min, extraction time 140min) for extraction. After extraction, filter under normal pressure using double-layer qualitative filter paper, collect the filtrate into a 500mL beaker, and rinse the inner wall of the conical flask and the filter residue with 20mL of 60% ethanol solution. Add the washing liquid to the filtrate, start a rotary evaporator to concentrate under reduced pressure (water bath temperature 45℃, vacuum degree 0.09MPa, rotation speed 50r / min), concentrate to 1 / 5 of the original volume, stop concentration, and transfer the concentrate to a vacuum drying oven (set temperature 50℃, vacuum degree 0.09MPa) to dry for 6h to obtain crude extract of short-petaled golden lotus.

[0067] Take 50g of macroporous adsorption resin AB-8, put it into a 500mL beaker, add 200mL of 95% ethanol solution, and soak for 24h; then wash three times with 95% ethanol solution under reduced pressure until the eluent is clear after dilution with deionized water; then soak in 5% hydrochloric acid solution for 2h, filter, and wash with deionized water until pH neutral; finally soak in 5% sodium hydroxide solution for 2h, filter, and wash with deionized water until pH neutral to obtain the pretreated macroporous adsorption resin for later use;

[0068] The pretreated AB-8 resin was packed into a glass chromatography column (2.5 cm in diameter and 30 cm in height) using a wet packing method, with the column height controlled at 20 cm. The resin column was then flushed with an acetate-sodium acetate buffer solution at pH 4.0 (prepared by mixing 0.1 mol / L acetic acid solution and 0.1 mol / L sodium acetate solution at a volume ratio of 15:1 and calibrating with a pH meter) at a flow rate of 5 mL / min until the pH of the effluent stabilized at 4.0, thus completing the equilibration process.

[0069] Weigh 1g of crude extract from *Trollius chinensis* (short-petaled lotus) and add it to 100mL of acetate-sodium acetate buffer solution (pH 4.0). Stir magnetically for 30min to obtain the loading solution. Pump the loading solution into the chromatography column at a constant flow rate of 10mL / min using a constant flow pump. During the loading process, collect 5mL of eluent every 10min. When the target spot (consistent with the reference standard) appears in the eluent using thin-layer chromatography (TLC), stop the loading. After loading, rinse the chromatography column with deionized water at a flow rate of 10mL / min until the eluent is colorless and transparent to remove unadsorbed water-soluble impurities. Discard this portion of the eluent and elute with 50% ethanol solution at a flow rate of 8mL / min, collecting the eluent in fractions. Collect 1 portion of each 20 mL eluent, combine the effective eluents, and transfer the combined effective eluents to a 500 mL rotary evaporator. Start the rotary evaporator and set the parameters: water bath temperature 45℃, vacuum degree 0.08 MPa, rotation speed 55 r / min. Concentrate to a volume of 30 mL. After concentration, rinse the inner wall of the evaporator with a small amount of deionized water (5 mL). Combine the concentrates to a 50 mL lyophilization bottle and place it in an ultra-low temperature freezer at -80℃. Let it stand for 5 hours until the concentrate is completely frozen. Transfer the pre-frozen lyophilization bottle to a freeze dryer and freeze-dry for 24 hours at a cold trap temperature of -55℃ and a vacuum degree of 10 Pa. Take out the lyophilized powder, grind it, and pass it through an 80-mesh sieve to obtain the short-petaled golden lotus extract.

[0070] Preparation Example 6

[0071] The preparation method of the extract of sea buckthorn fruit includes the following steps:

[0072] Collect the residue after pressing oil from the prickly pear fruit, remove the shells, impurities, and unpressed kernel lumps, retaining the loose seed meal fragments. Dry the residue in a 50℃ forced-air drying oven for 5 hours (moisture content reduced to ≤8%), pulverize, pass through an 80-mesh sieve, collect 100g of the sieved powder, and pour it into a 2L microwave extraction beaker. Add deionized water at a material-to-liquid ratio of 1:10 (g / mL), and microwave treat (set microwave power to 250W, magnetic stirring speed to 200r / min, total microwave time to 60min). Transfer the microwave-treated mixture to a 2L round-bottom flask. Connect the reflux condenser, and connect the upper end of the condenser to the vacuum line (connected to the vacuum pump) and the thermometer interface. Place the flask in a constant temperature water bath, adjust the vacuum to 0.05 MPa and the water bath temperature to 40℃, and extract for 90 min. After extraction, filter the flask while it is still hot through a 200-mesh filter cloth, collect the filtrate into a 1L beaker, wash the filter residue twice with 50 mL of 40℃ distilled water, and add the washing liquid to the filtrate. Start the rotary evaporator (water bath temperature 45℃, vacuum 0.08 MPa, rotation speed 60 r / min), and stop when the volume is concentrated to 1 / 4 of the original volume to obtain the concentrated solution.

[0073] The concentrate was placed in a 5L beaker. Under magnetic stirring, a 95% ethanol solution was added dropwise to the concentrate at a rate of 140 mL / min using a constant flow pump. After the addition was complete, stirring was continued for 10 min. The mixture was then placed in a 4℃ refrigerator and allowed to stand for 2 h. The mixture was then filtered under reduced pressure (0.06 MPa) using a 200-mesh filter cloth. The filter cake was collected, transferred to a lyophilization bottle, and pre-frozen in an ultra-low temperature freezer at -80℃ for 4 h. The mixture was then transferred to a freeze dryer and freeze-dried at a cold trap temperature of -55℃ and a vacuum of 10 Pa for 24 h. Finally, the mixture was ground and passed through an 80-mesh sieve to obtain the *Cyprinus coccinea* extract.

[0074] Preparation Example 7

[0075] The preparation method of vetiver extract includes the following steps:

[0076] Select fresh vetiver roots, wash, dry, crush, pass through a 20-mesh sieve, and collect the powder that passes through the sieve.

[0077] Add 500 mL of deionized water to a 1000 mL round-bottom flask, connect a distillation stand with a sieve plate (5 mm aperture), and evenly spread 300 g of vetiver root powder on the sieve plate. Cover the top with a layer of absorbent cotton. Connect the condenser and the tail tube in sequence, inserting the end of the tail tube into a separatory funnel. Ensure the entire apparatus is sealed. After the water in the flask boils and produces stable steam, adjust the heating power to stabilize the steam generation rate (the distillate dripping rate at the condenser outlet should be 1-2 drops / second). Distill for 5 hours, then stop distillation and transfer the distillate to a container. The oil was transferred to a separatory funnel and allowed to stand for 30 minutes until the oil-water interface became clear. The lower layer of crude essential oil was then slowly released. The crude essential oil was transferred to an Erlenmeyer flask, and anhydrous sodium sulfate (10% of the essential oil mass) was added. The flask was sealed and placed on a shaker for 30 minutes. The dehydrated essential oil was filtered through qualitative filter paper to remove the anhydrous sodium sulfate particles, resulting in a pre-purified essential oil. The pre-purified essential oil was then placed in a -5°C freezer for 24 hours to allow the wax crystals to precipitate. The filtrate was then collected using a Buchner funnel pre-cooled to 0°C to obtain the vetiver extract.

[0078] Example 1

[0079] A method for preparing a facial moisturizing serum for sensitive skin includes the following steps:

[0080] S1. Take litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol, heat to 40℃, stir for 8 min to obtain phase A; the mass ratio of litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol is 1.2:1.8:1.4:1.2:1.8:1.8:81.9:0.3:0.4:0.2:8;

[0081] S2. Mix squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract, heat to 70°C, and stir for 10 minutes to obtain phase B; the mass ratio of squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract is 0.7:0.4:0.02:0.04:1.2.

[0082] S3. Add phase B to phase A, and homogenize and stir at 8000 r / min for 10 min at 45°C. Add phase C and homogenize and stir at 8000 r / min for 3 min to obtain the sensitive skin facial moisturizing essence.

[0083] Phase C comprises antioxidants, preservatives, and (daily-use) fragrances; the mass ratio of the antioxidants, preservatives, and (daily-use) fragrances is 3:1:2;

[0084] The mass ratio of phase A, phase B, and phase C is 72:17:1;

[0085] The thickener is selected from xanthan gum.

[0086] The moisturizer is selected from sodium hyaluronate.

[0087] The emulsifier is selected from PEG-10 polydimethylsiloxane.

[0088] The emollient is selected from ethylhexylglycerin.

[0089] The antioxidant is selected from tocopherol acetate.

[0090] The preservative is potassium sorbate.

[0091] Example 2

[0092] A method for preparing a facial moisturizing serum for sensitive skin includes the following steps:

[0093] S1. Take litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol, heat to 45℃, stir for 9 min to obtain phase A; the mass ratio of litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol is 1.8:2.7:1.6:1.3:2.0:2.2:78.3:0.35:0.5:0.25:9;

[0094] S2. Mix squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract, heat to 75°C, and stir for 8 minutes to obtain phase B; the mass ratio of squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract is 0.8:0.45:0.03:0.05:1.3.

[0095] S3. Add phase B to phase A, and homogenize and stir at 10000 r / min for 8 min at 45°C. Add phase C and homogenize and stir at 8000 r / min for 4 min to obtain the sensitive skin facial moisturizing essence.

[0096] Phase C comprises antioxidants, preservatives, and (daily-use) fragrances; the mass ratio of the antioxidants, preservatives, and (daily-use) fragrances is 5:2:3;

[0097] The mass ratio of phase A, phase B, and phase C is 77:22:1.5;

[0098] The thickener is selected from carbomer.

[0099] The humectant is selected from 1,2-hexanediol.

[0100] The emulsifier is selected from PEG-3 polydimethylsiloxane.

[0101] The emollient is selected from cetearyl stearate.

[0102] The antioxidant is selected from 3-o-ethyl ascorbic acid.

[0103] The preservative is potassium sorbate.

[0104] Example 3

[0105] A method for preparing a facial moisturizing serum for sensitive skin includes the following steps:

[0106] S1. Take litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol, heat to 50℃, stir for 10 min to obtain phase A; the mass ratio of litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol is 2.4:3.6:1.8:1.4:2.2:2.6:74.7:0.4:0.6:0.3:10;

[0107] S2. Mix squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract, heat to 80°C, and stir for 5 minutes to obtain phase B; the mass ratio of squalane, 5 viscosity silicone oil, emulsifier, emollient, and vetiver extract is 0.9:0.5:0.04:0.06:1.4.

[0108] S3. Add phase B to phase A, and homogenize and stir at 12000 r / min for 5 min at 45°C. Add phase C and homogenize and stir at 8000 r / min for 5 min to obtain the sensitive skin facial moisturizing essence.

[0109] Phase C comprises antioxidants, preservatives, and (daily-use) fragrances; the mass ratio of the antioxidants, preservatives, and (daily-use) fragrances is 7:3:4;

[0110] The mass ratio of phase A, phase B, and phase C is 81:27:2;

[0111] The thickener is selected from hydroxyethyl cellulose.

[0112] The moisturizer is selected from sodium hyaluronate.

[0113] The emulsifier is selected from PEG-10 polydimethylsiloxane.

[0114] The emollient is selected from cetyl palmitate.

[0115] The antioxidant is selected from 3-o-ethyl ascorbic acid.

[0116] The preservative is potassium sorbate.

[0117] Comparative Example 1

[0118] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain litchi seed extract. The reduced amount is allocated to the freeze-dried collagen powder of giant salamander, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, and vetiver extract in proportion to the proportions of the other components. The other components and their amounts remain unchanged.

[0119] Comparative Example 2

[0120] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain freeze-dried giant salamander collagen powder. The reduced amount is allocated to litchi seed extract, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract in proportion to the proportions of the other components. The other components and their amounts remain unchanged.

[0121] Comparative Example 3

[0122] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain black chokeberry extract. The reduced amount is allocated to litchi seed extract, giant salamander collagen freeze-dried powder, lentil seed extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract in proportion to the proportions of the other components. The other components and their amounts remain unchanged.

[0123] Comparative Example 4

[0124] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain lentil seed extract. The reduced amount is allocated to litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract in proportion to the proportions of the other components. The remaining components and their amounts remain unchanged.

[0125] Comparative Example 5

[0126] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain the short-petaled golden lotus extract. The reduced amount is allocated to the litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, sea buckthorn fruit extract, and vetiver extract in proportion to the number of parts. The remaining components and their amounts remain unchanged.

[0127] Comparative Example 6

[0128] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain the extract of *Symplocos edulis*. The reduced amount is allocated to the extracts of lychee seed, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, and vetiver extract in proportion to the number of parts. The remaining components and their amounts remain unchanged.

[0129] Comparative Example 7

[0130] This comparative example provides a facial moisturizing serum for sensitive skin. The only difference between this serum and Example 2 is that it does not contain vetiver extract. The reduced amount is allocated to litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, and sea buckthorn fruit extract in proportion to the proportions of the other components. The remaining components and their amounts remain unchanged.

[0131] Performance testing

[0132] 1) Moisturizing performance test

[0133] A multi-probe skin testing system, in conjunction with a skin moisture probe, was used to test the moisture content of the subject's stratum corneum. The measured value directly reflects the level of moisture content in the stratum corneum.

[0134] Fifty healthy volunteers aged 38-48 years, without skin diseases, allergies to skincare products, who had not used hormones or immunosuppressants in the past month, and without serious systemic diseases, immunodeficiency, or autoimmune diseases were selected. Five volunteers were randomly divided into 10 groups, each corresponding to one of the serums prepared in Examples 1-3 and Comparative Examples 1-7.

[0135] Two hours prior to the test, the skin should not come into contact with water. All subjects must be thoroughly cleaned before the test, i.e., wiped with a dry paper towel. Subjects should sit quietly for 30 minutes in a laboratory environment with a temperature of (21±1)℃ and humidity of 50%±10%. Control and test areas should be marked on the inner sides of each subject's left and right forearms, respectively. After measuring the baseline skin moisture value (T0), the concentration should be (2.0±0.1) mg / cm³. 2Equal amounts of deionized water and serum were applied to each group, and the skin moisture content was measured 8 hours after using the serum. The data were recorded and the skin moisture content change rate (skin improvement degree) was calculated. The average value of each group was taken and summarized. The test results are shown in Table 1 below.

[0136] The calculation formula is as follows:

[0137] Skin improvement level = (Skin moisture value in test area - Skin moisture value in control area) / Skin moisture value in control area × 100%

[0138] Table 1

[0139]

[0140] As shown in Table 1, the serums prepared in Examples 1-3 of this application have good moisturizing effects and can increase the water content of the stratum corneum of the skin, thus achieving the effect of hydrated skin. The serums prepared in Comparative Examples 1-7 lack the synergistic effect between the components, resulting in a decrease in moisturizing effect compared with each example.

[0141] 2) Sensitive skin repair performance test

[0142] Female volunteers aged 25-35 years who met the diagnostic criteria for sensitive skin were randomly divided into 10 groups of 5 people each. An appropriate amount of the serum prepared in Examples 1-3 and Comparative Examples 1-7 was applied evenly to the red and swollen areas, followed by gentle massage for 3-5 minutes. This was done twice daily, morning and evening, for 28 consecutive days. Throughout the treatment, a regular diet and lifestyle were maintained, and the affected areas should not be squeezed or frequently touched. Facial images were captured using VISIA-CR before and after treatment, and skin a* value analysis was performed. The lower the value, the milder the redness. The test results are shown in Table 4 below.

[0143] Table 4

[0144]

[0145] The experimental results above show that the serums prepared in Examples 1-3 of this application have good skin repair and soothing effects on sensitive skin, which are superior to the comparative groups.

[0146] In summary, this application, through the addition of lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, sea buckthorn fruit extract, and vetiver extract, achieves excellent moisturizing effects through the synergistic interaction of these components, resulting in hydrated skin and improving and repairing sensitive skin issues.

[0147] The litchi seed extract is rich in litchi seed polysaccharides, which can bind water molecules through hydrogen bonds, increase the moisture content of the skin surface, and promote the synthesis of intercellular lipids in keratinocytes, thus strengthening the skin barrier function. This property helps to relieve redness, stinging and other problems caused by barrier damage in sensitive skin.

[0148] The freeze-dried collagen powder from giant salamanders is rich in small molecule peptide active ingredients that can penetrate deep into the skin. By promoting cell metabolism, it enhances the skin's ability to retain moisture, reduces water loss, maintains the skin's hydration, stimulates the proliferation of keratinocytes, strengthens the skin barrier structure, indirectly enhances the epidermis's ability to retain water, improves sensitivity caused by dryness, accelerates the repair of damaged tissue, reduces discomfort such as redness and stinging caused by external stimuli, balances the skin's metabolic cycle, repairs sensitivity caused by barrier damage, and enhances the tolerance of sensitive skin.

[0149] The polysaccharides in the extract of *Sorbus nigra* (such as pyranose, furanose, α-glycosidic bonds, β-glycosidic bonds, etc., with the α configuration being the most prevalent) have good water solubility and film-forming properties, which can form a physical barrier on the skin surface to block exogenous stimuli and prevent moisture loss. Polysaccharides with α-glycosidic bonds are more easily recognized by skin keratinocytes, promoting barrier regeneration. They can also regulate inflammatory pathways, relieve redness and itching of sensitive skin, reduce inflammatory response from the source, promote the secretion of anti-inflammatory factors, inhibit histamine release, and quickly relieve acute discomfort symptoms of sensitive skin. They can also prolong the antioxidant effect of polysaccharides in the skin, activate the skin's own antioxidant system, and reduce the recurrence frequency of sensitive skin.

[0150] Stilt seed extract is rich in active ingredients such as stilt polysaccharides, phytosterols, and polyphenols, which work synergistically from four dimensions: "barrier repair, inflammation suppression, moisturizing and water locking, and antioxidant protection" to specifically address the core problems of sensitive skin, such as a fragile barrier, susceptibility to irritation, rapid moisture loss, and recurring inflammation.

[0151] Short-petaled golden lotus extract can regulate the balance of capillary contraction and relaxation, enhance the stability of blood vessel walls, repair the vascular endothelial barrier, activate antioxidant enzymes, improve abnormal capillary function, synergistically repair the stratum corneum barrier, reduce oxidative stress, and reduce the frequency of sensitivity recurrence. It is especially effective for sensitive skin with rosacea and sensitive skin that is prone to redness and burning.

[0152] The core of the benefits of sea buckthorn fruit extract for improving and repairing sensitive skin lies in its rich content of unsaturated fatty acids, phytosterols, polyphenolic compounds, and other active ingredients. These ingredients can promote ceramide synthesis, enhance epidermal hydration and replenish surface lipids, repair the skin barrier, and improve sensitive skin.

[0153] Vetiver extract can effectively eliminate the stress hormone cortisol, induce the secretion of β-endorphin, promote nerve relaxation, and has excellent anti-inflammatory ability. It can effectively inhibit the inflammatory cascade reaction, relieve skin stress, and reduce skin discomfort.

[0154] The extracts of sea buckthorn fruit and litchi seed simultaneously promote the synthesis of lipids between keratinocytes, fill the lipid gap outside of ceramides, and improve the lipid structure of the stratum corneum; the freeze-dried collagen powder of giant salamander further penetrates into the superficial dermis, stimulates the proliferation of keratinocytes, increases the density of stratum corneum cells, and reduces the penetration of external irritants.

[0155] The fatty acid composition of the sea buckthorn fruit extract is highly compatible with human sebum, which can instantly replenish the surface lipids lost by sensitive skin; while the lentil seed extract reduces the excessive secretion of sebum due to the damage of the barrier by regulating the activity of sebaceous glands, thereby achieving long-term balance of the sebum film. The two work together to make the sebum film more stable.

[0156] Short-petaled golden lotus extract improves capillary contraction and relaxation by repairing the vascular endothelial barrier and enhancing vascular wall stability. At the same time, its activated antioxidant enzymes can reduce oxidative damage to the vascular endothelium, forming a dual protection from the inside out with the stratum corneum barrier repair effects of sea buckthorn fruit extract and litchi seed extract.

[0157] Black chokeberry extract has excellent water solubility and film-forming properties, forming a physical barrier on the skin surface to directly block moisture evaporation; litchi seed extract binds water molecules through hydrogen bonds, and the two work together to increase surface moisture content while avoiding a heavy film feeling.

[0158] The synergistic effect of extracts from sea buckthorn fruit and lychee seed can improve the lipid structure of the stratum corneum, while extracts from lentil seed can increase the content of epidermal mucopolysaccharides and enhance the water retention capacity of the middle layer of skin. The three work together to reduce water loss from the epidermis to the outside world. After the freeze-dried collagen powder of giant salamander penetrates into the dermis, it promotes fibroblast metabolism and increases the synthesis of hyaluronic acid in the dermis, thereby improving the skin's water retention capacity from deep within. At the same time, its stimulation of keratinocyte proliferation can enhance the epidermis's ability to absorb water, completely solving the problem of recurring dryness in sensitive skin.

[0159] In addition, black chokeberry extract can directly regulate inflammatory pathways and inhibit the release of histamine, a core mediator of allergies and acute irritation, to quickly relieve acute discomfort such as redness and stinging. Its promoted secretion of anti-inflammatory factors can further enhance the acute soothing effect. Soldier bean seed extract achieves multi-dimensional anti-inflammatory effects by clearing inflammatory mediators and inhibiting inflammatory cascade reactions. Green prickly pear fruit extract and short-petaled golden lotus extract reduce oxidative stress-induced inflammation through antioxidant effects. The components work together to reduce the frequency of inflammation recurrence and avoid repeated stimulation of sensitive skin.

[0160] Vetiver extract relieves stress-induced sensitivity and discomfort by eliminating the stress hormone cortisol and inducing the secretion of the anti-inflammatory neurotransmitter β-endorphin; its inhibition of the inflammatory cascade complements the anti-inflammatory mechanisms of black chokeberry and lentil seed, making the anti-inflammatory effect more comprehensive;

[0161] Black chokeberry extract prolongs the antioxidant effect and can continuously remove epidermal ROS; lentil seed extract and sea buckthorn fruit extract directly neutralize free radicals through phenolic hydroxyl groups, especially targeting UV-induced oxidative damage. The three work together to reduce epidermal oxidative stress.

[0162] Short-petaled golden lotus extract and vetiver extract can regulate cell metabolism and enhance the activity of the skin's own antioxidant enzymes. Together with direct antioxidant ingredients, they form an antioxidant synergy of external cleansing and internal protection, reducing long-term damage to the skin barrier caused by oxidative stress and lowering the frequency of sensitivity recurrence.

[0163] The synergistic effect of the seven extracts can simultaneously address the specific needs of different sensitive skin types, ultimately forming a complete closed loop of protection, repair, stabilization, and soothing, achieving a synergistic effect of short-term soothing and long-term repair.

[0164] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A sensitive skin face moisturizing serum, characterized in that, include: Phase A: Litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol; Phase B: Squalane, silicone oil, emulsifiers, emollients, and vetiver extract; Phase C: Antioxidants, preservatives, and everyday fragrances; The preparation method of the litchi seed extract includes the following steps: litchi seeds are washed, crushed, and sieved to obtain seed powder; the seed powder is adjusted to pH 4.5 with deionized water, sodium dodecyl sulfate and cellulase are added, and the mixture is stirred at 45℃ for 60 min; the mixture is refluxed at 80℃ for 2 h, concentrated, and then subjected to a 75% ethanol solution for standing. The mixture is then filtered, washed, and the ethanol is evaporated to obtain the litchi seed extract; the ratio of seed powder, deionized water, surfactant, and cellulase is 15 g: 200 mL: 0.4 g: 300000 U. The preparation method of the giant salamander collagen freeze-dried powder includes the following steps: taking giant salamander skin tissue and subjecting it to two defatting, protein removal, acid extraction, dialysis, and freeze-drying to obtain a crude extract; the crude extract is subjected to neutral protease hydrolysis, enzyme inactivation, centrifugation, collection of supernatant for dialysis, and freeze-drying to obtain the giant salamander collagen freeze-dried powder; The preparation method of the black chokeberry extract includes the following steps: freeze-drying, pulverizing and sieving black chokeberry fruit, defatting and hot extraction, concentrating and adding 3 times the volume of pre-cooled 93% ethanol solution for precipitation; removing impurities from the precipitate, preparing a polysaccharide solution, removing protein, dialyzing, freeze-drying, grinding and sieving to obtain the black chokeberry extract. The preparation method of the lentil seed extract includes the following steps: pulverize and sieve lentil seeds, add 70% ethanol solution at a material-to-liquid ratio of 1:15, heat and reflux to extract, collect the filtrate, concentrate and freeze dry to obtain the lentil seed extract. The preparation method of the short-petaled golden lotus extract includes the following steps: crushing and sieving the short-petaled golden lotus, extracting with alcohol, filtering, concentrating and drying the filtrate to obtain a crude extract; purifying with pretreated AB-8 resin, eluting with 50% ethanol solution, concentrating the eluent, freeze-drying, and sieving to obtain the short-petaled golden lotus extract. The preparation method of the prickly pear fruit extract includes the following steps: take prickly pear fruit oil residue, dry, crush and sieve it, add water, microwave treat and vacuum extract it, concentrate it and add 95% ethanol solution to precipitate it, filter it, take the filter cake, pre-freeze, freeze dry it, grind and sieve it to obtain the prickly pear fruit extract. The preparation method of the vetiver extract includes the following steps: pulverizing and sieving vetiver root, steam distilling to obtain crude essential oil; dehydrating with anhydrous sodium sulfate, freezing at -5℃ to remove wax, filtering, and collecting the filtrate to obtain the vetiver extract; In phase A, the mass ratio of litchi seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, humectant, allantoin, and butylene glycol is 1.2-2.4:1.8-3.6:1.4-1.8:1.2-1.4:1.8-2.2:1.8-2.6:74.7-81.9:0.3-0.4:0.4-0.6:0.2-0.3:8-10; In phase B, the mass ratio of squalane, silicone oil, emulsifier, emollient and vetiver extract is 0.7-0.9:0.4-0.5:0.02-0.04:0.04-0.06:1.2-1.4; In phase C, the mass ratio of the antioxidant, preservative and daily fragrance is 3-7:1-3:2-4; The thickener is selected from at least one of xanthan gum, carbomer, and hydroxyethyl cellulose; The moisturizer is selected from at least one of sodium hyaluronate and 1,2-hexanediol; The emulsifier is selected from at least one of PEG-10 polydimethylsiloxane and PEG-3 polydimethylsiloxane; The emollient is selected from at least one of ethylhexylglycerin, cetearyl stearate, and cetearyl palmitate.

2. The method for preparing a facial moisturizing essence for sensitive skin according to claim 1, characterized in that, Includes the following steps: S1. Take lychee seed extract, giant salamander collagen freeze-dried powder, black chokeberry extract, lentil seed extract, short-petaled golden lotus extract, green prickly pear fruit extract, deionized water, thickener, moisturizer, allantoin and butylene glycol, heat to 40-50℃, stir for 8-10 minutes to obtain phase A. S2. Mix squalane, silicone oil, emulsifier, emollient, and vetiver extract, heat to 70-80℃, and stir for 5-10 minutes to obtain phase B; S3. Add phase B to phase A, and homogenize and stir at 8000-12000 r / min for 5-10 min at 45°C. Add phase C and homogenize and stir at 8000 r / min for 3-5 min to obtain the sensitive skin facial moisturizing essence.

3. The method for preparing a facial moisturizing essence for sensitive skin according to claim 2, characterized in that, The mass ratio of phase A, phase B, and phase C is 72-81:17-27:1-2.

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