A cooling agent composition, its preparation and use

Abstract

The application belongs to the technical field of nursing products, and particularly discloses a cooling agent composition, a preparation method and application thereof; the cooling agent composition is prepared from the following raw materials in a total mass fraction of 100%: 76-95.29% of 1,3-propanediol, 2-9% of methyl diisopropylpropionamide, 2-8.5% of menthane formyl ethylamine, 0.5-3.5% of hydroxypropyl cellulose, 0.1-2% of hydroxypropyl-beta-cyclodextrin, 0.1-2% of borneol and 0.01-1% of oil and fat. The cooling agent composition provided by the application has the characteristics of long-lasting cooling sensation and good stability; the preparation process of the cooling agent composition is simple, the cost is controllable, and the industrialized production is easy.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of nursing products, and particularly relates to a cooling agent composition and a preparation method and application thereof. BACKGROUND

[0002] With the improvement of people's living standards and the increasing demand for comfort, textiles, personal care products (such as skin care products, shampoos, wet wipes), plastic products, etc. with cooling function are increasingly popular in the market; the core of giving these products a cooling feeling is to add a cooling agent ingredient with a cooling feeling. At present, the mainstream cooling agents on the market can be divided into two categories: the first category is represented by menthol and its derivatives (such as menthyl lactate, WS-3, etc.) natural or synthetic cooling substances; this kind of substance activates the transient receptor potential M8 (TRPM8) cold receptor on the human skin, producing a sharp and rapid cooling sensation. The second category is represented by N-ethyl-p-menthane-3-carboxamide (WS-23), dimethyl heptanedioate, etc. as a representative of synthetic high-efficiency cooling agent. They also act on the TRPM8 receptor, but usually have a more pure and intense cooling than menthol, and do not have the pungent taste and irritation of menthol.

[0003] The above-mentioned traditional cooling agents have been widely used in many fields. For example, in the textile industry, microencapsulated menthol or WS-23 is attached to the surface of the fiber through the finishing process; in the daily chemical industry, it is directly added to the formula to provide an instant cooling experience when the product is used. Although the above-mentioned traditional cooling agents have been widely used, they still have some inherent technical defects that need to be solved urgently, mainly in the two aspects of cooling duration and application stability:

[0004] 1) Short cooling duration, unable to achieve long-acting cooling: whether it is menthol or WS-23 and other synthetic cooling agents, their mechanism of action is to rapidly bind to the receptors on the surface of the skin and quickly dissociate. This process results in a fast and fast cooling. Especially after the textile is washed several times or the daily chemical product is applied to the skin and rubbed, the cooling effect will be sharply attenuated, which cannot meet the consumer's demand for "long-acting" or "continuous" cooling.

[0005] 2) Volatile and migratory, leading to unstable product efficacy: most small molecule cooling agents have high volatility (such as menthol) or strong migration. During storage, the effective ingredients will gradually volatilize and lose from the product matrix (such as fabric, paste); during use, they are also easily lost due to friction and sweat flushing. This not only shortens the effective life of the product, but also leads to a huge difference in cooling intensity between the initial and later stages of use, resulting in inconsistent user experience.

[0006] 3) Compatibility issues with substrates: Some synthetic cooling agents may have poor compatibility in certain application scenarios (such as in specific plastic or chemical fiber materials), which may lead to precipitation, frosting and other phenomena, affecting the appearance and performance of the product.

[0007] 4) Limitations of microencapsulation technology used to achieve durability: Existing technologies often employ microencapsulation to address volatilization and durability issues. However, this technology is complex and costly, and the microcapsule wall material may affect the instantaneous release of the cooling agent, leading to uncontrollable capsule wall rupture and uneven cooling release. Typically, encapsulation materials use phospholipids and other similar ingredients, resulting in a greasy feel that is unsuitable for use as cosmetic ingredients.

[0008] In view of the above problems, this invention is proposed. Summary of the Invention

[0009] To address the aforementioned technical problems, one objective of this invention is to provide a cooling agent composition that exhibits significant long-lasting cooling properties and good stability.

[0010] The second objective of this invention is to provide a preparation process for the above-mentioned cooling agent composition, which is simple, cost-controllable, and easy to industrialize.

[0011] A third objective of this invention is to provide the application of the above-mentioned cooling agent composition in products with cooling effects, thereby enriching the application scenarios of the composition.

[0012] To achieve the above objectives, the present invention adopts the following technical solution:

[0013] In a first aspect, the present invention provides a cooling agent composition, prepared from the following raw materials in 100% by mass fraction: 76-95.29% 1,3-propanediol, 2-9% methyl diisopropylpropionamide, 2-8.5% menthol alkylformyl ethylamine, 0.5-3.5% hydroxypropyl cellulose, 0.1-2% hydroxypropyl-β-cyclodextrin, 0.1-2% borneol, and 0.01-1% oil.

[0014] As a preferred embodiment of the present invention, the following raw materials are used to prepare the product, with a total mass fraction of 100%: 77-95% 1,3-propanediol, 3-8% methyl diisopropylpropionamide, 3-8% menthol alkylformyl ethylamine, 0.9-3% hydroxypropyl cellulose, 0.4-1.6% hydroxypropyl-β-cyclodextrin, 0.4-1.6% borneol, and 0.02-0.8% oil.

[0015] As a preferred embodiment of the present invention, the following raw materials are used to prepare the product, with a total mass fraction of 100%: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkylformyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% oil.

[0016] As a preferred embodiment of the present invention, the following raw materials are used to prepare the product, with a total mass fraction of 100%: 79.5% 1,3-propanediol, 8% methyl diisopropylpropionamide, 8% menthol alkylformyl ethylamine, 3% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% oil.

[0017] As a preferred embodiment of the present invention, the following raw materials are used to prepare the product, with a total mass fraction of 100%: 94% 1,3-propanediol, 2% methyl diisopropylpropionamide, 2% menthol alkylformyl ethylamine, 0.5% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% oil.

[0018] The oil is selected from one or more of butylene glycol dioctanoic acid / didecanoate, isononyl isononanoate, and lemon eucalyptus oil.

[0019] As a preferred embodiment of the present invention, the oil is butanediol dioctanoic acid / didecanoic acid ester. Butanediol dioctanoic acid / didecanoic acid ester can not only effectively dissolve components such as borneol in the core, but also is miscible with hydroxypropyl cellulose in the outer core, thereby forming a stable multi-layer encapsulation system.

[0020] As a preferred embodiment of the present invention, the hydroxypropyl cellulose is a highly substituted hydroxypropyl cellulose, and the hydroxypropyl content in the hydroxypropyl cellulose is 60-70%.

[0021] Secondly, the present invention also provides a method for preparing the above-mentioned cooling agent composition, comprising the following steps:

[0022] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (part 1) are mixed in the specified proportions and then homogenized to obtain phase A.

[0023] S2. Dissolve borneol and oil in the second part of 1,3-propanediol, stir and process to obtain phase B;

[0024] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir and then homogenize to obtain phase C.

[0025] S4. Add methyl diisopropyl propionamide to phase C obtained in step S3, stir and then homogenize to obtain phase D;

[0026] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred, and then homogenized. After the homogenization is completed, the mixture is cooled and filtered to obtain the cooling agent composition.

[0027] As a preferred embodiment of the technical solution of the present invention, in step S1, the temperature of the stirring and mixing treatment is 10~35℃, the rotation speed is 50~500rpm, and the treatment time is 60~120min; the rotation speed of the homogenization treatment is 1000~10000rpm, and the treatment time is 5~30min.

[0028] The mass ratio of the sum of the masses of hydroxypropyl cellulose and hydroxypropyl-β-cyclodextrin to the mass of 1,3-propanediol in Part I is 1:(10~20).

[0029] As a preferred embodiment of the technical solution of the present invention, in step S2, the stirring temperature is 40~65℃, the rotation speed is 10~60rpm, and the processing time is 10~60min.

[0030] As a preferred embodiment of the technical solution of the present invention, in step S3, the stirring temperature is 40~60℃ and the processing time is 30~120min; the homogenization speed is 1000~10000rpm and the processing time is 5~30min.

[0031] As a preferred embodiment of the technical solution of the present invention, in step S4, the stirring temperature is 75~90℃, the rotation speed is 50~500rpm, and the processing time is 30~120min; the homogenization speed is 1000~10000rpm, and the processing time is 5~30min.

[0032] In step S5, the heating and stirring temperature is 75~90℃, the rotation speed is 50~500rpm, and the processing time is 30~120min; the homogenization speed is 1000~10000rpm, and the processing time is 5~30min; the temperature is lowered to 20~40℃; and the filtration mesh size is 150~250 mesh.

[0033] Thirdly, the present invention seeks protection for the use of the above-mentioned cooling agent composition in the preparation of products with cooling effects; the product forms include, but are not limited to, skin care products, shampoos, wet wipes, etc.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] (1) The cooling agent composition prepared by this invention has excellent long-lasting cooling effect and significantly prolongs the duration of action. Through unique composition design and innovative preparation process, a stable multi-encapsulation system is formed, thereby enabling the cooling ingredients to have a long-lasting sustained-release effect. This composition can overcome the shortcomings of traditional single cooling agents with short duration of action. Specifically, this invention first encapsulates the cooling ingredients by selecting suitable oil phases to form a stable oil phase core. Then, the particles encapsulating the cooling ingredients are dispersed in a protective system. Through a special process, micelles are formed to encapsulate the protective system and the cooling agent particles, which are then applied to an aqueous formulation. When the product is applied to the skin surface, the water evaporates, and the encapsulated shell forms a barrier to control the release of the cooling agent. After the carrier structure collapses, it disintegrates upon contact with water, and the cooling ingredients dissolved in the core are released a second time, producing a continuous cooling sensation.

[0036] (2) The cooling agent composition prepared by the present invention can provide a gentle and comfortable cooling experience, avoiding strong stimulation. Through scientific compounding, the "explosiveness" and "duration" of the cooling sensation can be adjusted, avoiding the cold and stinging sensation caused by a single high-intensity cooling agent, making the cooling sensation more gentle, comfortable and natural, and easier for consumers to accept.

[0037] (3) The cooling agent composition prepared by the present invention is based on a multi-encapsulation system of hydroxypropyl cellulose and hydroxypropyl cyclodextrin, which can intelligently enhance the cooling sensation when the user sweats, meet dynamic needs, and is especially suitable for sports, outdoor and other scenarios.

[0038] (4) The cooling agent composition prepared by the present invention has a simple preparation process, is environmentally friendly, and is conducive to industrial production. The preparation method of the present invention avoids the complex microcapsule coating process, has mild reaction conditions, simple steps, does not require the use of special or expensive equipment, has low production cost and high yield, and is very suitable for large-scale industrial production and promotion. Attached Figure Description

[0039] Figure 1 This is a schematic diagram of the products obtained in Example 1 and Comparative Example 6.

[0040] Figure 2 This is a comparison chart of the test results of Example 1 and the control group in Test Example 1.

[0041] Figure 3 This is a comparison chart of the test results of the control group and comparative example 1 in test example 1.

[0042] Figure 4 This is a comparison chart of the test results of the control group and comparative example 2 in test example 1.

[0043] Figure 5 This is a comparison chart of the test results of the control group and comparative example 3 in test example 1.

[0044] Figure 6 This is a comparison chart of the test results of the control group and comparative example 4 in test example 1.

[0045] Figure 7 This is a comparison chart of the test results of the control group and comparative example 5 in test example 1.

[0046] Figure 8 This is a comparison chart of the test results of the control group and comparative example 7 in test example 1.

[0047] Figure 9 This is a comparison chart of the test results of Example 1 and the control group in Test Example 2.

[0048] Figure 10 This is a comparison chart of the test results of Comparative Example 1 and the control group in Test Example 2.

[0049] Figure 11 This is a comparison chart of the test results of Comparative Example 2 and the control group in Test Example 2.

[0050] Figure 12 This is a comparison chart of the test results of Comparative Example 7 and the control group in Test Example 2.

[0051] Figure 13 This is a comparison chart of the test results of Comparative Example 8 and the control group in Test Example 2.

[0052] Figure 14 This is the TME diagram for the product test in Example 1.

[0053] Figure 15 The TME diagram is for the product test in Comparative Example 2.

[0054] Figure 16 The TME diagram is for the test of product 8 in Comparative Example 8. Detailed Implementation

[0055] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0056] Unless otherwise specified, all raw and auxiliary materials used in this invention are readily available and their specifications comply with national pharmaceutical standards.

[0057] As partly exemplary, information on some of the substances used in the embodiments of the present invention is as follows:

[0058] 1,3-Propanediol: purchased from DuPont;

[0059] Hydroxypropyl cellulose was purchased from Jinan Beiding New Material Technology Co., Ltd.

[0060] Hydroxypropyl-β-cyclodextrin was purchased from Shandong Jiake Biotechnology Co., Ltd.

[0061] Borneol was purchased from Xi'an Weisbo Biotechnology Co., Ltd.

[0062] Methyl diisopropyl propionamide was purchased from Wuhan Kemike Biomedical Technology Co., Ltd.

[0063] Menthylcarbamate was purchased from Wuhan Kemic Biomedical Technology Co., Ltd.

[0064] Butylene glycol dioctanoate / didecanoate, purchased from Oleochemicals, Germany;

[0065] Lemon eucalyptus oil, purchased from Xi'an Weisbo Biotechnology Co., Ltd.

[0066] Isonononyl isononanoate was purchased from Croda Chemicals (Shanghai) Co., Ltd.

[0067] Example 1

[0068] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0069] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0070] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0071] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0072] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0073] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0074] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0075] Example 2

[0076] A cooling agent composition, prepared from the following raw materials in 100% by weight: 79.5% 1,3-propanediol, 8% methyl diisopropylpropionamide, 8% menthol alkyl ethylamine, 3% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0077] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0078] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0079] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0080] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0081] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0082] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0083] Example 3

[0084] A cooling agent composition, prepared from the following raw materials in 100% by weight: 94% 1,3-propanediol, 2% methyl diisopropylpropionamide, 2% menthol alkyl ethylamine, 0.5% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0085] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0086] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0087] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0088] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0089] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0090] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0091] Example 4

[0092] A cooling agent composition, prepared from the following raw materials in 100% by weight: 85.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 2% borneol, and 1% butylene glycol dioctanoic acid / didecanoate.

[0093] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0094] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0095] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0096] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0097] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0098] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0099] Example 5

[0100] A cooling agent composition, prepared from the following raw materials in 100% by weight: 88.09% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol ethylcarbamate, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.1% borneol, and 0.01% lemon eucalyptus oil.

[0101] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0102] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0103] S2. Dissolve borneol and lemon eucalyptus oil in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0104] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0105] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0106] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0107] Example 6

[0108] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0109] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0110] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:20) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0111] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0112] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0113] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0114] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0115] Example 7

[0116] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0117] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0118] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0119] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (40℃, 100rpm, 60min) to obtain phase B;

[0120] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0121] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0122] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0123] Example 8

[0124] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0125] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0126] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0127] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0128] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (40℃, 120min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0129] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0130] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0131] Example 9

[0132] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0133] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0134] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0135] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0136] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0137] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (90℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0138] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0139] Example 10

[0140] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0141] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0142] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0143] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0144] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0145] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (3000 rpm, 40 min) to obtain the D phase.

[0146] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0147] Example 11

[0148] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0149] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0150] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0151] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0152] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0153] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0154] S5. Menthanecarbamate was added to phase D, heated and stirred (90℃, 50 rpm, 40 min), and then homogenized (8000 rpm, 30 min). After homogenization, the mixture was cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0155] Example 12

[0156] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0157] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0158] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0159] S2. Dissolve borneol and butylene glycol dioctanoic acid / didecanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0160] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0161] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0162] S5. Menthanecarbamate was added to phase D, heated and stirred (85°C, 50 rpm, 30 min), and then homogenized (3000 rpm, 35 min). After homogenization, the mixture was cooled to 40°C and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0163] Example 13

[0164] A cooling agent composition, prepared from the following raw materials in 100% by weight: 94% 1,3-propanediol, 2% methyl diisopropylpropionamide, 2% menthol alkyl ethylamine, 0.5% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% isononyl isononanoate.

[0165] In this embodiment, a method for preparing the above-mentioned cooling agent composition is also provided, comprising the following steps:

[0166] S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (the mass ratio of hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol is 1:11) are stirred and mixed according to the formula (30℃, 100rpm, 90min), and then homogenized (8000rpm, 5min) to obtain phase A.

[0167] S2. Dissolve borneol and isononyl isononanoate in the remaining 1,3-propanediol, and stir (60℃, 100rpm, 30min) to obtain phase B;

[0168] S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir (60℃, 60min), and then homogenize (8000rpm, 5min) to obtain phase C.

[0169] S4. Add methyl diisopropyl propionamide to the C phase obtained in step S3, stir (85℃, 50 rpm, 30 min), and then homogenize (8000 rpm, 30 min) to obtain the D phase.

[0170] S5. Menthaneformyl ethylamine is added to phase D, heated and stirred (85℃, 50 rpm, 30 min), and then homogenized (8000 rpm, 30 min). After the homogenization is completed, the mixture is cooled to 40℃ and filtered through a 200-mesh filter to obtain the cooling agent composition.

[0171] Comparative Example 1

[0172] Compared to Example 1, the use of hydroxypropyl cellulose was omitted, but everything else remained the same, with corresponding adjustments made to the preparation process.

[0173] Comparative Example 2

[0174] Compared with Example 1, the use of hydroxypropyl-β-cyclodextrin was omitted, but everything else was the same, and the preparation process was adjusted accordingly.

[0175] Comparative Example 3

[0176] Compared with Example 1, the use of butanediol dioctanoic acid / didecanoic acid ester was omitted, while the rest remained the same, with corresponding adjustments made to the preparation process.

[0177] Comparative Example 4

[0178] Compared with Example 1, the use of methyl diisopropyl propionamide was omitted, but everything else was the same, and the preparation process was adjusted accordingly.

[0179] Comparative Example 5

[0180] Compared with Example 1, the use of menthol carbamoyl ethylamine was omitted, but everything else was the same, with the preparation process adjusted accordingly.

[0181] Comparative Example 6

[0182] Compared with Example 1, the dissolution temperature for preparing phase A was adjusted to 60°C, and the rest was the same as in Example 1.

[0183] The A phase prepared in Example 1 is as follows Figure 1 The left image shows a uniform pre-dissolved state with no large particles. In Comparative Example 6, high-temperature mixing during the preparation of phase A resulted in ineffective swelling of hydroxypropyl cellulose, leading to the appearance of undissolved white lumps in the material (such as...). Figure 1 (See right figure). This has a significant impact on subsequent processes and the appearance of the final product, and it cannot pass through 200-mesh filter cloth during filtration, which has a significant impact on production yield.

[0184] Comparative Example 7

[0185] Compared with Example 1, the temperature was adjusted to 60°C after adding methyl diisopropyl propionamide and menthol carbamoyl ethylamine, and the rest was the same as in Example 1.

[0186] Comparative Example 8

[0187] A cooling agent composition, prepared from the following raw materials in 100% by weight: 87.2% 1,3-propanediol, 6% methyl diisopropylpropionamide, 3.5% menthol alkyl ethylamine, 1.8% hydroxypropyl cellulose, 0.5% hydroxypropyl-β-cyclodextrin, 0.5% borneol, and 0.5% butylene glycol dioctanoic acid / didecanoic acid ester.

[0188] This comparative example also provides a method for preparing the above-mentioned cooling agent composition, comprising the following steps:

[0189] Methyl diisopropylpropionamide, menthol carbamoyl ethylamine, hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, borneol, and butylene glycol dioctanoic acid / didecanoic acid ester were added to 1,3-propanediol, stirred at 65°C for 60 min, homogenized at 8000 rpm for 10 min, and then cooled to 40°C.

[0190] Test Example 1: Cooling Test Based on Percutaneous Transdermal Current Threshold (PCT)

[0191] Volunteers meeting the eligibility criteria were selected to participate in the test, which was conducted on the inner forearms of both arms. After applying the test sample, stimulation was performed with or without water, and measurements were taken at corresponding time points using a sensory nerve quantitative instrument via electrical stimulation. At 5 Hz, unmyelinated C fibers were primarily excited, mainly targeting pain, slow pain, temperature sensation, and postganglionic sympathetic nerves; at 250 Hz, A fibers were primarily excited, mainly targeting mechanoreceptors such as pressure, temperature, and fast pain; and at 2000 Hz, A fibers were primarily excited, mainly targeting skin touch and pressure sensation. Therefore, this test was designed to measure changes in human temperature sensation after using different amounts of sample at 5 Hz, with a higher signal indicating a lower perceived temperature.

[0192] Test area: the inner side of the forearms of both arms.

[0193] Sample application method: During the testing period, staff will apply the test sample to the corresponding test area according to the random table.

[0194] Test process:

[0195] ① Volunteer screening: Registration of enrollment information and informed consent

[0196] ② Apply the sample.

[0197] ③ Sensory nerve quantitative detection instrument electrical stimulation measurement method: After applying the sample, apply the coupling agent and detect the minimum electrical stimulation intensity change value at the corresponding time point.

[0198] Test period: 1 day.

[0199] Test time points: before applying the sample, 0 min, 5 min, 10 min, 20 min, 30 min, 60 min, 90 min, and 120 min after applying the sample.

[0200] Test samples: Example 1, Comparative Example 1, Comparative Example 2, Comparative Example 3, Comparative Example 4, Comparative Example 5, Comparative Example 7.

[0201] The test sample was prepared as a 0.5% aqueous solution for testing, while the control group was treated with water. The test results are shown in the figure. Figures 2-8 As shown.

[0202] Skin nerve sensitivity can be assessed using a current perception threshold (CPT) device. The CPT value in the sensitive skin group was significantly lower than that in the non-sensitive group, objectively reflecting changes in nerve sensitivity. The increase in CPT value after the application of the cooling substance indicates a reduction in skin nerve sensitivity, confirming its cooling effect. The onset time and duration of action of different cooling substances were studied using CPT. The test results show that the peak and duration of cooling sensation in Example 1 are superior to those in the comparative examples. The cooling sensation duration in Comparative Examples 1, 2, 3, and 7 is poor; the nerve potential sensitivity at 30 minutes is significantly lower than the peak value, indicating poor sustained cooling performance. The peak cooling sensation in Comparative Examples 4 and 5 is lower, and their cooling intensity is not as good as that in Example 1.

[0203] Test Example 2: Secondary Cooling Sensation Assessment Based on Percutaneous Transdermal Threshold (PCT)

[0204] Test area: the inner side of the forearms of both arms.

[0205] Sample application method: During the testing period, staff will apply the test sample to the corresponding test area according to the random table.

[0206] Test process:

[0207] 1) Volunteer screening: Registration of enrollment information and informed consent

[0208] 2) Apply the sample.

[0209] 3) Sensory nerve quantitative detection instrument electrical stimulation measurement method: After applying the sample, apply the coupling agent and detect the minimum electrical stimulation intensity change value at the corresponding time point.

[0210] 4) For the secondary cooling stimulation test upon contact with water, non-woven fabric was applied for 5 seconds at the test time point. After the water evaporated, coupling agent was applied and the change value of minimum electrical stimulation intensity was measured.

[0211] Test period: 1 day.

[0212] Test time points: before applying the sample, 0 min, 15 min, 30 min, 60 min after applying the sample, immediately after contact with water, 15 min after contact with water, 30 min after contact with water, and 60 min after contact with water.

[0213] Test samples: Example 1, Comparative Example 1, Comparative Example 2, Comparative Example 7, Comparative Example 8.

[0214] The test sample was prepared as a 0.5% aqueous solution for testing, while the control group was treated with water. The test results are shown in the figure. Figures 9-13 As shown.

[0215] The test results show that the duration of both the primary and secondary cooling sensations in Example 1 is superior to that in the comparative examples. The duration of the secondary cooling sensation in Comparative Examples 1, 2, 7, and 8 is shorter. Because the preparation process in the comparative examples cannot form a good multiple encapsulation system, their encapsulation of cooling ingredients and long-lasting sustained-release performance are poor. Furthermore, due to the poor ability to encapsulate the cooling agent, the comparative examples exhibit a high peak instantaneous cooling intensity upon first skin contact, which can irritate the skin.

[0216] Test Example 3: Transmission Electron Microscopy (TEM) Observation of Cooling Agent Composition

[0217] The samples prepared in Example 1, Comparative Example 2, and Comparative Example 8 were subjected to TEM detection.

[0218] Weigh out the test sample and drop it onto a copper mesh. After a few seconds, gently remove the copper mesh sample with tweezers. Use filter paper to absorb excess liquid along one side, place the membrane side up on the filter paper to dry, and observe and photograph it using a transmission electron microscope. The results are as follows: Figures 14-16 As shown.

[0219] As shown in the figure, the product prepared in Example 1 can uniformly disperse the particles encapsulating the cooling agent components in the system, forming a stable multi-encapsulation system, while the products prepared in Comparative Examples 2 and 8 have poor ability to encapsulate the cooling agent.

[0220] The applicant declares that the present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of individual raw materials in the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A cooling agent composition, characterized in that, Based on a total mass fraction of 100%, it is prepared from the following raw materials: 76-95.29% 1,3-propanediol, 2-9% methyl diisopropyl propionamide, 2-8.5% menthol alkylformyl ethylamine, 0.5-3.5% hydroxypropyl cellulose, 0.1-2% hydroxypropyl-β-cyclodextrin, 0.1-2% borneol, and 0.01-1% oil; The preparation method of the cooling agent composition includes the following steps: S1. Hydroxypropyl cellulose, hydroxypropyl-β-cyclodextrin, and 1,3-propanediol (part 1) are mixed in the specified proportions and then homogenized to obtain phase A. S2. Dissolve borneol and oil in the second part of 1,3-propanediol, stir and process to obtain phase B; S3. Add phase A obtained in step S1 to phase B obtained in step S2, stir and then homogenize to obtain phase C. S4. Add methyl diisopropyl propionamide to phase C obtained in step S3, stir and then homogenize to obtain phase D; S5. Menthaneformyl ethylamine is added to phase D, heated and stirred, and then homogenized. After the homogenization is completed, the mixture is cooled and filtered to obtain the cooling agent composition. In step S1, the stirring and mixing temperature is 30℃, the rotation speed is 50~500rpm, and the processing time is 60~120min; the homogenization speed is 1000~10000rpm, and the processing time is 5~30min. The mass ratio of the sum of the masses of hydroxypropyl cellulose and hydroxypropyl-β-cyclodextrin to the mass of 1,3-propanediol in the first part is 1:(10~20). In step S2, the stirring temperature is 40~65℃, the stirring speed is 10~60rpm, and the processing time is 10~60min. In step S3, the stirring temperature is 40~60℃ and the processing time is 30~120min; the homogenization speed is 1000~10000rpm and the processing time is 5~30min. In step S4, the stirring temperature is 85℃, the speed is 50~500rpm, and the processing time is 30~120min; the homogenization speed is 1000~10000rpm, and the processing time is 5~30min. In step S5, the heating and stirring temperature is 85℃, the rotation speed is 50~500rpm, and the processing time is 30~120min; the homogenization speed is 1000~10000rpm, and the processing time is 5~30min; the temperature is lowered to 20~40℃; and the filtration mesh size is 150~250 mesh.

2. The cooling agent composition according to claim 1, characterized in that, It is prepared from the following raw materials in a total mass fraction of 100%: 77-95% 1,3-propanediol, 3-8% methyl diisopropyl propionamide, 3-8% menthol alkylformyl ethylamine, 0.9-3% hydroxypropyl cellulose, 0.4-1.6% hydroxypropyl-β-cyclodextrin, 0.4-1.6% borneol, and 0.02-0.8% oil.

3. The cooling agent composition according to claim 1, characterized in that, The oil is selected from one or more of butylene glycol dioctanoic acid / didecanoate, isononyl isononanoate, and lemon eucalyptus oil.

4. The use of the cooling agent composition according to any one of claims 1 to 3 in the preparation of a product having a cooling effect.

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