Cooling agent and preparation method thereof

By using long-chain alkyl modified starch and sulfonated chitosan as wall materials, combined with crosslinking agents, antioxidants and anti-light agents, a microcapsule with good stability is formed, which solves the shortcomings of existing cooling agents in terms of stability and cooling effects, and achieves long-term cooling effect and good stability of the cooling agent.

CN119523069APending Publication Date: 2025-02-28KUNSHAN YAXIANG SPICEL CO LTD
View PDF 0 Cites 0 Cited by

Patent Information

Application Number
CN202411713609.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-27
Publication Date
2025-02-28

AI Technical Summary

Technical Problem

The existing cooling agent formulas have problems in stability, solubility and taste, especially during long-term storage, where the active ingredients are prone to separation or deterioration, resulting in a weakening of the cooling effect.

Method used

Long-chain alkyl modified starch and sulfonated chitosan are used as wall materials, combined with crosslinking agents, antioxidants and anti-light agents, and through specific formula ratios and preparation methods, a good stability microcapsule is formed to control the release rate of the cooling agent.

Benefits of technology

It achieves the long-term cooling effect and good stability of the coolant, can quickly release the cool smell in the initial stage, and continuously and slowly release it for a long time, maintaining a cool feeling, while improving the quality of the product and user experience.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure BDA0005156366860000081
    Figure BDA0005156366860000081
  • Figure BDA0005156366860000091
    Figure BDA0005156366860000091
Patent Text Reader

Abstract

The invention relates to a cooling agent and a preparation method thereof, and relates to the field of food additives, and the cooling agent comprises the following components in parts by mass: 40-60 parts of a freshener, 1-3 parts of an emulsifier, 30-40 parts of long-chain alkyl modified starch, 20-30 parts of sulfonated chitosan, 0.4-0.8 part of a cross-linking agent, 5-10 parts of a compound cooling improver, 1-3 parts of an antioxidant and 0.5-1 part of an anti-light agent. The preparation method comprises the following steps: preparing a core material emulsion from a freshener, an emulsifier and a compound cool taste improver, preparing a long-chain alkyl modified starch solution, and preparing a mixed solution from sulfonated chitosan, an antioxidant and an anti-light agent; preparing a cross-linking agent solution; adding the core material emulsion into the long-chain alkyl modified starch solution while stirring to obtain an emulsion; adding the mixed solution into the emulsion while stirring, adding a cross-linking agent solution, and stirring for reaction after adding to obtain a suspension; and centrifuging, washing and drying the suspension to obtain the cooling agent. The cooling effect and stability of the cooling agent can be improved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present application relates to the field of food additives, and in particular to a cooling agent and a preparation method thereof. Background Art

[0002] As a common food additive, cooling agents are widely used in the food industry. They not only provide a cooling sensation, but also enhance the taste and flavor of the product, meeting consumers' demand for product diversity. As consumers pay more and more attention to health and natural ingredients, the development of new cooling agents has become a key research direction for major food companies and research institutions. In recent years, a variety of cooling agents have appeared on the market, such as natural extracts and synthetic compounds. These cooling agents show different performance characteristics in different application scenarios, which has promoted the technological innovation and development of the entire industry.

[0003] However, existing cooling agent formulations have some shortcomings. Single-ingredient cooling agents often fail to achieve the desired cooling effect, and although multi-ingredient compound cooling agents can improve the cooling sensation, they still have problems with stability, solubility, and taste. Especially during long-term storage, the active ingredients of cooling agents are prone to separation or deterioration, resulting in a weakened cooling effect, affecting product quality and user experience. Therefore, it is necessary to provide a cooling agent with excellent cooling effect and good stability. Summary of the invention

[0004] In order to improve the cooling effect and stability of a cooling agent, the present application provides a cooling agent and a preparation method thereof.

[0005] The present application provides a cooling agent and a preparation method thereof using the following technical solutions: In the first aspect, the present application provides a cooling agent, which adopts the following technical solution: A cooling agent, the raw materials for preparing the cooling agent include the following components in parts by weight: 40-60 servings of cooling agent Emulsifier 1-3 parts 30-40 parts of long-chain alkyl modified starch Sulfonated chitosan 20-30 parts Crosslinking agent 0.4-0.8 parts 5-10 parts of compound cool taste enhancer 1-3 servings of antioxidants Light stabilizer 0.5-1 part.

[0006] Long-chain alkyl modified starch and sulfonated chitosan are used as wall materials, which can effectively wrap the cooling agent and the compound cooling enhancer, control their release rate, and enable the cooling agent to be continuously released for a long time, thereby enhancing the durability of the cooling effect; the cross-linking agent promotes further cross-linking of the wall material, enhances the structural strength and stability of the wall material, regulates the pore structure of the wall material, controls the release rate of the cooling agent, and reduces the influence of external environmental factors, thereby improving the stability of the cooling agent; the antioxidant and light stabilizer are dispersed in the wall material, which can protect the cooling agent from oxidation and photodegradation, and enhance the stability of the cooling agent; the cooling agent prepared by the above components can quickly release the coolness in the initial stage, bringing an immediate cooling shock, and then continue to release slowly over a long period of time to maintain the cooling feeling, and the cooling agent has good cooling effect and stability.

[0007] Preferably, the raw materials for preparing the long-chain alkyl modified starch include starch, long-chain alkyl acid and p-toluenesulfonic acid.

[0008] p-Toluenesulfonic acid acts as a catalyst to promote the reaction between long-chain alkyl acids and starch, allowing long-chain alkyl groups to be successfully grafted onto starch molecules; long-chain alkyl groups can enhance the hydrophobicity and stability of starch, change the spatial structure of starch, and enable starch to better interact with sulfonated chitosan, more effectively encapsulate and slowly release the cooling agent, further optimize the release performance of the cooling agent, and provide a long-lasting and uniform cooling effect; long-chain alkyl acids can also improve the compatibility of the cooling agent with other ingredients, contributing to the overall stability and uniformity of the cooling agent.

[0009] Preferably, the long chain alkyl acid includes palmitic acid and stearic acid.

[0010] Palmitic acid and fatty acids have hydrophobic long-chain alkyl structures. Long-chain alkyl groups grafted onto starch molecules can enhance the hydrophobicity of starch, better resist the invasion of external moisture, improve the stability of cooling agent microcapsules in humid environments, and prevent problems such as deterioration of cooling agents or premature release due to moisture; the introduction of long-chain alkyl groups will change the spatial structure and intermolecular forces of starch, so that the modified starch can more effectively wrap the cooling agent, and can adjust the release rate of the cooling agent so that it can be released slowly and continuously, prolong the duration of the cooling effect, and provide a more lasting cooling feeling; long-chain alkyl acids can also help improve the compatibility and synergy between starch and sulfonated chitosan, enhance the stability of the wall material, and thus improve the quality and cooling effect of cooling agent products.

[0011] Preferably, the mass ratio of the starch, the long-chain alkyl acid and p-toluenesulfonic acid is 1:(0.5-0.7):0.02.

[0012] The long-chain alkyl modified starch prepared according to the above mass ratio has good hydrophobic properties and spatial structure, can effectively wrap and protect the cooling agent, and enhance the cooling effect and stability of the cooling agent.

[0013] Preferably, the raw materials for preparing the sulfonated chitosan include carboxymethyl chitosan and aminosulfonic acid.

[0014] Aminosulfonic acid introduces sulfonic acid groups into chitosan molecules, and sulfonated chitosan has good water solubility and ion exchange properties, which can enhance the stability of the wall material; good water solubility helps sulfonated chitosan and long-chain alkyl modified starch to better blend and cross-link, forming microcapsules with good stability to encapsulate the cooling agent molecules; the introduction of sulfonic acid groups increases the negative charge density of chitosan molecules, which can prevent cationic substances from invading the cooling agent molecules, thereby improving the stability of the cooling agent and reducing the influence of external ions on the performance of the cooling agent; sulfonated chitosan can also further optimize the structure and performance of the wall material by interacting with long-chain alkyl modified starch, forming a tighter network structure through electrostatic attraction or hydrogen bonding, controlling the release rate of the cooling agent, and providing a lasting and stable cooling sensation.

[0015] Preferably, the mass ratio of the carboxymethyl chitosan to aminosulfonic acid is 1:(0.3-0.6).

[0016] The sulfonated chitosan prepared according to the above mass ratio has good compatibility, can effectively improve the stability of the wall material, and regulate the pore structure of the wall material, thereby improving the cooling effect and stability of the cooling agent.

[0017] Preferably, the compound cool taste enhancing agent includes menthol, menthone and spearmint extract.

[0018] Menthol has a strong cooling sensation and can activate cold receptors to produce a cooling sensation; menthone has a mild cooling effect and provides a relatively soft cooling initial sensation at the beginning. With the slow release and action, the cooling effect gradually increases and lasts longer, making the cooling effect more three-dimensional and lasting; spearmint extract has a cooling aroma and taste, which can blend with the taste of the cooling agent to enrich the cooling layer of the cooling agent. The synergistic effect of menthol, menthone and spearmint extract can enhance the cooling layer and persistence of the cooling agent, thereby enhancing the cooling effect of the cooling agent.

[0019] Preferably, the antioxidant comprises tea polyphenols.

[0020] Tea polyphenols have good antioxidant properties, can capture free radicals, interrupt the chain process of oxidation reactions, improve the stability and durability of cooling agents, and enable them to exert a cooling effect for a long time; tea polyphenols can work synergistically with cooling agents to enhance the body's perception of cooling, thereby enhancing the cooling effect; tea polyphenols can also react with long-chain alkyl modified starch and sulfonated chitosan such as hydrogen bonding to enhance the mechanical strength and stability of the wall material, thereby regulating the pore structure and permeability of the wall material, and improving the stability of the cooling agent and the durability of the cooling effect.

[0021] Preferably, the light stabilizer comprises benzophenone.

[0022] Benzophenone has good anti-ultraviolet properties. Under the action of ultraviolet rays, electrons will jump from the ground state to the excited state, absorbing the energy of ultraviolet photons, thereby preventing ultraviolet rays from destroying the coolant molecules, thereby improving the cooling effect and stability of the coolant; benzophenone molecules have both polar and non-polar parts, which can promote the uniform dispersion of the coolant and improve the uniformity and stability of the coolant product; benzophenone has a rose scent, which can enhance the freshness and experience of the coolant; the benzene ring structure in benzophenone has the characteristics of electron delocalization, which can capture free radicals, interrupt the chain reaction process of the oxidation reaction, and synergize with antioxidants to improve the stability of the coolant.

[0023] In a second aspect, the present application provides a method for preparing a cooling agent, using the following technical solution: A method for preparing a cooling agent comprises the following steps: Dispersing a cooling agent, an emulsifier and a compound cool taste enhancer in water, stirring to obtain a core material emulsion; dispersing a long-chain alkyl modified starch in water, heating and stirring to obtain a long-chain alkyl modified starch solution; dispersing sulfonated chitosan, an antioxidant and a light stabilizer in an acetic acid aqueous solution, stirring to obtain a mixed solution; dispersing a crosslinking agent in water to obtain a crosslinking agent solution; The core material emulsion is added to the long-chain alkyl modified starch solution, and stirred while adding to obtain an emulsion; while stirring, the mixed liquid is added to the emulsion, and after the addition is completed, a cross-linking agent solution is added, and after the addition is completed, stirring and reacting are continued to obtain a suspension; the suspension is centrifuged, washed with water, and then heated and vacuum dried to obtain a cooling agent.

[0024] The cooling agent prepared according to the above steps has good cooling effect and stability. The cooling agent can quickly release a shocking cooling taste in the initial stage and continue to release slowly over a long period of time, thus having a long-lasting cooling effect.

[0025] In summary, the present application includes at least one of the following beneficial technical effects: 1. Long-chain alkyl modified starch and sulfonated chitosan are used as wall materials, which can effectively wrap the cooling agent and the compound cooling enhancer, control their release rate, and enable the cooling agent to be continuously released for a long time, thereby enhancing the durability of the cooling effect; the cross-linking agent promotes further cross-linking of the wall material, enhances the structural strength and stability of the wall material, regulates the pore structure of the wall material, controls the release rate of the cooling agent, and reduces the influence of external environmental factors, thereby improving the stability of the cooling agent; the antioxidant and light stabilizer are dispersed in the wall material, which can protect the cooling agent from oxidation and photodegradation, and enhance the stability of the cooling agent; the cooling agent prepared by the above components can quickly release the coolness in the initial stage, bringing an immediate cooling impact, and then continue to release slowly for a long time to maintain the cooling feeling, so that the cooling agent has a good cooling effect and stability.

[0026] 2. p-Toluenesulfonic acid acts as a catalyst to promote the reaction between long-chain alkyl acids and starch, allowing long-chain alkyl groups to be successfully grafted onto starch molecules; long-chain alkyl groups can enhance the hydrophobicity and stability of starch, change the spatial structure of starch, and enable starch to better interact with sulfonated chitosan, more effectively encapsulate and slowly release the cooling agent, further optimize the release performance of the cooling agent, and provide a long-lasting and uniform cooling effect; long-chain alkyl acids can also improve the compatibility of the cooling agent with other ingredients, which contributes to the overall stability and uniformity of the cooling agent.

[0027] 3. Aminosulfonic acid introduces sulfonic acid groups into chitosan molecules. Sulfonated chitosan has good water solubility and ion exchange properties, which can enhance the stability of the wall material. Good water solubility helps sulfonated chitosan and long-chain alkyl modified starch to better blend and cross-link, forming stable microcapsules to encapsulate the cooling agent molecules. The introduction of sulfonic acid groups increases the negative charge density of chitosan molecules, which can prevent cationic substances from invading the cooling agent molecules, thereby improving the stability of the cooling agent and reducing the impact of external ions on the performance of the cooling agent. Sulfonated chitosan may also further optimize the structure and performance of the wall material by interacting with long-chain alkyl modified starch, forming a tighter network structure through electrostatic attraction or hydrogen bonding, controlling the release rate of the cooling agent, and providing a lasting and stable cooling sensation. DETAILED DESCRIPTION

[0028] The present application discloses a cooling agent and a preparation method thereof. The raw materials used in the present application can be obtained from commercially available raw materials unless otherwise specified. The present application is further described in detail below in conjunction with the examples: Raw materials: Starch is corn starch, palmitic acid (CAS No.: 57-10-3), stearic acid (CAS No.: 57-11-4), p-toluenesulfonic acid (CAS No.: 104-15-4), carboxymethyl chitosan (CAS No.: 83512-85-0), aminosulfonic acid (CAS No.: 5329-14-6), the model of the cooling agent is WS-30, and the emulsifier is Tween-80 (CAS No.: 9 005-65-6), menthol (CAS No. 89-78-1), menthone (CAS No. 10458-14-7), spearmint extract (CAS No. 84696-51-5), antioxidant is tea polyphenols (CAS No. 84650-60-2), light stabilizer is benzophenone (CAS No. 119-61-9), crosslinker is citric acid (CAS No. 77-92-9).

[0029] Example 1 Preparation of long-chain alkyl-modified starch 32.89 g of starch was dispersed in 300 mL of cyclohexane, and the mixture was stirred at 300 rpm for 20 min to obtain a starch suspension; 16.45 g of palmitic acid and 0.66 g of p-toluenesulfonic acid were added to the starch suspension, the temperature was raised to 90° C., and the mixture was stirred at 500 rpm for reaction for 5 h. After the mixture was cooled to 30° C., a 10% by weight sodium carbonate aqueous solution was added until the pH value was 7 to obtain a reacted mixed solution, the reacted mixed solution was allowed to stand for stratification, and a lower precipitate was obtained by separation. The lower precipitate was washed with deionized water for 5 times, and dried in an oven at 60° C. to obtain a long-chain alkyl modified starch.

[0030] Preparation of sulfonated chitosan 38.46 g of carboxymethyl chitosan was dispersed into 500 mL of 3% acetic acid aqueous solution, and the mixture was stirred at 300 rpm for 30 min to obtain a carboxymethyl chitosan solution; 11.54 g of aminosulfonic acid was added to the carboxymethyl chitosan solution, and the mixture was stirred at 300 rpm. The mixture was heated to 60° C. and reacted for 8 h to obtain a modified solution. Ethanol was added to the modified solution for precipitation, and a precipitate was obtained by filtering. The precipitate was washed with deionized water for 5 times, and the washed precipitate was dried in a vacuum drying oven at 50° C. to obtain a sulfonated chitosan.

[0031] Preparation of cooling agent 40g of cooling agent, 1g of emulsifier and 5g of compound cool taste enhancer are dispersed in 200mL of deionized water, wherein the mass ratio of menthol, menthone and spearmint extract in the compound cool taste enhancer is 0.5:1:1, and stirred at 300rpm for 15min to obtain a core material emulsion; 30g of long-chain alkyl modified starch is dispersed in 300mL of deionized water, and stirred at 300rpm for 30min at 70°C to obtain a long-chain alkyl modified starch solution; 20g of sulfonated chitosan, 1g of antioxidant and 0.5g of light stabilizer are dispersed in 300mL of 3% acetic acid aqueous solution by mass, and stirred at 300rpm for 30min to obtain a mixed solution; 0.4g of cross-linking agent is dispersed in 20mL of deionized water to obtain a cross-linking agent solution.

[0032] The core material emulsion is added to the long-chain alkyl modified starch solution, and stirred at a speed of 500 rpm for 30 minutes to obtain an emulsion; while stirring at a speed of 500 rpm, the mixed solution is added to the emulsion at a speed of 10 mL / min. After the addition is completed, the cross-linking agent solution is added at a speed of 2 mL / min. After the addition is completed, the stirring is continued at a speed of 500 rpm for 1 hour to obtain a suspension; the suspension is centrifuged, washed with deionized water, and then vacuum dried at 60°C to obtain a cooling agent.

[0033] Example 2 Preparation of long-chain alkyl-modified starch 29.07 g of starch was dispersed in 300 mL of cyclohexane, and stirred at a speed of 300 rpm for 20 min to obtain a starch suspension; 20.35 g of palmitic acid and 0.58 g of p-toluenesulfonic acid were added to the starch suspension, the temperature was raised to 90° C., and the mixture was stirred at a speed of 500 rpm for reaction for 5 h. After cooling to 30° C., a sodium carbonate aqueous solution with a mass percentage of 10% was added until the pH value was 7 to obtain a reacted mixed solution, the reacted mixed solution was allowed to stand for stratification, and a lower precipitate was separated to obtain a lower precipitate, the lower precipitate was washed with deionized water for 5 times, and dried in an oven at 60° C. to obtain a long-chain alkyl modified starch.

[0034] Preparation of sulfonated chitosan 31.25 g of carboxymethyl chitosan was dispersed into 500 mL of 3% acetic acid aqueous solution, and the mixture was stirred at 300 rpm for 30 min to obtain a carboxymethyl chitosan solution; 18.75 g of aminosulfonic acid was added to the carboxymethyl chitosan solution, and the mixture was stirred at 300 rpm. The mixture was heated to 60° C. and reacted for 8 h to obtain a modified solution. Ethanol was added to the modified solution for precipitation, and a precipitate was obtained by filtering. The precipitate was washed with deionized water for 5 times, and the washed precipitate was dried in a vacuum drying oven at 50° C. to obtain a sulfonated chitosan.

[0035] Preparation of cooling agent 60g of cooling agent, 3g of emulsifier and 10g of compound cool taste enhancer are dispersed in 200mL of deionized water, wherein the mass ratio of menthol, menthone and spearmint extract in the compound cool taste enhancer is 0.5:1:1, and stirred at 300rpm for 15min to obtain a core material emulsion; 40g of long-chain alkyl modified starch is dispersed in 300mL of deionized water, and stirred at 300rpm for 30min at 70°C to obtain a long-chain alkyl modified starch solution; 30g of sulfonated chitosan, 3g of antioxidant and 1g of light stabilizer are dispersed in 300mL of 3% acetic acid aqueous solution by mass, and stirred at 300rpm for 30min to obtain a mixed solution; 0.8g of cross-linking agent is dispersed in 20mL of deionized water to obtain a cross-linking agent solution.

[0036] The core material emulsion is added to the long-chain alkyl modified starch solution, and stirred at a speed of 500 rpm for 30 minutes to obtain an emulsion; while stirring at a speed of 500 rpm, the mixed solution is added to the emulsion at a speed of 10 mL / min. After the addition is completed, the cross-linking agent solution is added at a speed of 2 mL / min. After the addition is completed, the stirring is continued at a speed of 500 rpm for 1 hour to obtain a suspension; the suspension is centrifuged, washed with deionized water, and then vacuum dried at 60°C to obtain a cooling agent.

[0037] Example 3 Preparation of long-chain alkyl-modified starch 30.86 g of starch was dispersed in 300 mL of cyclohexane, and the mixture was stirred at 300 rpm for 20 min to obtain a starch suspension; 18.52 g of stearic acid and 0.62 g of p-toluenesulfonic acid were added to the starch suspension, the temperature was raised to 90° C., and the mixture was stirred at 500 rpm for reaction for 5 h. After the mixture was cooled to 30° C., a 10% by weight sodium carbonate aqueous solution was added to a pH value of 7 to obtain a reacted mixed solution, the reacted mixed solution was allowed to stand for stratification, and a lower precipitate was separated to obtain the lower precipitate, the lower precipitate was washed with deionized water for 5 times, and dried in an oven at 60° C. to obtain a long-chain alkyl modified starch.

[0038] Preparation of sulfonated chitosan 34.48 g of carboxymethyl chitosan was dispersed into 500 mL of 3% acetic acid aqueous solution, and the mixture was stirred at 300 rpm for 30 min to obtain a carboxymethyl chitosan solution; 15.52 g of aminosulfonic acid was added to the carboxymethyl chitosan solution, and the mixture was stirred at 300 rpm. The mixture was heated to 60° C. and reacted for 8 h to obtain a modified solution. Ethanol was added to the modified solution for precipitation, and a precipitate was obtained by filtering. The precipitate was washed with deionized water for 5 times, and the washed precipitate was dried in a vacuum drying oven at 50° C. to obtain a sulfonated chitosan.

[0039] Preparation of cooling agent 50g of cooling agent, 2g of emulsifier and 7.5g of compound cool taste enhancer are dispersed in 200mL of deionized water, wherein the mass ratio of menthol, menthone and spearmint extract in the compound cool taste enhancer is 0.5:1:1, and stirred at 300rpm for 15min to obtain a core material emulsion; 35g of long-chain alkyl modified starch is dispersed in 300mL of deionized water, and stirred at 300rpm for 30min at 70°C to obtain a long-chain alkyl modified starch solution; 25g of sulfonated chitosan, 2g of antioxidant and 0.75g of light stabilizer are dispersed in 300mL of 3% acetic acid aqueous solution by mass, and stirred at 300rpm for 30min to obtain a mixed solution; 0.6g of cross-linking agent is dispersed in 20mL of deionized water to obtain a cross-linking agent solution.

[0040] The core material emulsion is added to the long-chain alkyl modified starch solution, and stirred at a speed of 500 rpm for 30 minutes to obtain an emulsion; while stirring at a speed of 500 rpm, the mixed solution is added to the emulsion at a speed of 10 mL / min. After the addition is completed, the cross-linking agent solution is added at a speed of 2 mL / min. After the addition is completed, the stirring is continued at a speed of 500 rpm for 1 hour to obtain a suspension; the suspension is centrifuged, washed with deionized water, and then vacuum dried at 60°C to obtain a cooling agent.

[0041] Example 4 Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in Example 4, the amount of starch used is 35.21 g, the amount of long-chain alkyl acid used is 14.08 g, and the amount of p-toluenesulfonic acid used is 0.71 g.

[0042] Example 5 Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, the amount of starch used is 27.47 g, the amount of long-chain alkyl acid used is 21.98 g, and the amount of p-toluenesulfonic acid used is 0.55 g.

[0043] Example 6 Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that in Example 6, the amount of carboxymethyl chitosan used is 43.48 g, and the amount of aminosulfonic acid used is 6.52 g.

[0044] Example 7 Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that in Example 7, the amount of carboxymethyl chitosan used is 28.57 g, and the amount of aminosulfonic acid used is 21.43 g.

[0045] Example 8 Example 8 is based on Example 3. The only difference between Example 8 and Example 3 is that spearmint extract is not added to the compound cool taste enhancing agent in Example 8.

[0046] Example 9 Example 9 is based on Example 3. The only difference between Example 9 and Example 3 is that spearmint extract and menthol are not added to the compound cool taste enhancing agent in Example 9.

[0047] Comparative Example 1 Comparative Example 1 is based on Example 3, and the only difference between Comparative Example 1 and Example 3 is that in Comparative Example 1, the long-chain alkyl modified starch is replaced by starch.

[0048] Comparative Example 2 Comparative Example 2 is based on Example 3, and the only difference between Comparative Example 2 and Example 3 is that in Comparative Example 2, sulfonated chitosan is replaced by hydroxymethyl chitosan.

[0049] Comparative Example 3 Comparative Example 3 is based on Example 3, and the only difference between Comparative Example 3 and Example 3 is that the compound cool taste enhancing agent is not added in Comparative Example 3.

[0050] Comparative Example 4 Comparative Example 4 is based on Example 3, and the only difference between Comparative Example 4 and Example 3 is that no antioxidant is added in Comparative Example 4.

[0051] Comparative Example 5 Comparative Example 5 is based on Example 3, and the only difference between Comparative Example 5 and Example 3 is that no light stabilizer is added in Comparative Example 5.

[0052] Performance testing (1) Cooling agent duration test: 10 healthy people with normal sense of smell and taste and who have not suffered from cold, rhinitis or other diseases recently were selected as test subjects. 5 g of the sample was dispersed in 100 mL of deionized water to obtain a sample dispersion. A blank control solution without adding the sample was set up. The filter paper disc was soaked in the sample dispersion for 5 min and then taken out. The test subjects put the soaked filter paper disc into their mouths and recorded the time when the cooling intensity of the sample was close to that of the blank control. After measurement, the highest and lowest values ​​were removed and the remaining values ​​were averaged. The results are recorded in Table 1.

[0053] (2) Cooling agent stability test: The samples were placed in an ozone atmosphere with a flow rate of 200 mL / min and under ultraviolet light with a light intensity of 3000 lux for 24 h. The initial concentration and post-treatment concentration of the ingredients in the cooling agent were tested, and the concentration change rate was calculated. Each sample was tested three times, and the average value was taken after measurement. The results are recorded in Table 1.

[0054] Table 1 Test results of the cooling effect and stability of the cooling agent It can be seen from Table 1 that the cooling effect of Examples 1-3 lasts for more than 46 minutes, the concentration change rate after oxidation treatment is less than 6.6%, and the concentration change rate under ultraviolet light is less than 4.4%, which shows that the cooling agent prepared in the present application has good cooling effect and stability.

[0055] As can be seen from Table 1, the only difference between Examples 4 and 5 and Example 3 is that the mass ratio of starch, long-chain alkyl acid and p-toluenesulfonic acid in Example 4 is 1:0.4:0.02, and the mass ratio of starch, long-chain alkyl acid and p-toluenesulfonic acid in Example 5 is 1:0.8:0.02. Compared with Example 3, the cooling effect and stability of Examples 4 and 5 are reduced; this is because the ratio of the synthetic components of the long-chain alkyl modified starch is not within the specified range, which affects the spatial structure and intermolecular forces of the long-chain alkyl modified starch, and further affects its synergistic effect with sulfonated chitosan, and the stability and pore structure of the wall material are affected, thereby reducing the cooling effect and stability of the cooling agent.

[0056] As can be seen from Table 1, the only difference between Examples 6 and 7 and Example 3 is that the mass ratio of carboxymethyl chitosan to aminosulfonic acid in Example 6 is 1:0.15, and the mass ratio of carboxymethyl chitosan to aminosulfonic acid in Example 7 is 1:0.75. Compared with Example 3, Examples 6 and 7 have reduced cooling effects and stability. This is because the ratio of the synthetic components of sulfonated chitosan is not within the specified range, which will affect the interaction between sulfonated chitosan and long-chain alkyl modified starch, and the stability and pore structure of the wall material are affected, thereby reducing the cooling effect and stability.

[0057] As can be seen from Table 1, the only difference between Examples 8 and 9 and Example 3 is that: in Example 8, no spearmint extract is added to the compound cool taste enhancing agent, and in Example 9, no spearmint extract and menthol are added to the compound cool taste enhancing agent. Compared with Example 3, Examples 8 and 9 have a reduced cooling effect; this is because after reducing the components in the compound cool taste enhancing agent, the synergistic effect decreases, the cooling feeling of the cooling agent lacks layers, and the duration of the cooling feeling is also reduced.

[0058] As can be seen from Table 1, the only difference between Comparative Examples 1 and 2 and Example 3 is that: Comparative Example 1 replaces the long-chain alkyl modified starch with starch, and Comparative Example 2 replaces the sulfonated chitosan with hydroxymethyl chitosan. Compared with Example 3, Comparative Examples 1 and 2 have significantly reduced cooling effects and stability; this is because if starch or hydroxymethyl chitosan lacks modification treatment, the interaction between the two is weakened, the stability of the wall material is reduced, and the pore structure becomes worse, thereby significantly reducing the cooling effect and stability.

[0059] As can be seen from Table 1, the only difference between Comparative Example 3 and Example 3 is that Comparative Example 3 does not add the compound cool taste enhancing agent, and the cooling effect of Comparative Example 3 is significantly reduced compared with Example 3; this is because there is a lack of synergistic effect of the compound cool taste enhancing agent, and the layering and intensity of the cooling effect are reduced.

[0060] As can be seen from Table 1, the only difference between Comparative Examples 4 and 5 and Example 3 is that Comparative Example 4 does not add an antioxidant, and Comparative Example 5 does not add a light stabilizer. Compared with Example 3, the stability of Comparative Examples 4 and 5 is significantly reduced; this is because without adding a light stabilizer or an antioxidant, the active components in the cooling agent are more susceptible to external environmental factors, thereby significantly reducing the stability.

[0061] This specific embodiment is only an explanation of the present application, and it is not a limitation of the present application. Through the above description, relevant staff can make various changes and modifications without deviating from the technical idea of ​​the present application. The technical scope of the present application is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A cooling agent, characterized in that: The raw materials for preparation include the following components in parts by weight: 40-60 servings of cooling agent Emulsifier 1-3 parts 30-40 parts of long-chain alkyl modified starch Sulfonated chitosan 20-30 parts Crosslinking agent 0.4-0.8 parts 5-10 parts of compound cool taste enhancer 1-3 servings of antioxidants Light stabilizer 0.5-1 part.

2. A cooling agent according to claim 1, characterized in that: The raw materials for preparing the long-chain alkyl modified starch include starch, long-chain alkyl acid and p-toluenesulfonic acid.

3. A cooling agent according to claim 2, characterized in that: The long chain alkyl acids include palmitic acid and stearic acid.

4. A cooling agent according to claim 3, characterized in that: The mass ratio of the starch, the long-chain alkyl acid and the p-toluenesulfonic acid is 1:(0.5-0.7):0.

02.

5. The cooling agent according to claim 1, characterized in that: The raw materials for preparing the sulfonated chitosan include carboxymethyl chitosan and aminosulfonic acid.

6. A cooling agent according to claim 5, characterized in that: The mass ratio of the carboxymethyl chitosan to aminosulfonic acid is 1:(0.3-0.6).

7. The cooling agent according to claim 1, characterized in that: The compound cool taste enhancing agent comprises menthol, menthone and spearmint extract.

8. The cooling agent according to claim 1, characterized in that: The antioxidant includes tea polyphenols.

9. The cooling agent according to claim 1, characterized in that: The light stabilizer includes benzophenone.

10. A method for preparing the cooling agent as claimed in any one of claims 1 to 9, characterized in that: The steps include: Dispersing a cooling agent, an emulsifier and a compound cool taste enhancer in water, stirring to obtain a core material emulsion; dispersing a long-chain alkyl modified starch in water, heating and stirring to obtain a long-chain alkyl modified starch solution; dispersing sulfonated chitosan, an antioxidant and a light stabilizer in an acetic acid aqueous solution, stirring to obtain a mixed solution; dispersing a crosslinking agent in water to obtain a crosslinking agent solution; The core material emulsion is added to the long-chain alkyl modified starch solution, and stirred while adding to obtain an emulsion; while stirring, the mixed liquid is added to the emulsion, and after the addition is completed, a cross-linking agent solution is added, and after the addition is completed, stirring and reacting are continued to obtain a suspension; the suspension is centrifuged, washed with water, and then heated and vacuum dried to obtain a cooling agent.