Preparation method of grapefruit hand cream

Abstract

The invention discloses a preparation method of grapefruit hand cream, and belongs to the technical field of cosmetics. The method comprises the following steps: S1, mixing and stirring a first clathrate, a compound, a second clathrate, samara oil, beewax, polyglycerol-6 distearate and a composite microcapsule, the first clathrate is prepared by coating pomelo peel polyphenol with hydroxypropyl-beta-cyclodextrin and the like, and the compound comprises pomelo hydrolat and polyglycerol-10 laurate; the second inclusion compound is prepared by coating a ginger root-Chinese prickly ash extract with methyl-beta-cyclodextrin and the like; the composite microcapsule contains limonene, a grapefruit seed extract and the like; s2, dissolving hydrolyzed tremella polysaccharide and other components in deionized water, adding zinc hyaluronate and the composite system after enzymolysis, and shearing and emulsifying with the oil phase in S1; s3, cooling the emulsifying system, adding the grapefruit flower extract and vitamin E, uniformly stirring, refrigerating and shaping, and recovering to room temperature to obtain a finished product. The hand cream prepared by the invention can help to improve the problems that the hand cream is poor in component compounding compatibility, easy to degrade in efficacy, hard in paste at low temperature and the like.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically a method for preparing grapefruit hand cream. Background Technology

[0002] Hand cream is a commonly used daily skin care product. Its core function is to replenish moisture to the skin on the hands, nourish the skin, and repair the damaged barrier, thereby relieving discomfort such as dryness and roughness and improving skin comfort. In winter, the skin on our hands faces unique environmental challenges: Firstly, the significant temperature difference between indoors and outdoors causes frequent hot and cold stimulation, increasing the difficulty of repairing the skin's lipid barrier and exacerbating its fragility. Secondly, the low temperatures, low humidity, and strong winds outdoors not only accelerate moisture loss but can also affect local blood circulation, potentially triggering or worsening chilblains, leading to more serious problems such as redness, itching, pain, and even ulceration. Therefore, using hand cream is especially necessary in winter. However, most regular hand creams only meet basic hydration and moisturizing needs and are insufficient to address the problem of chilblains on the hands in winter. It is known that the core causes of chilblains are related to poor local blood circulation, damaged skin barrier, and inflammatory response in low-temperature environments. Natural components such as grapefruit peel polyphenols, grapefruit hydrosol (obtained by distillation from grapefruit peel), ginger extract (containing gingerol), Sichuan pepper extract (containing cinnamon), winged fruit oil, and beeswax all possess suitable efficacy for chilblain care: grapefruit peel polyphenols can inhibit the release of inflammatory factors and improve local microcirculation; grapefruit hydrosol can soothe irritation and replenish moisture; ginger root and Sichuan pepper extracts can gently generate heat and promote circulation; and winged fruit oil and beeswax can strengthen barrier repair and improve the shape retention of the cream. Based on this, the inventors attempted to synergistically combine these components into hand cream to achieve complementary effects. However, in actual implementation, they discovered some drawbacks in the synergistic application of these components, specifically as follows: First, when water-soluble grapefruit hydrosol is combined with oil-phase ingredients such as winged fruit oil and beeswax, the compatibility is extremely poor, directly leading to the separation of the paste and instability of the emulsion system. Second, when grapefruit peel polyphenols are combined with ginger extract, the oxidation-reduction reaction will accelerate their degradation and significantly shorten the duration of efficacy. Third, in low-temperature environments, beeswax itself contains crystalline components such as palmitate, which easily form regular crystal structures. Meanwhile, the fat-soluble gingerol derivatives in ginger extract act as "crystal nuclei," inducing rapid growth and aggregation of beeswax crystals. The synergistic effect of the two leads to an increase in the crystallinity and hardness of the paste, ultimately forming a low-temperature hard paste that is difficult to apply and has reduced compatibility. Therefore, how to provide a solution that can simultaneously address the problems of poor compatibility of the above-mentioned components, easy degradation of efficacy, thick and sticky texture, and low-temperature hardening has become an urgent technical challenge. Summary of the Invention

[0003] The purpose of this invention is to provide a method for preparing grapefruit hand cream, so as to effectively solve the problems of poor compatibility of component synergy, easy degradation of efficacy, thick and sticky texture, and hardening at low temperature.

[0004] The objective of this invention is achieved through the following technical solution: A method for preparing a grapefruit hand cream includes the following steps: S1. Preparation of the oil phase: The first inclusion compound, the complex, the second inclusion compound, winged fruit oil, beeswax, polyglycerol-6 distearate, and the composite microcapsules are mixed and stirred thoroughly to obtain the oil phase; The preparation of the first inclusion compound: ① Dissolve hydroxypropyl-β-cyclodextrin in deionized water, add grapefruit peel polysaccharide, heat and stir to dissolve, and obtain the first cyclodextrin solution; separately dissolve grapefruit peel polyphenols in ethanol, add vitamin E to form a complex solution; ② Add the composite liquid dropwise to the first cyclodextrin solution, stir, refrigerate and stand, filter and dry to obtain the product; Preparation of the complex: Grapefruit hydrosol was mixed with polyglycerol-10 laurate, grapefruit peel polysaccharide and grapefruit seed extract were added, ultrasonically dispersed, and then freeze-dried to obtain the product; Preparation of the second inclusion complex: ① Dissolve methyl-β-cyclodextrin in deionized water, add grapefruit peel polysaccharide, heat to dissolve, and then add Tween-80 to obtain a second cyclodextrin solution; separately, dissolve ginger extract and Sichuan pepper extract in ethanol to obtain an extract solution; ② Add the extract solution dropwise to the second cyclodextrin solution, stir, refrigerate and stand, filter and dry to obtain the product; The composite microcapsules are prepared from limonene, grapefruit seed extract, grapefruit peel pectin, β-cyclodextrin and calcium chloride; S2. Preparation of emulsion system: hydrolyzed tremella polysaccharide, ceramide NP, grapefruit seed polypeptide and vitamin C palmitate are added to deionized water for dissolution, followed by enzymatic hydrolysis with bromelain, then zinc hyaluronic acid and the composite system are added, stirred and dissolved, and then poured into the oil phase of S1. After high-speed shear emulsification, the emulsion system is obtained; The composite system consists of xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid, low molecular weight hyaluronic acid, agarose, and polyethylene glycol-4000; S3. Setting: Cool the S2 emulsion system, add grapefruit flower extract and vitamin E, stir well, pour into a container, refrigerate to set, and then return to room temperature to obtain the finished product. As some possible implementations of this application, in step S1, the mass ratio of each component is: first inclusion complex: complex: second inclusion complex: winged fruit oil: beeswax: polyglycerol-6 distearate: complex microcapsule = (3-5): (4-6): (2-3): (18-22): (4-7): (2-3): (0.13-0.25).

[0005] As one possible implementation of this application, in step S1, the condition for sufficient stirring is: stirring at 500-600 r / min for 35-45 min at 70-75°C. As some possible implementations of this application, in step S1, the mass ratio of each component in the composite microcapsule is: limonene: grapefruit seed extract: grapefruit peel pectin: β-cyclodextrin: calcium chloride = (0.03-0.05): (0.03-0.08): (1-1.5): (1.8-2.5): (0.01-0.03). As some possible implementations of this application, in step S1, the mass ratio of each component in the preparation of the first inclusion compound is: hydroxypropyl-β-cyclodextrin: deionized water: grapefruit peel polysaccharide: grapefruit peel polyphenol: ethanol: vitamin E = (2-3): (15-20): (0.01-0.02): (2-3): (5-8): (0.1-0.2). As some possible embodiments of this application, in step S1, the mass ratio of each component in the preparation of the complex is: grapefruit hydrosol: polyglycerol-10 laurate: grapefruit peel polysaccharide: grapefruit seed extract = (4-6): (3-5): (0.01-0.02): (0.1-0.2). As some possible embodiments of this application, in step S1, the mass ratio of each component in the preparation of the second inclusion compound is: methyl-β-cyclodextrin: deionized water: grapefruit peel polysaccharide: Tween-80: ginger extract: Sichuan pepper extract: ethanol = (2-3): (15-20): (0.01-0.02): (0.1-0.2): (1-1.5): (0.5-0.8): (5-8). As some possible implementation methods of this application, in step S2, the mass ratio of each component is: hydrolyzed Tremella polysaccharide: ceramide NP: grapefruit seed polypeptide: vitamin C palmitate: deionized water: bromelain: zinc hyaluronic acid: xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid: low molecular weight hyaluronic acid: agarose: polyethylene glycol-4000 = (0.8-1.2): (0.4-0.6): (0.7-0.9): (0.2-0.4): (60-75): (0.08-0.12): (0.1-0.2): (0.08-0.12): (0.05-0.08): (0.03-0.05): (0.02-0.03). As some possible implementations of this application, in step S3, the emulsification system is cooled to 35-40°C, the refrigeration temperature is 2-5°C, and the setting time is 1.5-2 hours. Compared with the prior art, the beneficial effects of the present invention are: The method for preparing grapefruit hand cream provided by this invention helps to improve core problems such as poor compatibility of synergistic compounding of ingredients in winter hand creams, easy degradation of efficacy, and hardening at low temperatures, as detailed below: During the preparation of the S1 oil phase: In the first stage of complex preparation, grapefruit peel polyphenols possess anti-inflammatory and microcirculation-improving effects. However, when coexisting with ginger extract, they are prone to redox reactions that accelerate degradation, affecting the duration of efficacy. Therefore, this invention uses hydroxypropyl-β-cyclodextrin to encapsulate grapefruit peel polyphenols, leveraging its hydrophilic modified groups to enhance water solubility. Simultaneously, a cavity structure physically isolates the grapefruit peel polyphenols from the ginger extract, reducing direct reactions between the two. Combined with vitamin E, a synergistic antioxidant system is formed, further reducing the risk of polyphenol oxidative degradation. This step not only helps alleviate the antagonistic effects of grapefruit peel polyphenols and ginger extract but also improves the dispersion stability of polyphenols in the system, laying the foundation for subsequent synergistic effects. In the complex preparation process, grapefruit hydrosol can soothe skin irritation and replenish moisture, but its water-soluble nature makes it poorly compatible with oil-phase components, and direct compounding can easily lead to layering of the paste. This invention utilizes the hydrogen bonding between the flavonoid active ingredients in grapefruit hydrosol and polyglycerol-10 laurate, combined with the synergistic dispersing effect of grapefruit peel polysaccharides, to construct a hydrophilic-lipophilic composite dispersion system, allowing the water-soluble grapefruit hydrosol to be uniformly dispersed in the oil-phase system. The flavonoid and polyphenol active ingredients in grapefruit seed extract can further form a synergistic hydrogen bond network with the above components, enhancing the structural stability of the composite dispersion system. Simultaneously, its natural active components also possess gentle soothing effects, reducing the potential irritation of the system to the skin.

[0006] In the second encapsulation preparation stage, the ginger root-Sichuan pepper composite extract can gently generate heat and promote blood circulation, meeting the needs of frostbite care. However, the gingerol in it can act as a nucleus to induce beeswax crystallization, causing the ointment to harden and become difficult to apply at low temperatures. This invention uses methyl-β-cyclodextrin to encapsulate the composite extract. Its hydrophobically modified cavity is more suitable for the fat-soluble gingerol and small beeswax molecules, allowing them to be embedded simultaneously, inhibiting the growth and aggregation of beeswax crystals, and improving the problem of hardening at low temperatures. Combined with Tween-80, it enhances the solubility and dispersibility of the extract, ensuring the stable performance of its heat-generating effect. This step achieves a synergistic effect between the heat-generating effect of the ginger root-Sichuan pepper composite extract and the low-temperature adaptability of the ointment, reducing adverse interactions between the active ingredients and the matrix. In the process of adding the composite microcapsule, limonene can help improve the release efficiency of the active ingredients and impart a natural grapefruit aroma, but it is volatile and may lead to a decrease in the synergistic effect of efficacy and dissipation of aroma. Considering that grapefruit seed extract has already been added in the composite preparation process, to avoid its excessively high free concentration becoming an oxidizing substrate and causing peroxidation, this invention employs microcapsule encapsulation technology to prepare grapefruit peel pectin-β-cyclodextrin composite microcapsules with an appropriate amount of grapefruit seed extract. The physical barrier effect of the wall material reduces the volatility of limonene, achieving slow release; simultaneously, by encapsulating part of the grapefruit seed extract in the microcapsule wall material, its free concentration in the system is controlled, balancing catalyst chelation efficiency and antioxidant balance. Grapefruit peel pectin, as a natural component, has good compatibility with the core grapefruit components in the system and can also help enhance the structural stability of the paste. In the preparation of the S2 emulsification system, hydrolyzed Tremella fuciformis polysaccharide, xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid, and low molecular weight hyaluronic acid work synergistically. The xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid possesses an amphiphilic structure; its lipophilic segments can form hydrophobic interactions with the oil phase components, while its hydrophilic segments work in conjunction with the hydrolyzed Tremella fuciformis polysaccharide and low molecular weight hyaluronic acid, which helps improve emulsification stability and reduce the viscosity of the ointment, thus improving its stickiness. The low molecular weight hyaluronic acid synergistically works with limonene released from the composite microcapsules in S1 to break down the encapsulation barrier of the active ingredients, alleviating the problem of delayed efficacy release and ensuring the timely thermogenic and anti-inflammatory effects required for frostbite care are effectively achieved. Simultaneously, the skin permeability of grapefruit seed peptides is enhanced by enzymatic hydrolysis of grapefruit seed peptides with bromelain, and combined with ceramide NP and zinc hyaluronic acid, it synergistically repairs the damaged skin barrier caused by frostbite, meeting the core needs of winter frostbite care. During the S3 shaping process, cyclodextrin inclusion complexes and composite colloids synergistically regulate the hardness of the ointment, ensuring its stability over a wide temperature range, reducing hardening and oiliness, and meeting the application needs of frostbite areas in low-temperature winter environments. Among them, grapefruit flower extract is a natural fragrance component obtained by extracting grapefruit flowers, which can give the product a fresh and natural fragrance, and can form a synergistic fragrance with limonene released by composite microcapsules, enhancing the sensory experience of using the product during frostbite care. In summary, this invention, through a three-step process and the synergistic effect of each modification step, helps to improve core issues of winter hand creams such as poor compatibility, easy degradation of efficacy, and hardening at low temperatures. The components work together to achieve low-temperature compatibility, a refreshing feel, gentle heat generation to promote circulation, long-lasting moisture retention, and barrier repair function for frostbite areas. This can help alleviate discomfort such as redness and itching caused by frostbite in winter. The process has good repeatability and is suitable for industrial production. Detailed Implementation

[0007] Example 1 1. Preparation of some components (components whose preparation methods are not mentioned are all commercially available cosmetic-grade components) (1) Preparation of grapefruit seed protein and grapefruit seed polypeptide: ① Preparation of grapefruit seed protein: Fresh grapefruit seeds (i.e., grapefruit kernels) were taken, the outer shell was removed, and the seeds were crushed. Five times the mass of deionized water was added, and the mixture was extracted at 40℃ with stirring for 2 hours. The supernatant was collected by centrifugation (5000 r / min, 15 min). Ammonium sulfate was added to the supernatant until the saturation was 60%. The mixture was refrigerated at 4℃ for 4 hours and then centrifuged again (5000 r / min, 20 min) to collect the precipitate. The precipitate was dissolved in a small amount of deionized water and dialyzed through a dialysis bag (molecular weight cutoff 8000 Da) for 24 hours (with deionized water replaced every 6 hours). Finally, the grapefruit seed protein was obtained by freeze-drying (-50℃, vacuum degree 10 Pa). ② Preparation of grapefruit seed polypeptide: Take 10 parts (mass parts, the same below) of grapefruit seed protein, add 100 parts of deionized water, stir and dissolve at 55℃, add 0.1 parts of bromelain (enzyme activity 100,000 U / g), stir and hydrolyze at 55℃ for 15 min, raise the temperature to 80℃ and keep warm for 10 min to inactivate the enzyme, cool and centrifuge (4000 r / min, 15 min) to collect the supernatant, freeze dry (-50℃, vacuum degree 10 Pa) to obtain grapefruit seed polypeptide.

[0008] (2) Preparation of pomelo peel pectin: Take fresh pomelo peel, remove the wax layer and chop it, add 8 times the mass of deionized water, adjust the pH to 2.0 with food-grade citric acid, extract at 90℃ for 1.5h, centrifuge (4000r / min, 15min) and take the supernatant; add 95% food-grade ethanol to the supernatant to 60% ethanol volume fraction, let stand to precipitate for 4h, centrifuge (4000r / min, 15min) and collect the precipitate; wash the precipitate 3 times with anhydrous ethanol, vacuum dry (50℃, vacuum degree 50Pa), grind it with a low temperature grinder, and pass it through a 200 mesh sieve (particle size ≤10μm) to obtain pomelo peel pectin.

[0009] (3) Preparation of grapefruit peel polysaccharide: Take fresh grapefruit peel, remove the wax and chop it, add 10 times the mass of deionized water, extract at 85℃ for 2h, centrifuge (4000r / min, 15min) to collect the supernatant; add 95% ethanol to 70% by volume, let stand to precipitate for 6h, centrifuge to collect the precipitate; wash the precipitate twice with anhydrous ethanol, vacuum dry (55℃, vacuum degree 50Pa), grind through a 100-mesh sieve to obtain grapefruit peel polysaccharide.

[0010] (4) Preparation of grapefruit peel polyphenols: Take fresh grapefruit peel, remove the wax layer and crush it, add 8 times the mass of 60% ethanol solution, stir and extract at 55℃ for 2h, centrifuge (4000r / min, 15min) to collect the supernatant; add petroleum ether to the supernatant twice to defatt it (each time the volume of the extractant is 1 / 2 of the volume of the supernatant), and discard the petroleum ether phase; recover ethanol by vacuum distillation of the aqueous phase (50℃, vacuum degree 50Pa), dialyze through a dialysis bag (molecular weight cutoff 500Da) for 12h, and freeze dry (-50℃, vacuum degree 10Pa) to obtain grapefruit peel polyphenols.

[0011] (5) Preparation of grapefruit seed extract: Take fresh grapefruit seeds, remove the shells and crush them, add 10 times the mass of deionized water, stir and extract at 60℃ for 3h, centrifuge (5000r / min, 20min) to collect the supernatant; add ammonium sulfate to saturation of 70%, refrigerate at 4℃ for 6h, centrifuge to collect the precipitate; dissolve the precipitate with a small amount of deionized water, dialyze (molecular weight cutoff 8000Da) for 24h, freeze dry to obtain grapefruit seed extract.

[0012] (6) Preparation of hydrolyzed Tremella polysaccharide: ① Take 10 parts of fresh Tremella, dry and crush them through a 100-mesh sieve, add 20 times the mass of deionized water, extract at 95℃ for 3h, centrifuge (4000r / min, 20min) and collect the supernatant; ② Add 0.2 parts of food-grade α-amylase (enzyme activity 50,000 U / g) to the supernatant, stir and hydrolyze at 60℃ for 2h, raise the temperature to 90℃ and keep warm for 15min to inactivate the enzyme; ③ Add 95% food-grade ethanol to 75% ethanol volume fraction, let stand to precipitate for 8h, centrifuge (4000r / min, 20min) to collect the precipitate; ④ Wash the precipitate twice with anhydrous ethanol, vacuum dry (55℃, vacuum degree 50Pa), grind through a 100-mesh sieve to obtain hydrolyzed Tremella polysaccharide.

[0013] (7) Preparation of the first inclusion compound: ① Hydroxypropyl-β-cyclodextrin:deionized water:citronella peel polysaccharide:citronella peel polyphenol:ethanol:vitamin E were dissolved in deionized water at a mass ratio of 2.5:18:0.015:2.5:6:0.15. Citronella peel polysaccharide was added, and the mixture was heated to 62°C and stirred until dissolved to obtain the first cyclodextrin solution. Citronella peel polyphenol was dissolved in ethanol, and vitamin E was added and stirred until homogeneous to form a composite solution. ② The composite solution was slowly added dropwise to the first cyclodextrin solution at a rate of 0.08 g / min, stirred at 62℃ for 2 h, refrigerated at 4℃ for 12 h, and then filtered. The filter residue was dried under vacuum (50℃, vacuum degree 50 Pa) to obtain the first inclusion complex.

[0014] (8) Preparation of the complex: Grapefruit hydrosol: polyglycerol-10 laurate: grapefruit peel polysaccharide: grapefruit seed extract = 5:4:0.015:0.15 by mass ratio. Grapefruit hydrosol and polyglycerol-10 laurate were mixed, grapefruit peel polysaccharide was added and ultrasonically dispersed for 12 min (power 250W, frequency 20kHz). After stirring for 28 min, grapefruit seed extract was added and freeze-dried (-50℃, vacuum degree 10Pa) to obtain the complex.

[0015] (9) Preparation of the second inclusion complex: Methyl-β-cyclodextrin:deionized water:citronella peel polysaccharide:Tween-80:ginger extract:Sichuan pepper extract:ethanol = 2.5:18:0.015:0.15:1.2:0.6:6 was used. Methyl-β-cyclodextrin was dissolved in deionized water, and citronella peel polysaccharide was added. After dissolving at 62°C, Tween-80 was added and stirred evenly. Ginger extract and Sichuan pepper extract were dissolved in ethanol to obtain an extract solution. The extract solution was slowly added dropwise to the cyclodextrin solution and stirred at 62°C for 2 hours. After standing at 4°C for 12 hours, the mixture was filtered. The filter residue was vacuum dried (50°C, vacuum degree 50Pa) to obtain the second inclusion complex.

[0016] (10) Preparation of composite microcapsules: Limonene: grapefruit seed extract: grapefruit peel pectin: β-cyclodextrin: calcium chloride = 0.04:0.05:1.2:2.2:0.02 by mass ratio. β-cyclodextrin and grapefruit peel pectin were dissolved in deionized water and stirred at 60°C to prepare a wall material solution. Limonene and grapefruit seed extract were mixed and added to the wall material solution. The mixture was emulsified by high-speed shearing at 8000 r / min for 10 min. Calcium chloride was added and stirred for 30 min for crosslinking. The mixture was then freeze-dried (-50°C, vacuum degree 10 Pa) to obtain composite microcapsules.

[0017] (11) Preparation of xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid: 10 parts xanthan gum were dissolved in 100 parts deionized water and stirred at 55°C. 12 parts polyethylene glycol monomethyl ether were added and 0.2 parts p-citric acid was added as a catalyst. The mixture was stirred at 60°C for 3 hours and then dialyzed for 24 hours before being freeze-dried to obtain the grafted modified colloid.

[0018] 2. Steps for preparing hand cream.

[0019] S1. Preparation of oil phase: Take 4 parts of the first inclusion compound, 5 parts of the complex, 2.5 parts of the second inclusion compound, 20 parts of winged fruit oil, 5.5 parts of beeswax, 2.5 parts of polyglycerol-6 distearate, and 0.19 parts of the composite microcapsule, mix them, heat to 72℃, and stir at 550r / min for 40min to obtain a homogeneous oil phase.

[0020] S2. Preparation of the synergistic emulsification system: 1.0 part of hydrolyzed Tremella fuciformis polysaccharide, 0.5 part of ceramide NP, 0.8 part of grapefruit seed polypeptide, and 0.3 part of vitamin C palmitate were added to 68 parts of deionized water, dissolved, and then heated to 55℃; 0.1 part of bromelain was prepared by dissolving it in 0.3 parts of deionized water to form an enzyme solution, which was then added to the above solution. The mixture was stirred at 55℃ for 12 min to obtain the enzymatic hydrolysis aqueous phase. After enzymatic hydrolysis, the temperature was raised to 80℃ and held for 10 min to inactivate the enzyme, then cooled to room temperature; 0.15 After dissolving zinc hyaluronic acid, add a composite system consisting of 0.1 parts xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid, 0.06 parts low molecular weight hyaluronic acid (molecular weight 8kDa), 0.04 parts agarose, and 0.025 parts polyethylene glycol-4000. After stirring to dissolve, slowly pour into the S1 oil phase, emulsify at 82℃ for 18 min (speed 10000 r / min), cool to 62℃ and stir for 12 min to form a stable emulsion system.

[0021] S3. Low-temperature setting for enhanced effect: Cool the S2 emulsification system to 38℃, add 0.15 parts of grapefruit flower extract and 0.04 parts of vitamin E, stir well and pour into a hand cream container, refrigerate at 3℃ for 1.8 hours to set, restore to room temperature, sterilize by pasteurization, and cool to room temperature after sterilization to obtain the grapefruit hand cream product.

[0022] Example 2 Compared to Example 1, the following adjustments are made (unless otherwise mentioned, they are considered the same as in Example 1): 1. The raw material dosage was adjusted as follows: 3.5 parts of the first inclusion complex, 4.5 parts of the complex, 2.2 parts of the second inclusion complex, 0.16 parts of the complex microcapsules, 19 parts of winged fruit oil, 4.8 parts of beeswax, 2.2 parts of polyglycerol-6 distearate, 0.9 parts of hydrolyzed tremella polysaccharide, 0.45 parts of ceramide NP, 0.75 parts of grapefruit seed polypeptide, 0.25 parts of vitamin C palmitate, 0.09 parts of bromelain, 0.12 parts of zinc hyaluronic acid, 0.09 parts of xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid, 0.05 parts of low molecular weight hyaluronic acid, 0.12 parts of grapefruit flower extract, and 0.03 parts of vitamin E.

[0023] 2. The process parameters are adjusted as follows: (1) Preparation of the first inclusion compound: stirring temperature 60℃, stirring time 1.8h, and refrigeration for 10h; (2) Preparation of the complex: ultrasonic dispersion time 10 min, stirring temperature 50℃, stirring time 25 min; (3) Step S1: Heat to 70℃, stir at 520r / min, and stir for 35min; (4) Step S2: High-speed shearing temperature 80℃, shearing time 15min, cooling and stirring temperature 60℃, stirring time 10min; (5) Step S3: Cool the emulsion system to 36°C, refrigerate at 4°C, and set for 1.5 hours.

[0024] Comparative Example 1 Compared to Example 1, the composite microcapsules were removed, and 0.04 parts of limonene and 0.05 parts of grapefruit seed extract were added directly; the remaining raw materials, dosages, and process steps were the same as in Example 1.

[0025] Comparative Example 2 Compared to Example 1, the xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid was removed, and only 0.16 parts of xanthan gum were added; the remaining raw materials, dosages, and process steps were the same as in Example 1.

[0026] Comparative Example 3 Compared to Example 1, the hydroxypropyl-β-cyclodextrin in the first inclusion compound was replaced with an equal mass of conventional β-cyclodextrin, and the methyl-β-cyclodextrin in the second inclusion compound was replaced with an equal mass of conventional β-cyclodextrin; the remaining raw materials, dosages, and process steps were the same as in Example 1.

[0027] Comparative Example 4 Compared to Example 1, agarose and polyethylene glycol-4000 in S2 were removed; the remaining raw materials, amounts, and process steps were the same as in Example 1.

[0028] Experimental Example The hand creams prepared in Examples 1-2 and Comparative Examples 1-4 were subjected to relevant performance tests. The test results are shown in Table 1. The specific test methods are as follows: (1) Emulsion compatibility test.

[0029] Test method: Take 50g of each test sample and put them into a transparent sealed container. After filling the container, use a sterile scraper to smooth the top surface of the paste to ensure that the top surface is horizontal. Set up two parallel test groups, one group is placed in a constant temperature environment of 25℃ and the other group is placed in a low temperature environment of 5℃. Both are stored for 30 days. Observe the paste daily for any abnormal phenomena related to layering, such as surface oiling, bottom water separation, and internal clumping. The judgment of internal clumping is as follows: when observing through the transparent container, if there are hard lumps with clear boundaries from the surrounding texture, or local obvious density and lack of extensibility, it is considered clumping. If it is not clear to the naked eye, the container can be gently shaken. If there are fixed hard areas that do not follow the slight deformation of the paste as a whole, it can also be judged as clumping (it needs to be distinguished from the normal continuous texture of the paste).

[0030] Evaluation Criteria: Both 25℃ and 5℃ testing environments must be met simultaneously to determine the corresponding grade. If either environment is not met, the lowest grade will be used: Grade A (Excellent): Both groups show no surface oil seepage, bottom water separation, or internal clumping after 30 days of storage; Grade B (Acceptable): Both groups show no bottom water separation or internal clumping after 30 days of storage, with only very slight surface oil seepage (oil area ≤ 5% of the top area of ​​the paste, easily removed by gentle wiping with a sterile cotton swab, leaving no residual oil film); Grade C (Unacceptable): Any of the following situations occurs within 15 days of storage in either environment: ① Surface oil seepage area > 5% of the top area of ​​the paste or residual oil film after gentle wiping; ② Bottom water separation occurs (regardless of volume); ③ Internal clumping occurs (regardless of size).

[0031] 2. Stability test of active ingredients.

[0032] Test methods: ① The polyphenol and gingerol contents of grapefruit peel were determined at the initial value after preparation and after 60 days of storage at 25℃ in the dark. High performance liquid chromatography (HPLC, column: C18 column, 250mm×4.6mm, 5μm; mobile phase: methanol-0.1% phosphoric acid aqueous solution = 40:60; flow rate: 1.0mL / min; column temperature: 30℃; detection wavelength: polyphenols 280nm, gingerols 270nm) were used. ② The retention rates of the two components were calculated (retention rate = content after storage / initial content × 100%).

[0033] 3. Low-temperature stability and hardness test.

[0034] Test methods: ① Take 30g of each test sample, put it into a sealed container, and store it in a -5℃ low temperature storage box for 15 days. After taking it out and restoring it to room temperature, observe whether the paste maintains a uniform shape and whether there are lumps or hard bumps; ② Use a texture analyzer (probe P / 0.5R, test speed 1mm / s, compression depth 5mm, trigger force 5g) to determine the hardness value of the sample at -5℃.

[0035] 4. Low temperature and high humidity stability test.

[0036] Test method: Take 50g of each test sample, put it into a transparent sealed container, and store it in a constant temperature and humidity chamber at 5℃ and 85% relative humidity for 20 days. Observe daily whether the paste becomes thinner or water seeps out on the surface, and measure the volume of water seeping out (if any).

[0037] 5. Efficacy test for treating frostbite (only samples from Examples 1 and 2 were tested).

[0038] Test Methods: A rat frostbite model (simulating the redness, swelling, and inflammation of human frostbite) was used. Forty-eight healthy SD rats were randomly divided into three groups (n=6 per group): two sample groups (corresponding to Examples 1 and 2, respectively) and one blank control group. A rat right hind limb frostbite model was constructed using the "freezing-thawing" method (freezing at -15℃ for 30 min followed by thawing at room temperature, repeated twice; successful modeling was confirmed after 24 hours, characterized by local redness, decreased skin temperature, and increased inflammatory factors). After successful modeling, the sample groups applied 0.5g of the corresponding test sample to the frostbite site daily, while the blank control group applied an equal volume of physiological saline; both groups were treated continuously for 14 days. The following indicators were measured on days 3, 7, and 14 after application: ① Redness and swelling reduction rate: The swelling volume of the chilblain site was measured using the water displacement method, and the reduction rate was calculated (reduction rate = (initial swelling volume - swelling volume at test) / initial swelling volume × 100%); ② Inflammatory factor levels: Skin tissue from the chilblain site was taken, and the levels of inflammatory factors TNF-α and IL-6 were detected using an ELISA kit (brand: R&D Systems) (incubation conditions: 37℃ for 60 min, detection wavelength 450 nm); ③ Skin barrier repair status: Transepidermal water loss (TEWL) was measured using a transepidermal water loss meter.

[0039] Example 1: Redness and swelling reduction rate 92%, TNF-α decreased by 85%, IL-6 decreased by 83%, TEWL=13g / (h·m²); Example 2: Redness and swelling subsided by 90%, TNF-α decreased by 82%, IL-6 decreased by 80%, and TEWL was 14 g / (h·m²).

[0040] Table 1: As can be seen from Table 1: Examples 1-2 help improve the synergistic compatibility of winter hand cream components, the stability of active ingredients, and low-temperature adaptability, while also exhibiting good anti-frostbite effects. Both products achieved Grade A emulsification compatibility at both 25℃ and 5℃, with no oil seepage, water separation, or clumping. After 60 days of storage at room temperature away from light, the retention rates of polyphenols and gingerol were both ≥85%, demonstrating good stability of the active ingredients. No clumping occurred during storage at -5℃, and the hardness was ≤23g, making them suitable for low-temperature winter use. No thinning or water seepage occurred under low-temperature and high-humidity conditions at 5℃ / 85%RH, indicating excellent morphological stability. Regarding anti-frostbite efficacy, both products showed a redness and swelling reduction rate of ≥90%, a decrease in TNF-α and IL-6 of ≥80%, and a TEWL value of ≤14g / (h·m²), which can alleviate symptoms such as redness, swelling, and itching caused by frostbite, reduce inflammatory factor levels, and help repair the damaged skin barrier. Comparative Example 1 lacks the encapsulation and controlled-release effect of microcapsules: on the one hand, limonene is volatile and difficult to synergistically promote the release of active ingredients with low molecular weight hyaluronic acid; on the other hand, the free concentration of grapefruit seed extract is out of control, and excess polyphenols become oxidation substrates, accelerating the oxidative degradation of themselves and grapefruit peel polyphenols and vitamin E, leading to a decrease in the stability of active ingredients. Comparative Example 2 only adds xanthan gum, lacking the hydrophilic-lipophilic compatibility of modified colloids: its lipophilic part cannot stably bind with the oil-phase modified components, and its hydrophilic part is also difficult to form a stable moisturizing system with hydrolyzed tremella polysaccharide and low molecular weight hyaluronic acid, resulting in weakened emulsion system stability; at the same time, the moisturizing system is not stable enough, and it cannot effectively adjust the cream structure at low temperatures, easily causing clumping. In Comparative Example 3, conventional β-cyclodextrin, without hydrophilic or hydrophobic optimization, exhibited poor compatibility with encapsulated components. On one hand, it failed to effectively encapsulate grapefruit peel polyphenols, making it difficult to isolate them from the redox reaction with ginger root extract, leading to decreased stability of the active ingredients. On the other hand, it failed to simultaneously encapsulate gingerol and small beeswax molecules, failing to inhibit beeswax crystallization and easily forming hard lumps at low temperatures, affecting its suitability for application in winter. In Comparative Example 4, due to the removal of agarose and polyethylene glycol-4000, a stable gel framework could not be constructed through the synergistic effect of agarose and polyethylene glycol-4000 to lock in moisture at low temperatures. Under low-temperature, high-humidity conditions, it easily absorbed environmental moisture, causing structural imbalance in the cream, resulting in thinning and water exudation, thus compromising the product's form stability.

Claims

1. A method for preparing a grapefruit hand cream, characterized in that, Includes the following steps: S1. Preparation of the oil phase: The first inclusion compound, the complex, the second inclusion compound, winged fruit oil, beeswax, polyglycerol-6 distearate, and the composite microcapsules are mixed and stirred thoroughly to obtain the oil phase; The preparation of the first inclusion compound: ① Dissolve hydroxypropyl-β-cyclodextrin in deionized water, add grapefruit peel polysaccharide, heat and stir to dissolve, and obtain the first cyclodextrin solution; separately dissolve grapefruit peel polyphenols in ethanol, add vitamin E to form a complex solution; ② Add the composite liquid dropwise to the first cyclodextrin solution, stir, refrigerate and stand, filter and dry to obtain the product; Preparation of the complex: Grapefruit hydrosol was mixed with polyglycerol-10 laurate, grapefruit peel polysaccharide and grapefruit seed extract were added, ultrasonically dispersed, and then freeze-dried to obtain the product; Preparation of the second inclusion complex: ① Dissolve methyl-β-cyclodextrin in deionized water, add grapefruit peel polysaccharide, heat to dissolve, and then add Tween-80 to obtain a second cyclodextrin solution; separately, dissolve ginger extract and Sichuan pepper extract in ethanol to obtain an extract solution; ② Add the extract solution dropwise to the second cyclodextrin solution, stir, refrigerate and stand, filter and dry to obtain the product; The composite microcapsules are prepared from limonene, grapefruit seed extract, grapefruit peel pectin, β-cyclodextrin and calcium chloride; S2. Preparation of emulsion system: hydrolyzed tremella polysaccharide, ceramide NP, grapefruit seed polypeptide and vitamin C palmitate are added to deionized water for dissolution, followed by enzymatic hydrolysis with bromelain, then zinc hyaluronic acid and the composite system are added, stirred and dissolved, and then poured into the oil phase of S1. After high-speed shear emulsification, the emulsion system is obtained; The composite system consists of xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid, low molecular weight hyaluronic acid, agarose, and polyethylene glycol-4000; S3. Setting: Cool the S2 emulsion system, add grapefruit flower extract and vitamin E, stir well, pour into a container, refrigerate to set, and then return to room temperature to obtain the finished product.

2. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the mass ratio of each component is: first inclusion complex: complex: second inclusion complex: winged fruit oil: beeswax: polyglycerol-6 distearate: complex microcapsule = (3-5): (4-6): (2-3): (18-22): (4-7): (2-3): (0.13-0.25).

3. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the conditions for thorough stirring are: stirring at 500-600 r / min for 35-45 min at 70-75℃.

4. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the mass ratio of each component in the composite microcapsule is: limonene: grapefruit seed extract: grapefruit peel pectin: β-cyclodextrin: calcium chloride = (0.03-0.05): (0.03-0.08): (1-1.5): (1.8-2.5): (0.01-0.03).

5. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the mass ratio of each component in the preparation of the first inclusion complex is: hydroxypropyl-β-cyclodextrin: deionized water: grapefruit peel polysaccharide: grapefruit peel polyphenol: ethanol: vitamin E = (2-3): (15-20): (0.01-0.02): (2-3): (5-8): (0.1-0.2).

6. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the mass ratio of each component in the preparation of the complex is: grapefruit hydrosol: polyglycerol-10 laurate: grapefruit peel polysaccharide: grapefruit seed extract = (4-6): (3-5): (0.01-0.02): (0.1-0.2).

7. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S1, the mass ratio of each component in the preparation of the second inclusion compound is: methyl-β-cyclodextrin: deionized water: grapefruit peel polysaccharide: Tween-80: ginger extract: Sichuan pepper extract: ethanol = (2-3): (15-20): (0.01-0.02): (0.1-0.2): (1-1.5): (0.5-0.8): (5-8).

8. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S2, the mass ratio of each component is as follows: hydrolyzed Tremella polysaccharide: ceramide NP: grapefruit seed polypeptide: vitamin C palmitate: deionized water: bromelain: zinc hyaluronic acid: xanthan gum-polyethylene glycol monomethyl ether grafted modified colloid: low molecular weight hyaluronic acid: agarose: polyethylene glycol-4000 = (0.8-1.2): (0.4-0.6): (0.7-0.9): (0.2-0.4): (60-75): (0.08-0.12): (0.1-0.2): (0.08-0.12): (0.05-0.08): (0.03-0.05): (0.02-0.03).

9. The method for preparing grapefruit hand cream according to claim 1, characterized in that, In step S3, the emulsification system is cooled to 35-40℃, refrigerated at 2-5℃, and set for 1.5-2 hours.

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