Long-acting cool and refreshing resident paste based on compound matrix slow release and preparation method of long-acting cool and refreshing resident paste

Abstract

The invention discloses a long-acting cool and refreshing lingering paste based on compound matrix slow release and a preparation method thereof, and belongs to the technical field of cosmetics. The ointment body comprises 20-24 parts of beewax, 35-40 parts of a substance with an HLB (Hydrophile-Lipophile Balance) value of 12-15, 28-35 parts of a freshener and 5-7 parts of a plant extract composition. The plant extract is embedded into the matrix in the form of nano emulsion by combining staged temperature control with a nano emulsion technology. The invention has the following effects: by regulating and controlling the proportion of the beewax and the esters with high HLB (Hydrophile Lipophile Balance) value, a honeycomb porous structure is formed, and the body temperature triggered slow release of high-concentration cooling components is realized; through a low-temperature gradient process, staged temperature control (melting-> 40 DEG C emulsification) is combined with a nano-emulsification technology, and the activity of volatile components is retained (the retention rate gt is 98%). The product provided by the invention has the advantages that the cooling feeling lasts for 4-6 hours, the irritation is obviously lower than that of similar products, and the product is suitable for non-face resident type cooling and refreshing nursing for adults.

Description

Technical Field

[0001] The present invention belongs to the technical field of cosmetics, and particularly relates to a long-acting cooling and staying paste based on composite matrix sustained release and a preparation method thereof. Background Art

[0002] In modern fast-paced life, people are faced with various pressures from work, study, and life, and are prone to problems such as fatigue, drowsiness, and inattention. According to relevant survey data, among office workers, more than 80% of people report experiencing varying degrees of fatigue in their daily work. Working in front of a computer for a long time leads to difficulty in concentrating and a decrease in work efficiency. The same is true for students. Studies have shown that during the exam preparation stage, approximately 75% of students feel sleepy due to long hours of study, seriously affecting their learning effects. For drivers, fatigue driving is one of the important inducements for traffic accidents during long-distance driving. According to statistics, traffic accidents caused by fatigue driving account for about 20%. Therefore, whether it is office workers, students, or drivers, there is an urgent need for a product that can quickly refresh the mind and relieve fatigue to help them maintain a good mental state and improve work and learning efficiency.

[0003] Currently, there are many types of cooling and refreshing products on the market, such as essential balm, essential oil, and refreshing patches. However, these products generally have some deficiencies. For example: 1. When the menthol content in a commercially available cooling paste (a certain brand of mint paste) > 20%, the irritant reaction rate in human patch tests is as high as 35% (data source: J. Cosmet. Dermatol. 2023); 2. A commercially available cooling paste (a certain brand of mint paste) (such as polyacrylate) makes the paste sticky (consumer negative review rate 42%). There are also some technical defects, such as: 1. The activity loss of lavender extract > 30% under high-temperature processes; 2. The compatibility between traditional beeswax matrix and plant components is poor and prone to layering (oil phase separation rate > 15% after 3 months of accelerated testing). And some products use chemically synthesized ingredients, which may pose potential risks to human health in the long term. For example, some chemical components may cause skin allergic reactions. A survey of 1000 consumers showed that among people using cooling products containing chemically synthesized ingredients, about 15% of people have experienced varying degrees of skin allergic symptoms. Moreover, the cooling and refreshing effects of these products last for a short time and are difficult to meet long-term needs. Relevant experiments have shown that the effective action time of most traditional cooling and refreshing products can only last for 1 - 2 hours. In addition, traditional products also have defects in terms of the use experience, such as a strong greasy feeling and a pungent smell after application, which affect the user experience and social image.

[0004] To solve the above problems of existing products, the inventors of this case focused on: 1. How to achieve the slow release and low irritation of high-concentration (>30%) cooling agents (such as menthol and camphor) without adding synthetic penetration enhancers; 2. How to improve the stability and transdermal efficiency of plant extracts through matrix structure design and process optimization, and strive to develop a safer, more efficient and better user experience cooling and refreshing product. Summary of the Invention

[0005] The purpose of the present invention is to provide a long-lasting cooling and staying ointment based on the slow release of a composite matrix and its preparation method, providing a new choice for consumers, and achieving a more lasting and gentle cooling and refreshing effect through the use of natural herbal ingredients and unique formulations.

[0006] To achieve the above purpose, the technical solution of the present invention is: A long-lasting cooling and staying ointment based on the slow release of a composite matrix, in parts by weight, the ointment comprises the following components: 20 parts - 24 parts of beeswax, 35 parts - 40 parts of a substance with an HLB value of 12 - 15, 28 parts - 35 parts of a cooling agent, and 5 parts - 7 parts of a plant extract composition; The substance with an HLB value of 12 - 15 includes plant-derived PEG esters or synthetic esters. The plant-derived PEG esters include coconut oil PEG-10 esters, palm oil PEG-8 esters, castor oil PEG-12 esters, or babassu oil PEG-10 esters; the synthetic esters include PPG-15 stearyl ether or polyglycerol-6 distearate.

[0007] Further, the cooling agent includes menthol and / or camphor, and the substance with an HLB value of 12 - 15 is coconut oil PEG-10 esters; the ointment contains 20 parts - 25 parts of menthol and 8 parts - 12 parts of camphor.

[0008] Further, the plant extract composition includes at least two combinations of basil extract, aloe extract, lavender leaf extract, spearmint leaf extract, and lysimachia foenum-graecum extract.

[0009] Further, the ointment further includes 1 part - 2 parts of a preservative.

[0010] Further, the preservative includes p-hydroxyacetophenone and / or 1,2-hexanediol.

[0011] Further, by weight, the paste comprises the following components: 21.96 parts of white beeswax, 37.61 parts of coconut oil PEG-10 esters, 22.64 parts of menthol, 10.00 parts of camphor, 0.60 parts of basil extract, 0.50 parts of aloe extract, 0.70 parts of lavender leaf extract, 0.01 parts of lysimachia foenum-graecum extract, 4.50 parts of mentha spicata leaf extract, 0.49 parts of p-hydroxyacetophenone, and 0.99 parts of 1,2-hexanediol.

[0012] Further, the beeswax is white beeswax.

[0013] After adopting the above technical solution, the long-acting cooling and staying paste based on composite matrix sustained release of the present invention has the following beneficial effects: Through the specific ratio regulation of beeswax and substances with high HLB value (esters, etc.), a honeycomb-like porous structure of "rigid skeleton + flexible filling" is formed, realizing the balance between the sustained release of high-concentration cooling components and the hardness of the paste, and realizing the body temperature-triggered sustained release of high-concentration cooling components.

[0014] Further, the long-acting cooling and staying paste based on composite matrix sustained release of the present invention has the following beneficial effects: 1. Long-acting cooling and low irritation: Through the honeycomb-like porous structure design of the composite matrix of beeswax and substances with an HLB value of 12-15 (taking esters as an example), the body temperature-triggered sustained release of high-concentration cooling components (the total of menthol and camphor is 32.64%) is realized, and the cooling sensation lasts for 4-6 hours, which is significantly better than that of commercially available products (1-2 hours); Linalool in the lavender leaf extract and menthol synergistically regulate the TRPV1 receptor, reducing the erythema index by 76.8%, and the irritation reaction rate is only 6.7% (34.5% for commercially available products).

[0015] Compared with the traditional technology: The 24-hour release rate of menthol is 78% (93% for the traditional matrix), avoiding skin irritation caused by burst release.

[0016] The penetrometer value of the paste is 112 mm / 10 (GB / T 4509), which is better than that of a single beeswax matrix (68 mm / 10) and a synthetic ester matrix (189 mm / 10).

[0017] 2. Synergy of plant component stability and efficacy: As a natural chelating agent, lysimachia foenum-graecum extract binds Fe²⁺ / Cu²⁺ ions to prevent the oxidative degradation of plant components, and the retention rate of active components is >95% after 6 months; Mentha spicata leaf extract and aloe polysaccharide form an antioxidant film, reducing the secondary irritation of free radicals to the skin and improving the mildness of the product.

[0018] The lavender leaf extract, spearmint leaf extract and menthol are compounded to form a triple-effect system of "cooling - soothing - antioxidant".

[0019] Linalool in the lavender leaf extract inhibits the over-activation of TRPV1 receptors, and the calcium fluorescence signal intensity decreases by 52%; Carotenoids in the spearmint leaf extract and aloe polysaccharides form an antioxidant film to reduce the damage of free radicals to the skin.

[0020] In addition, the composite matrix regulates the hardness of the paste (penetration 112mm / 10), solid at room temperature and melts at body temperature, which is convenient to use; in addition, there is no delamination after 3 months of accelerated test at 40℃ / 75%RH, and the paste stability is significantly better than that of the traditional beeswax matrix (oil phase separation rate > 15%).

[0021] A preparation method of the long-acting cooling retention paste described above includes the following steps: Step 1: Raw material pretreatment Disperse the plant extract to form a suspension; Step 2: Matrix melting and homogenization Add beeswax and a substance with an HLB value of 12 - 15 to the reaction kettle, heat to 50 - 55℃, stir at a rate of 250rpm for 15 minutes until completely melted and form a homogeneous matrix, and the particle size of white beeswax is less than 1mm; Step 3: Loading of the cooling agent Add the cooling agent to the homogeneous matrix in Step 2, control the temperature gradient to increase ≤2℃ every 5 minutes, and the final temperature ≤55℃, stir until completely dissolved and form a transparent solution as the main phase; Step 4: Embedding of the plant extract Add the suspension in Step 1 to the main phase in Step 3, cool to below 40℃, and perform nano-emulsification with a high-shear emulsifier to form a homogeneous emulsion with a particle size D50 = 150nm; Step 5: Filling and cooling Cool the homogeneous emulsion in Step 4 to room temperature, fill it into a container, and seal it for storage.

[0022] Furthermore, during the raw material pretreatment, the plant extract and the preservative are premixed and dispersed to form a suspension.

[0023] Furthermore, during the raw material pretreatment, the beeswax is crushed to ≤1mm.

[0024] After adopting the above scheme, the preparation method of the long-acting cooling retention paste based on composite matrix sustained release of the present invention uses staged temperature control (≤55℃, melting → 40℃ emulsification) combined with nano-emulsification technology to embed the plant extract in the matrix in the form of nano-emulsion (particle size D50 = 150nm), avoiding the destruction of active ingredients at high temperature.

[0025] Furthermore, a low-temperature gradient fusion process (≤55°C) is adopted to avoid the destruction of volatile components (such as linalool) at high temperatures, and the retention rate of active ingredients > 98%; specifically, the retention rate of linalool is 99.3% (while for the traditional high-temperature process, the retention rate of linalool is 87.6%). The process energy consumption is reduced by 34% (8.2 kWh / kg vs 12.5 kWh / kg for the traditional process), meeting the requirements of green production.

[0026] In addition, the composite matrix regulates the paste hardness (penetration 112 mm / 10), solid at room temperature and melts at body temperature, which is convenient to use; in addition, there is no delamination after 3 months of accelerated test at 40°C / 75%RH, and the paste stability is significantly better than that of the traditional beeswax matrix (oil phase separation rate > 15%). BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a flow chart of the operation steps of the paste of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0028] I. Product and Preparation Example 1 A long-acting cooling and staying paste based on composite matrix sustained release according to the present invention, in parts by weight, the paste comprises white beeswax: 20 parts - 24 parts, coconut oil PEG-10 esters: 35 parts - 40 parts, menthol: 20 parts - 25 parts, camphor: 8 parts - 12 parts, plant extract combination (basil, lavender, spearmint, etc.): 5 parts - 7 parts, preservative: 1 part - 2 parts.

[0029] In the present invention, the preservative can be added or not according to the situation.

[0030] The coconut oil PEG-10 esters are substances with an HLB value of 12 - 15. Substances with an HLB value of 12 - 15 can include plant-derived PEG esters or synthetic esters. The plant-derived PEG esters include coconut oil PEG-10 esters, palm oil PEG-8 esters, castor oil PEG-12 esters or babassu oil PEG-10 esters; the synthetic esters include PPG-15 stearyl ether or polyglycerol-6 distearate. The coconut oil PEG-10 esters can be equivalently replaced by the above substances, all within the protection scope of the present invention.

[0031] The white beeswax can also be equivalently replaced by candelilla wax, carnauba wax, etc., all within the protection scope of the present invention.

[0032] The plant extract is not limited to water-soluble extracts, but can also be oil-soluble extracts.

[0033] After adopting the above solution, a long-acting cooling and staying paste based on composite matrix sustained release of the present invention has the following beneficial effects: By regulating the specific ratio of beeswax and high-HLB esters, a honeycomb-like porous structure of "rigid skeleton + flexible filling" is formed, realizing the balance between the sustained release of high-concentration cooling components and the hardness of the paste, and achieving the body temperature-triggered sustained release of high-concentration cooling components.

[0034] A preparation method of a long-acting cooling and staying paste of the present invention includes the following steps: Step 1: Raw material pretreatment Disperse and process the plant extract and the preservative to form a suspension; Step 2: Matrix melting and homogenization Add white beeswax and coconut oil PEG-10 esters to the reaction kettle, heat to 50 - 55 °C, with a stirring rate of 250 rpm for 15 min until completely melted and a homogeneous matrix is formed, and the particle size of the white beeswax is less than 1 mm; Step 3: Loading of the cooling agent Sequentially add the cooling agents menthol and camphor to the homogeneous matrix in Step 2, control the temperature gradient to increase by ≤ 2 °C every 5 minutes, and the final temperature ≤ 55 °C, and stir until completely dissolved to form a transparent solution as the main phase; Step 4: Embedding of the plant extract Add the suspension in Step 1 to the main phase in Step 3, cool to below 40 °C, and perform nano-emulsification using a high-shear emulsifier (12000 rpm, 2 min) to form a homogeneous emulsion with a particle size D50 = 150 nm.

[0035] Step 5: Filling and cooling Cool the homogeneous emulsion in Step 4 to room temperature (25 °C), fill it into aluminum tubes or plastic containers, and seal and store.

[0036] After adopting the above solution, a preparation method of a long-acting cooling and staying paste based on composite matrix sustained release of the present invention uses staged temperature control (≤ 55 °C, melting → 40 °C emulsification) combined with nano-emulsification technology to embed the plant extract in the matrix in the form of a nano-emulsion (particle size D50 = 150 nm), avoiding the destruction of active ingredients at high temperatures.

[0037] Example 2 A long-acting cooling and staying paste based on composite matrix sustained release of the present invention, the composition of the paste and the functions of each component are specifically as shown in Table 1 below:

[0038] It should be noted that in the present invention, each component can be obtained by purchasing on the market.

[0039] The present invention relates to a long-acting cooling and staying ointment based on a composite matrix sustained release, which has the following beneficial effects: 1. Long-acting cooling and low irritation: Through the honeycomb-like porous structure design of the beeswax-ester composite matrix, the body temperature-triggered sustained release of high-concentration cooling components (a total of 32.64% of menthol + camphor) is achieved, and the cooling sensation lasts for 4-6 hours, significantly better than commercially available products (1-2 hours); Linalool in the lavender leaf extract and menthol synergistically regulate the TRPV1 receptor, reducing the erythema index by 76.8%, and the irritation reaction rate is only 6.7% (34.5% for commercially available products).

[0040] Compared with traditional technologies: the 24-hour release rate of menthol is 78% (93% for traditional matrices), avoiding skin irritation caused by burst release.

[0041] The penetration of the ointment is 112 mm / 10 (GB / T 4509), which is better than that of a single beeswax matrix (68 mm / 10) and a synthetic ester matrix (189 mm / 10).

[0042] 2. Synergy of plant component stability and efficacy: The lysimachia foenum-graecum extract (0.01%) acts as a natural chelating agent, binding Fe²⁺ / Cu²⁺ ions to prevent the oxidative degradation of plant components, and the retention rate of active components is >95% after 6 months; The mentha spicata leaf extract (4.5%) and aloe polysaccharide form an antioxidant film to reduce the secondary irritation of free radicals to the skin and improve the mildness of the product.

[0043] The lavender leaf extract (0.7%), mentha spicata leaf extract (4.5%) and menthol are compounded to form a "cooling - soothing - antioxidant" triple efficacy system.

[0044] Linalool in the lavender leaf extract inhibits the over-activation of the TRPV1 receptor, and the calcium fluorescence signal intensity is reduced by 52%; Carotenoids in the mentha spicata leaf extract and aloe polysaccharide form an antioxidant film to reduce the damage of free radicals to the skin.

[0045] The preparation method of a long-acting cooling and staying ointment based on a composite matrix sustained release of the present invention As Figure 1 shown, it includes the following steps: Step 1: Raw material pretreatment Crush white beeswax to a particle size ≤1 mm and set aside; Premix the plant extracts (basil extract, lavender leaf extract, mentha spicata leaf extract, lysimachia foenum-graecum extract) and preservatives (p-hydroxyacetophenone, 1,2-hexanediol), and disperse (40 kHz, 10 min) to form a homogeneous suspension.

[0046] Step 2: Matrix Melting and Homogenization Add white beeswax (21.96%) and PEG - 10 esters of coconut oil (37.61%) to the reaction kettle, heat to 50 - 55 °C, with a stirring rate of 250 rpm for 15 min until completely melted and a homogeneous matrix is formed.

[0047] Step 3: Loading of Cooling Agents Add menthol (22.64%) and camphor (10.00%) in sequence, control the temperature gradient to increase by ≤2 °C every 5 minutes, with a final temperature ≤55 °C, and stir until completely dissolved to form a transparent solution.

[0048] Step 4: Embedding of Plant Extracts Slowly add the premixed plant extract and preservative suspension to the main phase, cool to below 40 °C, and perform nano - emulsification using a high - shear emulsifier (12000 rpm, 2 min) to form a homogeneous emulsion with a particle size D50 = 150 nm.

[0049] Step 5: Filling and Cooling Cool the paste to room temperature (25 °C), fill it into aluminum tubes or plastic containers, and store it sealed.

[0050] After adopting the above - mentioned scheme, the preparation method of a long - acting cooling and staying ointment based on a composite matrix sustained release of the present invention has the following beneficial effects: 1. Long - acting Cooling and Low Irritation: Through the honeycomb - like porous structure design of the beeswax - ester composite matrix, the body - temperature - triggered sustained release of high - concentration cooling components (a total of 32.64% of menthol + camphor) is achieved, and the cooling sensation lasts for 4 - 6 hours, significantly better than commercially available products (1 - 2 hours); Linalool in lavender leaf extract and menthol synergistically regulate the TRPV1 receptor, reducing the erythema index by 76.8%, and the irritation reaction rate is only 6.7% (34.5% for commercially available products).

[0051] 2. Synergy of Plant Component Stability and Efficacy: Lysimachia foenum - graecum Hance extract (0.01%) as a natural chelating agent binds Fe²⁺ / Cu²⁺ ions to prevent the oxidative degradation of plant components, and the retention rate of active components is >95% after 6 months; Spearmint leaf extract (4.5%) and aloe polysaccharide form an antioxidant film to reduce the secondary irritation of free radicals to the skin and improve the mildness of the product.

[0052] 3. Process Energy Saving and Active Retention: Adopt a low-temperature gradient fusion process (≤55°C) to avoid the destruction of volatile components (such as linalool) at high temperatures, with the retention rate of active ingredients > 98%; specifically, the retention rate of linalool is 99.3% (while for the traditional high-temperature process, the retention rate of linalool is 87.6%). The process energy consumption is reduced by 34% (8.2 kWh / kg vs 12.5 kWh / kg for the traditional process), meeting the requirements of green production.

[0053] In addition, adopt staged temperature control (≤55°C, melting at 50°C → emulsifying at 40°C) combined with nanoemulsion technology to embed plant extracts in the matrix in the form of nanoemulsions (particle size D50 = 150 nm), avoiding the destruction of active ingredients at high temperatures.

[0054] 4. Paste stability and usage experience: The composite matrix regulates the hardness of the paste (penetration 112 mm / 10), solid at room temperature and melts at body temperature, making it convenient to use; in addition, there is no delamination after 3 months of accelerated testing at 40°C / 75% RH, and the paste stability is significantly better than that of the traditional beeswax matrix (oil phase separation rate > 15%).

[0055] In summary, through triple innovations in the design of the composite matrix structure, the synergistic anti-allergic effect of plant components, and the optimization of the low-temperature gradient process, the present invention solves the problems of irritation, stability, and efficacy persistence of high-concentration cooling agent retention products, and has significant technological progress and market application value.

[0056] Some technical improvement points of the present invention are compared with the prior art in Table 2 below:

[0057] Comparative Example 1: Remove all plant extracts, and keep the remaining components, addition amounts, and processes the same as in Example 2.

[0058] Comparative Example 2: Remove lavender leaf extract, lysimachia foenum-graecum extract, basil extract, aloe extract, mentha spicata leaf extract, and camphor. Keep the remaining components, addition amounts, and processes the same as in Example 2.

[0059] Comparative Example 3: Remove lysimachia foenum-graecum extract, basil extract, aloe extract, mentha spicata leaf extract, menthol, and camphor. Keep the remaining components, addition amounts, and processes the same as in Example 2.

[0060] Comparative Example 4: Remove lysimachia foenum-graecum extract, basil extract, aloe extract, mentha spicata leaf extract, and camphor. Keep the remaining components, addition amounts, and processes the same as in Example 2.

[0061] Comparative Example 5: The addition amount of beeswax was set as a variable, which were 18 parts, 20.0 parts, 21.96 parts (the above Example 2), 24.0 parts, and 26.0 parts respectively, and the remaining components, addition amounts, and processes remained unchanged. The effects on the hardness, moisture permeability, stability, and cool feeling of the paste were investigated.

[0062] Comparative Example 6: Coconut oil in the formula was deleted, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0063] Comparative Example 7: Coconut oil PEG-10 esters in the formula were replaced with isopropyl palmitate, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0064] In Comparative Example 8, coconut oil PEG-10 esters were replaced with mineral oil, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0065] Comparative Example 9: Lavender extract was removed, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0066] Comparative Example 10: Spearmint leaf extract was removed, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0067] Comparative Example 11: All extracts were removed, and the remaining components, addition amounts, and processes were the same as those in Example 2 and remained unchanged.

[0068] Comparative Example 12: It was the same as Example 2, but a conventional high-temperature melting process was adopted. The specific steps were as follows: at 75 - 85 °C, the matrix raw materials were added and mixed evenly to dissolve. After homogenization, the temperature was lowered to 60 - 65 °C, and then the cooling agent, plant extract, and preservative were added in sequence and mixed evenly. There was no low-temperature gradient fusion during the process. The experimental results are shown in Table 3 below:

[0069] II. Performance Testing Experiment 1 (I) Experimental Basis and Standards 1. Paste hardness: According to GB / T 4509-2010 "Determination Method for Penetration of Petroleum Asphalt".

[0070] 2. Moisture permeability: According to GB / T 12704.1-2009 "Textiles - Test Method for Moisture Permeability of Fabrics - Part 1: Moisture Absorption Method".

[0071] 3. Stability: Refer to the accelerated test conditions (40 °C / 75%RH, 3 months) in the "Technical Specifications for Cosmetics Safety" (2015 Edition).

[0072] 4. Erythema Index: According to GB / T 17149.2-1997 "Evaluation of Cosmetic Skin Adverse Reactions - Human Patch Test Method".

[0073] (II) Experimental Equipment and Materials 1. Penetrometer: Shanghai Changji NDJ-1 type penetrometer (standard needle weight 100g, constant temperature at 25°C).

[0074] 2. Moisture Permeability Tester: Shanghai Hengping BSH-100 type moisture permeability tester (in an environment of 38°C / 90%RH).

[0075] 3. Thermo-Hygrostat: ESPEC SH-641 type made in Japan (40°C / 75%RH).

[0076] 4. Skin Tester: German CK MPA580 type skin physiological tester (for measuring erythema index).

[0077] (III) Experimental Methods and Data 1. Paste Preparation Method: 2. Paste Hardness Test (Penetration Method) 2.1. Fill the paste sample into the standard penetrometer mold (diameter 50mm, height 30mm), and keep it at a constant temperature of 25°C for 24 hours.

[0078] 2.2. The standard needle (100g) of the penetrometer is vertically inserted into the surface of the paste, and the penetration depth (unit: 0.1mm) is read after 5 seconds.

[0079] 2.3. Each group of samples is tested 5 times, and the data is taken as the average value ± standard deviation Data Recording: Meaning of plus and minus signs: The ± value is the standard deviation, indicating the degree of dispersion of multiple measurements (for example, 112±1mm means the measured value fluctuates between 111 - 113mm).

[0080] 3. Moisture Permeability Rate Test (Moisture Absorption Method) Method: 3.1. Evenly coat the paste on the moisture permeability cup (diameter 30mm, area 0.0007m²), with a thickness of 1mm.

[0081] 3.2. Set the moisture permeability tester in an environment of 38°C / 90%RH, place it for 24 hours, and weigh the change in the weight of the moisture permeability cup.

[0082] 3.3. Moisture Permeability Rate Calculation Formula:

[0083] 3.4. Each group of samples is tested 3 times, and the data is taken as the average value ± standard deviation 4. Stability Test (Accelerated Test) Method: 4.1. The paste samples are placed in a thermo-hygrostat (40 °C / 75% RH) for 3 months.

[0084] 4.2. Observe the layering, oil leakage, color change, etc. of the paste, and calculate the stability (100% for no abnormal phenomena).

[0085] Repeat the test 3 times for 4.3 groups of samples, and the data is taken as the average value ± standard deviation 5. Erythema Index Test (Human Patch Test) Method: 5.1. Apply 0.1 g of the paste to the inner forearm of the subjects (30 healthy adults), and cover with a patch (2 cm × 2 cm).

[0086] 5.2. Remove the patch after 24 hours, and use a skin tester (MPA580) to measure the percentage of erythema area.

[0087] 5.3. Erythema index calculation formula:

[0088] 5.4. The data is taken as the average value ± standard deviation Experimental methods and data (*The plus-minus sign (±) in the data represents the standard deviation of the experimental results, reflecting the dispersion degree of the experimental data.) are shown in Table 4 below:

[0089] 6. Result Analysis 6.1. Paste hardness: The beeswax content is negatively correlated with the penetration. When the content is 21.96 parts, the hardness is moderate (112 mm / 10), meeting the requirements of GB / T 4509.

[0090] Too low content (18 parts) results in too soft paste (150 mm / 10), and too high content (26 parts) makes it too hard (80 mm / 10), affecting the user experience.

[0091] 6.2. Moisture permeability: As the beeswax content increases, the moisture permeability decreases significantly. When the content is 21.96 parts, the moisture permeability is 25 g / m²·24 h, balancing the breathability and sustained-release requirements.

[0092] Too high content (26 parts) leads to too low moisture permeability (15 g / m²·24 h), which may hinder normal skin respiration.

[0093] 6.3. Stability: The stability is optimal when the beeswax content is 21.96 parts (100% without delamination). When deviating from this ratio, the stability decreases (e.g., only 85% when it is 18 parts).

[0094] When the beeswax content is too high (26 parts), due to the excessive rigidity of the matrix, slight cracking occurs after the accelerated test (stability 90.3%).

[0095] 6.4. Erythema index: When the beeswax content is 21.96 parts, the erythema index is the lowest (8.0%), verifying the sustained-release and anti-allergic advantages of the composite matrix.

[0096] When the content is too low (18 parts), it causes the sudden release of the cooling agent, and the erythema index rises to 18.5%; when the content is too high (26 parts), due to insufficient release of plant components, the anti-allergic effect weakens, and the erythema index rebounds to 15.2%.

[0097] Conclusion When the beeswax content is 21.96 parts, the paste hardness, moisture permeability, stability and anti-allergic properties all reach the optimal balance, verifying the scientificity and necessity of the composite matrix design.

[0098] Experiment 2 Example 2 and Comparative Examples 6 - 8 verify the key role of coconut oil PEG - 10 esters in the composite matrix, and compare the effects of different matrices (without esters, isopropyl palmitate, mineral oil) on the paste properties.

[0099] (I) Experimental basis and standards 1. Penetration: GB / T 4509 - 2010 "Determination Method for Penetration of Petroleum Asphalt" 2. 24 - hour release rate of menthol: Franz diffusion cell method (simulating skin temperature at 32°C, receptor fluid is physiological saline) 3. Stability (40°C / 3M): Refer to the accelerated test conditions of "Technical Specifications for Cosmetics Safety" (2015 edition) (II) The experimental equipment and materials are as follows in Table 5:

[0100] (III) The experimental group design is as follows in Table 6:

[0101] (IV) Experimental procedures 1. Paste preparation (uniform process parameters) Raw material pretreatment: The beeswax is crushed to ≤1 mm, and the plant extract is ultrasonically dispersed (40 kHz, 10 min).

[0102] Melting and homogenization: The beeswax and esters are heated to 50 - 55°C and stirred at 250 rpm for 15 min.

[0103] Loading cooling agent: Add menthol (22.64 parts) and camphor (10.00 parts), and dissolve them while controlling the temperature ≤ 55°C.

[0104] Embedding plant extract: High-shear emulsification (12000 rpm, 2 min) at a temperature below 40°C.

[0105] 2. Penetration test Method: According to GB / T 4509-2010, keep the temperature constant at 25°C, the standard needle weighs 100 g, and the data is averaged ± standard deviation after 5 repetitions.

[0106] 3. 24-hour release rate test of menthol Method: 3.1. Uniformly coat the paste on the donor chamber of the Franz diffusion cell (thickness 0.5 mm), and the receptor fluid is physiological saline (kept at a constant temperature of 32°C).

[0107] 3.2. After 24 hours, take the receptor fluid and detect the menthol concentration by HPLC (chromatographic conditions: C18 column, mobile phase methanol:water = 70:30, flow rate 1 mL / min, detection wavelength 210 nm).

[0108] 3.3. Release rate calculation formula:

[0109] 3.4. Stability test (40°C / 3M) Method: Place the paste sample in a thermo-hygrostat (40°C / 75%RH) for 3 months, observe the phenomena of delamination and oil leakage, and calculate the stability (100% if there is no abnormality).

[0110] (V) The experimental data are shown in Table 7 below

[0111] (VI) Data analysis and conclusion 1. Penetration difference Example 2 (112 mm / 10): Beeswax and coconut oil PEG-10 esters (HLB = 13.5) form a honeycomb structure of "rigid skeleton + flexible filling", with moderate hardness.

[0112] Comparative Example 6 (68 mm / 10): Without ester filling, only the beeswax matrix is too rigid, and the paste is too hard (defect of the traditional beeswax matrix).

[0113] Comparative Example 7 (189 mm / 10): Isopropyl palmitate (HLB = 6) has poor compatibility with beeswax, forms a loose structure, and the paste is too soft.

[0114] Comparative Example 8 (155 mm / 10): Mineral oil is non-polar and cannot form a porous sustained-release structure, resulting in unbalanced hardness.

[0115] 2. Difference in menthol release rate Example 2 (78%): The honeycomb structure has a significant sustained-release effect, and the release rate is controllable within 24 hours.

[0116] Comparative Example 6 (93.5%): The low porosity of the non-ester matrix leads to the burst release of menthol (high risk of irritation).

[0117] Comparative Example 7 (65.2%): The poor compatibility between isopropyl palmitate and beeswax results in a dense structure that hinders release (insufficient cooling sensation).

[0118] Comparative Example 8 (71.3%): Mineral oil forms a closed film layer, and the release rate is uneven.

[0119] 3. Difference in stability Example 2 (100%): The composite matrix structure is stable, without stratification or oil leakage.

[0120] Comparative Example 6 (82.5%): Due to the difference in thermal expansion coefficient of the single beeswax matrix, oil phase separation occurs after the accelerated test.

[0121] Comparative Example 7 (88%): Isopropyl palmitate softens the paste at high temperatures, resulting in structural collapse.

[0122] Comparative Example 8 (90.5%): Poor compatibility between mineral oil and plant components, with slight oil leakage.

[0123] 4. Conclusion The high HLB value (13.5) and polar characteristics of coconut oil PEG-10 esters are the key to forming a honeycomb-like sustained-release structure. Its specific ratio with beeswax (1:1.71) achieves the optimal balance of hardness, sustained-release property, and stability. Replacing or deleting coconut oil PEG-10 esters will lead to a significant decline in the performance of the paste, verifying the necessity and innovation of the composite matrix design. Through comparative experiments, the irreplaceability of coconut oil PEG-10 esters in the formula of the present invention is clarified, providing core data support for the technical solution of the present invention, while revealing the defects of the prior art (single beeswax or low HLB esters) and highlighting the technical progress of the present invention.

[0124] Experiment 3 Experiments on Example 2, Comparative Examples 1-4, Comparative Examples 9-11, and the competitor group: Verify the synergistic anti-allergic effect of plant extracts (lavender, spearmint, etc.) and the sustained-release performance of the composite matrix, TRPV1 receptor inhibition and antioxidant efficacy, and compare the effects of different formulations on the erythema index, irritation response rate, duration and intensity of the cooling sensation.

[0125] (I) Experimental basis and standards 1. Erythema index: GB / T 17149.2-1997 "Evaluation of Cosmetic Skin Adverse Reactions - Human Patch Test Method" 2. TRPV1 receptor activity (calcium fluorescence signal): ISO 10993-22:2017 "Biological Evaluation of Medical Devices - Part 22: Detection of Cellular Signaling Pathways" 3. Free radical scavenging rate: GB / T 27579-2011 "Test Method for Antioxidant Properties of Cosmetics (DPPH Method)" 4. Cooling sensation duration and intensity: Cooling sensation evaluation: ISO 21331:2018 "Sensory Analysis - Guidelines for Quantitative Evaluation of Product Use Effects" (Subjective scoring by subjects, recorded using a standardized questionnaire) 5. Erythema index and irritation reaction rate: GB / T 17149.2-1997 "Evaluation of Cosmetic Skin Adverse Reactions - Human Patch Test Method" 6. Competing product control group: 30% menthol aqueous solution commercially available (simulating traditional highly irritating cooling products) (2) The experimental equipment and materials are as shown in Table 8 below

[0126] (3) The experimental group design is as shown in Table 9 below

[0127] (4) Experimental procedures 1. Sample preparation Prepare pastes according to the formulations of Example 2, Comparative Examples 1-4, and Comparative Examples 9-11 (the process is the same as before). For the competing product group, directly use 30% menthol aqueous solution

[0128] All samples are pretreated for accelerated stability (40°C / 75% RH, 3 months).

[0129] 2. Erythema index test Method: 2.1. Apply 0.1 g of the sample to the inner forearm of the subjects (30 healthy adults), and cover with a patch (2 cm × 2 cm).

[0130] 2.2. Remove the patch after 24 hours, and use a skin tester to measure the percentage of erythema area

[0131] 2.3. Erythema index calculation formula:

[0132] 3. Cooling sensation duration and intensity test Method: 3.1. Apply 0.1 g of the sample to the other forearm of the subjects (30 subjects in the same batch), and record the initial time of the cooling sensation.

[0133] 3.2. Ask the subjects about the intensity of the cooling sensation every 30 minutes (0 - 10 points, with 10 being the strongest) until the cooling sensation disappears (the duration is the end point).

[0134] 3.3. The data is taken as the mean ± standard deviation.

[0135] 4. TRPV1 Receptor Activity Test (Calcium Fluorescence Signal) 4.1 Method: TRPV1 cell type (HaCaT human keratinocytes), culture conditions (DMEM medium, 37 °C / 5% CO2), Inoculate into a 96 - well plate (density 1×10 4 / well).

[0136] Add the sample (0.1% concentration) and incubate for 24 h.

[0137] Load the Fluo - 4 AM fluorescent probe (5 μM), and detect the calcium signal intensity with a fluorescence microscope (excitation / emission wavelength 488 / 516 nm).

[0138] 4.2 Calculate the calcium signal inhibition rate:

[0139] 5. Free Radical Scavenging Rate Test (DPPH Method) 5.1 Method: Prepare a 0.1 mM DPPH ethanol solution.

[0140] Mix the sample (1 part of the extract solution) with the DPPH solution in equal volume and react in the dark for 30 min.

[0141] 5.2 Measure the absorbance at 517 nm with a spectrophotometer and calculate the scavenging rate:

[0142] (V) The experimental data is as shown in Table 10

[0143] (VI) Data Analysis and Conclusion 1. Erythema Index Example 2 is the lowest (8.0%): The synergy of lavender (linalool) and spearmint (antioxidant) inhibits the activation of TRPV1 receptors and reduces skin irritation.

[0144] Control 9 (12.4%): The absence of lavender leads to weakened TRPV1 regulation and a 52% increase in the erythema index.

[0145] Comparative Example 10 (10.8%): Lack of spearmint antioxidant film, increased free radical damage, and the erythema index is higher than that of Example 2.

[0146] The highest in the competitor group (34.5%): 30% of menthol is released suddenly, without anti-allergic components, and the irritation is significant.

[0147] 2. Duration of the cooling sensation The longest in Example 2 (4.8 h): The composite matrix slowly releases menthol, and the plant components prolong the cooling sensation.

[0148] Comparative Examples 1-2 (3.2 - 4.1 h): Without the synergistic effect of plants, the attenuation of the cooling sensation is accelerated.

[0149] The shortest in the competitor group (1.5 h): The aqueous solution has no slow release, and menthol volatilizes rapidly.

[0150] 3. Intensity of the cooling sensation The highest in the competitor group (9.5 points): High-concentration menthol has strong instantaneous irritation, but the duration is short.

[0151] Example 2 (8.5 points): The slow-release design reduces the initial intensity, but has better persistence.

[0152] Comparative Example 3 (0 points): Without menthol, there is no cooling effect.

[0153] 4. Multi-target synergistic mechanism: Example 2: Lavender (linalool) inhibits the TRPV1 receptor (a 52% reduction in calcium signal), spearmint scavenges free radicals (87.3%), and the erythema index of 8.0% is the lowest value.

[0154] Comparative Example 9 (without lavender): Only spearmint has antioxidant activity (87.0%), but the calcium signal inhibition rate is only 10.1%, and the erythema index rises to 12.4%, proving that TRPV1 regulation is indispensable.

[0155] Comparative Example 10 (without spearmint): Lavender inhibits TRPV1 (51.8%), but the free radical scavenging rate is only 16.5%, and the erythema index is 10.8%, indicating that the antioxidant film is also crucial for reducing irritation.

[0156] 5. Dose-effect relationship: Comparative Example 4 (halving the ingredients): Both the calcium signal inhibition rate (29.6%) and the free radical scavenging rate (62.4%) decrease, and the erythema index (14.2%) increases, proving that sufficient amounts of lavender and spearmint need to be added.

[0157] 6. Comparison with traditional competitors: Competitor group: Relying on synthetic penetration enhancers (azone), without TRPV1 inhibition and antioxidant capabilities, the erythema index is 34.5% at the highest, and the irritation reaction rate is 34.5%.

[0158] Example 2: The synergistic effect of natural ingredients reduces the erythema index by 76.8%, and the irritation reaction rate is only 1 / 5 of that of the competitor.

[0159] Conclusion Plant synergy for anti-allergy: Lavender (TRPV1 regulation) and spearmint (antioxidation) are both indispensable. The absence of any ingredient will significantly increase the erythema index (Comparative Examples 9-10). Composite matrix sustained release: The honeycomb structure of coconut oil PEG-10 esters prolongs the cooling time and avoids burst release irritation (Example 2 vs. competitor group). Defects of competitors: Although commercially available high-concentration menthol products have high initial strength, they have high irritation (erythema index 34.5%) and short duration (1.5 h), verifying the technical advantages of the present invention. Through systematic comparative experiments, the dual necessity of the composite matrix sustained release design and the plant synergy anti-allergy mechanism in the formula of the present invention is confirmed, and at the same time, the technical defects of traditional high-concentration cooling products are revealed, providing direct evidence for the innovation of the present invention.

[0160] The present invention focuses on the long-term pain points commonly existing in traditional cooling and refreshing products, such as high irritation, short efficacy, and poor stability. Through the breakthrough of three core technologies, namely "composite matrix sustained release technology", "plant synergy anti-allergy system", and "low-temperature gradient process", significant innovation and practical value of the technical solution are achieved. First, the composite matrix design of beeswax and high-HLB value esters (coconut oil PEG-10) (ratio 1:1.71) successfully constructs a honeycomb-like porous structure, breaking through the performance limitations of traditional single matrices. Experimental data show that this structure reduces the 24-hour release rate of menthol to 78% (93% for traditional matrices), effectively solving the skin irritation problem caused by the burst release of high-concentration cooling agents (32.64 parts). Secondly, the multi-target synergistic mechanism of lavender leaf extract (linalool) and spearmint leaf extract shows a significant anti-allergy effect. Linalool can target and inhibit the over-activation of TRPV1 receptors (calcium signal reduced by 52%), combined with the antioxidant film formed by spearmint leaf extract (free radical scavenging rate > 85%), reducing the erythema index from 34.5% of commercially available products to 8.0% significantly, opening up a technical path for natural ingredients to replace synthetic penetration enhancers. Moreover, the developed low-temperature gradient fusion process (≤55 °C) combined with nanoemulsion technology achieves a volatile component retention rate > 98% (12.4% loss in traditional processes), while reducing energy consumption by 34%. This process breakthrough solves the problem of the destruction of plant active ingredients by high-temperature processing, taking into account both production energy conservation and efficacy guarantee.

[0161] Through the "slow-release-anti-allergy-antioxidation" linkage mechanism of the composite matrix and plants, the product's cooling effect lasts for 4.8 hours (commercially available products are 1.5 hours), and the paste has no stratification in the 3-month accelerated test at 40°C, and the stability is improved to 100% (the traditional beeswax matrix oil phase separation rate is >15%), and the technical indicators are fully superior to the existing solutions. Human trials show that the irritation reaction rate of the product of the present invention is only 6.7% (commercially available products are 34.5%), which is suitable for people with sensitive skin and fills the market gap of high cooling demand and low irritation compatibility.

[0162] In addition, the paste is solid at room temperature and melts at body temperature (needle penetration 112mm / 10), which ensures the portability of the product and the non-sticky feeling during use, accurately meeting the needs of office workers, students, drivers and other groups for long-term refreshment. The reduction of process energy consumption and the use of natural plant ingredients are in line with the development trend of "streamlining ingredients and being environmentally friendly" in the cosmetics industry. Compared with the commercially available 30% menthol aqueous solution, the product of the present invention reduces the erythema index by 76.8% while maintaining the cooling intensity (score 8.5 / 10), extends the cooling time by 3 times, and has no irritating odor. A third-party survey shows that consumers' dissatisfaction with the stickiness (negative review rate 42%) and short-term effectiveness (negative review rate 68%) of traditional products has been fundamentally improved in this solution.

[0163] In summary, the present invention overcomes the industry difficulties of high-concentration cooling agent resident products through the integration of original technologies, combines technological innovation with market applicability, provides a safe, long-lasting and green solution for the cosmetics field, and has clear industrial transformation prospects and social benefits.

[0164] The above embodiments and drawings do not limit the product form and style of the present invention. Any appropriate changes or modifications made thereto by ordinary technicians in the relevant technical field should be deemed to be within the patent scope of the present invention.

Claims

1. A long-acting cooling and staying paste based on composite matrix sustained release, characterized in that: By weight, the paste comprises the following components: 20 to 24 parts of beeswax, 35 to 40 parts of a substance with an HLB value of 12 - 15, 28 to 35 parts of a cooling agent, and 5 to 7 parts of a plant extract composition; The substance with an HLB value of 12 - 15 includes plant-derived PEG esters or synthetic esters. The plant-derived PEG esters include coconut oil PEG-10 esters, palm oil PEG-8 esters, castor oil PEG-12 esters, or babassu oil PEG-10 esters; the synthetic esters include PPG-15 stearyl ether or polyglycerol-6 distearate.

2. The long-acting cooling and staying paste according to claim 1, wherein: The substance with an HLB value of 12 - 15 is coconut oil PEG-10 esters; the cooling agent includes menthol and / or camphor, and the paste contains 20 to 25 parts of menthol and 8 to 12 parts of camphor.

3. The long-acting cooling and staying paste according to claim 1, wherein: The plant extract composition includes at least two combinations of basil extract, aloe vera extract, lavender leaf extract, spearmint leaf extract, and lysimachia foenum-graecum extract.

4. The long-acting cooling and staying paste according to claim 1, wherein: The paste further includes 1 to 2 parts of a preservative.

5. The long-acting cooling and staying paste according to claim 4, characterized in that: The preservative includes p-hydroxyacetophenone and / or 1,2-hexanediol.

6. The long-acting cooling and staying paste according to claim 1, wherein: By weight, the paste comprises the following components: 21.96 parts of white beeswax, 37.61 parts of coconut oil PEG-10 esters, 22.64 parts of menthol, 10.00 parts of camphor, 0.60 parts of basil extract, 0.50 parts of aloe vera extract, 0.70 parts of lavender leaf extract, 0.01 parts of lysimachia foenum-graecum extract, 4.50 parts of spearmint leaf extract, 0.49 parts of p-hydroxyacetophenone, and 0.99 parts of 1,2-hexanediol.

7. The long-acting cooling and staying paste according to claim 1, wherein: The beeswax is white beeswax.

8. A method for preparing a long-acting cooling and staying paste as described in any one of claims 1 - 7, characterized in that, It includes the following steps: Step 1: Raw material pretreatment Disperse and process the plant extract to form a suspension; Step 2: Matrix melting and homogenization Add beeswax and the substance with an HLB value of 12 - 15 to a reaction kettle, heat to 50 - 55 °C, with a stirring rate of 250 rpm for 15 min until completely melted and a homogeneous matrix is formed, and the particle size of white beeswax is less than 1 mm; Step 3: Cooling agent loading Add the cooling agent to the homogeneous matrix in Step 2, control the temperature gradient to increase by ≤2 °C every 5 minutes, and the final temperature ≤55 °C, and stir until completely dissolved to form a transparent solution as the main phase; Step 4: Embedding of plant extract Add the suspension in Step 1 to the main phase in Step 3, cool down to below 40 °C, and perform nano-emulsification using a high-shear emulsifier to form a homogeneous emulsion with a particle size D50 = 150 nm; Step 5: Filling and cooling Cool the homogeneous emulsion in Step 4 to room temperature, fill it into a container, and seal it for storage.

9. The preparation method of the long-acting cooling and staying paste according to claim 8, characterized in that: During raw material pretreatment, premix and disperse the plant extract and the preservative to form a suspension.

10. The preparation method of the long-acting cooling and staying paste according to claim 8, characterized in that: During raw material pretreatment, crush the beeswax to ≤1 mm.

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