Cool feeling agent compound and preparation method thereof
Mint essential oil balls are prepared by combining peppermint essential oil with porous starch, sodium alginate and chitosan, and combining menthol with silica and dopamine hydrochloride, the problem of menthol is easily lost and long-term release during use is solved, and the controllable release of menthol is achieved and the stability and antibacterial properties of cooling agents are improved.
Patent Information
- Application Number
- CN202510102434.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-22
- Publication Date
- 2025-05-06
AI Technical Summary
Menthol is prone to lose its stability and long-term release during use, which affects its application effect in cooling agents.
Mint essential oil balls are prepared by combining menthol essential oil with porous starch, sodium alginate and chitosan, and menthol is bound to silica and dopamine hydrochloride to form a complex to slowly release menthol.
It effectively improves the stability and sustained release effect of peppermint essential oil, extends the stability and release time of cooling agents, and enhances antibacterial properties.
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Figure BDA0005254521480000081
Abstract
Description
Technical Field
[0001] The present application relates to the field of cooling agents, and in particular to a cooling agent composite and a preparation method thereof. Background Art
[0002] Cooling agents are a general term for all chemical substances that can produce a cooling effect and do not have strong medicinal properties.
[0003] Menthol is usually added to cooling agents. Menthol is a terpene organic compound with a chemical formula of C10H20O. Menthol is extracted from the leaves and stems of mint. It is a white crystal and is the main component of mint and peppermint essential oils. Menthol generally has two isomers (D-type and L-type). Natural menthol is mainly the left-handed isomer (L-menthol). The menthol here generally refers to racemic menthol (DL-menthol). Menthol can be used as a flavoring agent for toothpaste, perfume, beverages, and candies. In medicine, it is used as a stimulant, acting on the skin or mucous membranes, and has a cooling and itching effect. It can be taken orally as a wind-repellent for headaches and inflammation of the nose, pharynx, and throat. Its esters can also be used in spices and medicines.
[0004] However, menthol has a strong volatility, which limits its release to a certain extent, affecting its release stability and duration, so it needs to be improved. Summary of the invention
[0005] In order to further enhance the sustained-release effect of the cooling agent, the present application provides a cooling agent composite and a preparation method thereof.
[0006] The present application provides a cooling agent composite and a preparation method thereof using the following technical solutions: In the first aspect, the present application provides a cooling agent composite, which adopts the following technical solution: A cooling agent composite comprises the following components by weight: 40-50 parts of sw-23, 28-32 parts of peppermint essential oil globules, 22-26 parts of menthol complex, 13-15 parts of potassium sorbate, 8-12 parts of sodium bicarbonate; The raw materials of the peppermint essential oil pellets include peppermint essential oil, porous starch, sodium alginate and chitosan.
[0007] By adopting the above technical scheme, peppermint essential oil is a component extracted from peppermint by water distillation or subcritical low-temperature extraction, has a minty flavor, and is refreshing. It can be compounded with SW-23 to further enhance the cooling effect of the cooling agent. However, peppermint essential oil is easily oxidized and loses its activity. Peppermint essential oil is combined with porous starch, sodium alginate and chitosan to prepare peppermint essential oil spheres to form microcapsules, which can effectively encapsulate the peppermint essential oil and reduce the rapid inactivation and volatilization of the peppermint essential oil, thereby achieving the controllable release of the peppermint essential oil and improving the stability of the composite cooling agent.
[0008] Preferably, the porous starch is prepared by the following method: The citric acid-disodium hydrogen phosphate buffer solution is mixed with rice starch to obtain a starch suspension and stirred, alpha-amylase and saccharifying enzyme are added and stirred, and then a sodium hydroxide solution is added to inactivate the mixed enzyme to stop the reaction, centrifugation washing, freeze drying, and grinding to obtain porous starch.
[0009] By adopting the above technical scheme, rice starch is hydrolyzed by combining α-amylase and saccharifying enzyme, the surface of rice starch is corroded, and saccharifying enzyme produces concave internal corrosion and pitting cavity. The porous starch prepared by the composite of the two has the characteristics of large specific surface area and high adsorption performance. At the same time, the starch after enzyme treatment exposes more hydrophilic and lipophilic groups, making the peppermint essential oil loading more stable, further improving the stability of the prepared peppermint essential oil pellets.
[0010] Preferably, the peppermint essential oil globules are prepared by the following method: The porous starch is mixed with peppermint essential oil, and the mixture is centrifuged and washed after magnetic stirring. The precipitate is recovered after centrifugation again, and freeze-dried to obtain starch-composite peppermint essential oil powder. The peppermint starch composite powder, sodium alginate and water are mixed and stirred to obtain a mixed system, chitosan is mixed with a calcium chloride solution to obtain a solidified liquid, the mixed system is added to the solidified liquid for solidification, and the mixture is filtered, washed and dried to obtain peppermint essential oil pellets.
[0011] By adopting the above technical solution, sodium alginate is a high molecular weight polysaccharide with good gelation, stability and safety. The gel prepared by using only sodium alginate and calcium chloride has gaps. After adding porous starch, the gel strength can be improved. Chitosan has good biocompatibility. A large number of primary amino groups on the chitosan molecular chain and the carboxyl groups of sodium alginate are compounded as wall materials through electrostatic interaction. Then, menthol essential oil is adsorbed by porous starch as a profile. Ca in calcium chloride 2+ It can undergo ionic cross-linking with alginate to form a stable three-dimensional network structure, and after compounding, it forms peppermint essential oil spheres, thereby encapsulating the peppermint essential oil and further improving the overall stability and loading rate of the peppermint essential oil.
[0012] Preferably, the mass ratio between the starch composite peppermint essential oil powder and sodium alginate is (3.5-3.9):1.
[0013] By adopting the above technical solution, the mass ratio of the starch-composite peppermint essential oil powder is preferably within the above range, which can further improve the overall stability of the prepared peppermint essential oil pellets.
[0014] Preferably, the mass ratio of chitosan to calcium chloride in the solidifying liquid is (1.3-1.5):1.
[0015] By adopting the above technical solution, preferably the mass ratio of chitosan to calcium chloride is within the above range, which can further improve the overall stability of the prepared peppermint essential oil pellets and the loading rate of peppermint essential oil.
[0016] Preferably, the menthol complex comprises menthol, silicon dioxide and dopamine hydrochloride.
[0017] By adopting the above technical scheme, mesoporous silica has a large porosity and an open pore structure and has good biocompatibility. By combining silica, dopamine hydrochloride and menthol, menthol is encapsulated in the pores of silica, and dopamine hydrochloride is used as an encapsulation coating to coat menthol, so that menthol can be slowly released, further improving the stability of menthol, and allowing menthol to be slowly released, thereby improving the stability of the cooling agent, and having a long-lasting cooling feeling and antibacterial properties.
[0018] Preferably, the menthol complex is prepared by the following method: The hexadecyltrimethylammonium bromide is mixed with water, heated and stirred, then ammonia water is added, stirring is continued, n-hexane and ethyl orthosilicate are added, stirring for reaction, centrifugation is performed to collect the product, and the product is washed and dried, the system is mixed with concentrated hydrochloric acid and anhydrous ethanol, reflux extraction is performed under magnetic stirring to remove the hexadecyltrimethylammonium bromide, and the product is washed and dried to obtain silica microspheres; menthol is mixed with anhydrous ethanol, silica microspheres are added, ultrasonic dispersion is performed, and then dopamine hydrochloride is added under stirring, stirring is continued, and tris(hydroxymethyl)aminomethane is added to react, after the reaction is completed, the product is centrifuged and collected, washed, and dried to obtain a menthol complex.
[0019] By adopting the above technical scheme, mesoporous silica with large pores is prepared by liquid-liquid interface co-assembly assisted by n-hexane, and the pores of the two mesoporous silica microspheres are used as containers for menthol. Further, by the interfacial polymerization method, dopamine hydrochloride is oxidatively polymerized on the surface of the mesoporous silica microspheres in an aqueous solution to achieve polydopamine coating on the outer surface of the silica microspheres, thereby allowing menthol to be slowly released and improving the overall stability of menthol.
[0020] Preferably, the mass ratio of menthol, silicon dioxide and dopamine is 1:1:(0.35-0.45).
[0021] By adopting the above technical solution, preferably the mass ratio of silicon dioxide, menthol and dopamine hydrochloride is within the above range, the stability of the prepared menthol complex can be further improved.
[0022] In a second aspect, the present application provides a method for preparing a cooling agent composite, using the following technical solution: A method for preparing a cooling agent composite comprises the following steps: The cooling agent complex is obtained by mixing SW-23, peppermint essential oil globules, menthol complex, potassium sorbate and sodium bicarbonate.
[0023] In summary, the present application includes at least one of the following beneficial technical effects: 1. Porous starch, peppermint essential oil, sodium alginate and chitosan are compounded to prepare peppermint essential oil spheres, thereby forming microcapsules, which can effectively embed peppermint essential oil and reduce the rapid inactivation and volatilization of peppermint essential oil, thereby achieving controllable release of peppermint essential oil and improving the stability of peppermint cooling agent; 2. The porous starch is obtained by hydrolyzing rice starch with α-amylase and saccharifying enzyme. After the surface of the rice starch is corroded, the saccharifying enzyme produces concave internal corrosion and pitting corrosion, thereby preparing a porous starch with a large specific surface area and high adsorption performance. The treated porous starch exposes more hydrophilic and oily groups, further improving the loading rate of menthol essential oil; 3. Through the combination of menthol and silica, menthol is encapsulated into the pores of silica, and then dopamine hydrochloride is used to coat the silica, so that menthol can be slowly released, thereby improving the stability of menthol and achieving a long-term antibacterial effect. DETAILED DESCRIPTION
[0024] The present application is further described in detail below with reference to the embodiments: Raw materials description: All raw materials in the examples can be obtained commercially; Example 1 Preparation of porous starch: A citric acid-disodium hydrogen phosphate buffer solution with a pH value of 7 is mixed with rice starch (CAS number: 68412-29-3) to obtain a starch suspension with a rice starch concentration of 20%, and the mixture is stirred and kept warm for 10 minutes at 50° C., and a mixed enzyme with a rice starch mass of 2% is added, wherein the mixed enzyme is alpha-amylase (CAS number: 9000-90-2) and saccharifying enzyme (CAS number: 9032-08-0) mixed in a mass ratio of 1:3, and the mixture is stirred at a constant temperature of 50° C. for 6 hours, and then a 0.1M sodium hydroxide solution is added to inactivate the mixed enzyme to stop the reaction. When the pH value of the starch suspension after the reaction is 10, the mixture is stirred for 2 minutes, and then sodium chloride is used to adjust the pH value of the system to 7, and the mixture is centrifuged at a speed of 4000 r / min for 5 minutes, and distilled water is used to wash 3 times, and the mixture is centrifuged again, and the mixture is frozen at a temperature of -18° C. for 6 hours, and then dried for 48 hours, and ground to obtain porous starch.
[0025] To prepare peppermint essential oil pellets: 20 g of porous starch was mixed with 30 g of peppermint essential oil (CAS No.: 68917-18-0), magnetically stirred for 2 h, then centrifuged at a speed of 4000 r / min for 20 min, washed repeatedly with anhydrous ethanol for 3 times, recovered the precipitate after centrifugation, and freeze-dried at a temperature of -18°C for 24 h to obtain starch composite peppermint essential oil powder; 38.89 g of peppermint starch composite powder, 11.11 g of sodium alginate (CAS No.: 9005-38-3) and 200 g of deionized water were mixed and stirred for 30 min to obtain a mixed system, 113.04 g of chitosan (CAS No.: chitosan) was mixed with 86.96 g of calcium chloride solution to obtain a solidified liquid, the mixed system was added to the solidified liquid, solidified at a temperature of 25°C for 30 min, filtered and washed with deionized water, and dried to obtain peppermint essential oil pellets.
[0026] Preparation of menthol complex: 5 g of hexadecyltrimethylammonium bromide (CAS No.: 57-09-0) was mixed with 600 ml of deionized water, heated to 35°C in a water bath, stirred until the system was transparent, then 15 ml of 28 wt% ammonia water was added, stirring was continued for 10 min, 100 ml of n-hexane and 25 ml of tetraethyl orthosilicate (CAS No.: 78-10-4) were added, the reaction was stirred for 12 h, the product was collected by centrifugation, washed with anhydrous ethanol, dried, mixed with 5 g of concentrated hydrochloric acid and 500 g of anhydrous ethanol, refluxed under magnetic stirring for 5 h, the hexadecyltrimethylammonium bromide was extracted, washed with ethanol, and dried in a vacuum oven at 80°C for 12 h to obtain to silica microspheres; 12.77 g of menthol (CAS No.: 89-78-1) was mixed with 250 g of anhydrous ethanol, 12.77 g of silica microspheres was added, and ultrasonic dispersion was performed at 25° C. for 30 min, and then 4.46 g of dopamine hydrochloride (CAS No.: 62-31-7) was added under magnetic stirring, and after continuing to stir, 0.2 g of trishydroxymethylaminomethane (CAS No.: 77-86-1) was added, and the temperature was raised to 30° C. for reaction, and stirring was maintained at a speed of 300 r / min. After the reaction was completed, the product was collected by centrifugation, and washed alternately with deionized water for 3 times, and dried in an oven at 30° C. to obtain a menthol complex.
[0027] Preparation of cooling agent complex: 40 g of SW-23, 28 g of peppermint essential oil globules, 22 g of menthol complex, 13 g of potassium sorbate (CAS No.: 24634-61-5), and 8 g of sodium bicarbonate were mixed to obtain a cooling agent complex.
[0028] Example 2 Preparation of porous starch: The citric acid-disodium hydrogen phosphate buffer solution is mixed with rice starch to obtain a starch suspension with a rice starch concentration of 20%, and the mixture is stirred and kept warm for 10 minutes at 50° C., and a mixed enzyme with a mass percentage of 2% of the rice starch is added, wherein the mixed enzyme is obtained by mixing alpha-amylase and saccharifying enzyme in a mass ratio of 1:3, and the mixture is stirred at a constant temperature of 50° C. for 6 hours, and then a 0.1M sodium hydroxide solution is added to inactivate the mixed enzyme to stop the reaction. When the pH value of the starch suspension after the reaction is 10, the mixture is stirred for 2 minutes, and then sodium chloride is used to adjust the pH value of the system to 7, and the mixture is centrifuged at a speed of 4000 r / min for 5 minutes, and distilled water is used to wash 3 times, and the mixture is centrifuged again, and the mixture is frozen at a temperature of -18° C. for 6 hours, and then dried for 48 hours, and ground to obtain porous starch.
[0029] To prepare peppermint essential oil pellets: 20 g of porous starch was mixed with 30 g of peppermint essential oil, magnetically stirred for 2 h, and then centrifuged at a speed of 4000 r / min for 20 min, washed repeatedly with anhydrous ethanol for 3 times, and the precipitate was recovered after centrifugation, and freeze-dried at a temperature of -18°C for 24 h to obtain starch composite peppermint essential oil powder; 39.8 g of peppermint starch composite powder, 10.2 g of sodium alginate and 200 g of deionized water were mixed, stirred for 30 min to obtain a mixed system, 120 g of chitosan was mixed with 80 g of calcium chloride solution to obtain a solidified liquid, the mixed system was added to the solidified liquid, solidified at a temperature of 25°C for 30 min, filtered, washed with deionized water, and dried to obtain peppermint essential oil pellets.
[0030] Preparation of menthol complex: 5 g of hexadecyltrimethylammonium bromide was mixed with 600 ml of deionized water, heated to 35° C. in a water bath, stirred until the system was transparent, then 15 ml of 28 wt% ammonia water was added, stirring was continued for 10 min, 100 ml of n-hexane and 25 ml of ethyl orthosilicate were added, stirred for 12 h, the product was collected by centrifugation, washed with anhydrous ethanol, dried, mixed with 5 g of concentrated hydrochloric acid and 500 g of anhydrous ethanol, refluxed under magnetic stirring for 5 h, the hexadecyltrimethylammonium bromide was extracted, washed with ethanol, and then placed in a vacuum oven at 80° C. Dry for 12 hours to obtain silica microspheres; mix 12.24 g of menthol with 250 g of anhydrous ethanol, add 12.24 g of silica microspheres, ultrasonically disperse at 25°C for 30 minutes, then add 5.52 g of dopamine hydrochloride under magnetic stirring, continue stirring, add 0.2 g of tris(hydroxymethyl)aminomethane, heat to 30°C for reaction, and maintain stirring at 300 r / min. After the reaction is completed, collect the product by centrifugation, wash it alternately with deionized water 3 times, and dry it in an oven at 30°C to obtain a menthol complex.
[0031] Preparation of cooling agent complex: 50 g of SW-23, 32 g of peppermint essential oil globules, 26 g of menthol complex, 15 g of potassium sorbate, and 12 g of sodium bicarbonate were mixed to obtain a cooling agent complex.
[0032] Example 3 Preparation of porous starch: The citric acid-disodium hydrogen phosphate buffer solution is mixed with rice starch to obtain a starch suspension with a rice starch concentration of 20%, and the mixture is stirred and kept warm for 10 minutes at 50° C., and a mixed enzyme with a mass percentage of 2% of the rice starch is added, wherein the mixed enzyme is obtained by mixing alpha-amylase and saccharifying enzyme in a mass ratio of 1:3, and the mixture is stirred at a constant temperature of 50° C. for 6 hours, and then a 0.1M sodium hydroxide solution is added to inactivate the mixed enzyme to stop the reaction. When the pH value of the starch suspension after the reaction is 10, the mixture is stirred for 2 minutes, and then sodium chloride is used to adjust the pH value of the system to 7, and the mixture is centrifuged at a speed of 4000 r / min for 5 minutes, and distilled water is used to wash 3 times, and the mixture is centrifuged again, and the mixture is frozen at a temperature of -18° C. for 6 hours, and then dried for 48 hours, and ground to obtain porous starch.
[0033] To prepare peppermint essential oil pellets: 20 g of porous starch was mixed with 30 g of peppermint essential oil, magnetically stirred for 2 h, and then centrifuged at a speed of 4000 r / min for 20 min, washed repeatedly with anhydrous ethanol for 3 times, and the precipitate was recovered after centrifugation, and freeze-dried at a temperature of -18°C for 24 h to obtain starch composite peppermint essential oil powder; 39.36 g of peppermint starch composite powder, 10.64 g of sodium alginate and 200 g of deionized water were mixed, stirred for 30 min to obtain a mixed system, 116.67 g of chitosan was mixed with 83.33 g of calcium chloride solution to obtain a solidified liquid, the mixed system was added to the solidified liquid, solidified at a temperature of 25°C for 30 min, filtered, washed with deionized water, and dried to obtain peppermint essential oil pellets.
[0034] Preparation of menthol complex: 5 g of hexadecyltrimethylammonium bromide was mixed with 600 ml of deionized water, heated to 35° C. in a water bath, stirred until the system was transparent, then 15 ml of 28 wt% ammonia water was added, stirring was continued for 10 min, 100 ml of n-hexane and 25 ml of ethyl orthosilicate were added, stirred for 12 h, the product was collected by centrifugation, washed with anhydrous ethanol, dried, mixed with 5 g of concentrated hydrochloric acid and 500 g of anhydrous ethanol, refluxed under magnetic stirring for 5 h, the hexadecyltrimethylammonium bromide was extracted, washed with ethanol, and then refluxed under vacuum at 80° C. The mixture was dried in an oven for 12 hours to obtain silica microspheres; 12.5 g of menthol was mixed with 250 g of anhydrous ethanol, 12.5 g of silica microspheres were added, and ultrasonic dispersion was performed at 25°C for 30 minutes. Then, 5 g of dopamine hydrochloride was added under magnetic stirring, and after continued stirring, 0.2 g of tris(hydroxymethyl)aminomethane was added. The mixture was heated to 30°C for reaction and stirred at a speed of 300 r / min. After the reaction was completed, the product was collected by centrifugation and washed alternately with deionized water for 3 times, and dried in an oven at 30°C to obtain a menthol complex.
[0035] Preparation of cooling agent complex: 45 g of SW-23, 30 g of peppermint essential oil globules, 24 g of menthol complex, 14 g of potassium sorbate, and 10 g of sodium bicarbonate were mixed to obtain a cooling agent complex.
[0036] Example 4 Example 4 is based on Example 3. The difference between Example 4 and Example 3 is that when preparing the peppermint essential oil pellets, 37.5 g of peppermint starch composite powder and 12.5 g of sodium alginate are used.
[0037] Example 5 Example 5 is based on Example 3. The difference between Example 5 and Example 3 is that when preparing the peppermint essential oil balls, 40.74 g of peppermint starch composite powder and 9.26 g of sodium alginate are used.
[0038] Example 6 Example 6 is based on Example 3. The difference between Example 6 and Example 3 is that when preparing peppermint essential oil beads, 104.76 g of chitosan and 95.24 g of calcium chloride are used in the solidifying liquid.
[0039] Example 7 Example 7 is based on Example 3. The difference between Example 7 and Example 3 is that when preparing peppermint essential oil beads, 125.93 g of chitosan and 74.07 g of calcium chloride are used in the solidifying liquid.
[0040] Example 8 Example 8 is based on Example 3. The difference between Example 8 and Example 3 is that when preparing the menthol complex, the amount of menthol used is 13.64 g, the amount of silica microspheres used is 13.64 g, and the amount of dopamine hydrochloride used is 2.72 g.
[0041] Example 9 Example 9 is based on Example 3. The difference between Example 9 and Example 3 is that when preparing the menthol complex, the amount of menthol used is 11.54 g, the amount of silica microspheres used is 11.54 g, and the amount of dopamine hydrochloride used is 6.92 g.
[0042] Example 10 Example 10 is based on Example 3. The difference between Example 10 and Example 3 is that when preparing the peppermint essential oil balls, the porous starch is replaced by ordinary rice starch.
[0043] Embodiment 11 Example 11 is based on Example 3. The difference between Example 11 and Example 3 is that dopamine is not added when preparing the menthol complex.
[0044] Comparative Example 1 Comparative Example 1 is based on Example 3, and in Comparative Example 1, the peppermint essential oil spheres are replaced with an equal amount of peppermint starch composite powder.
[0045] Comparative Example 2 Comparative Example 2 is based on Example 3, and in Comparative Example 2, the menthol complex is replaced by ordinary menthol.
[0046] Performance testing The following performance tests were performed on the samples of Examples 1-11 and Comparative Examples 1-2: (1) Antibacterial performance test The antibacterial properties of the samples were tested according to GB / T 22731-2022, and the antibacterial properties were recorded after 3 and 7 days of culture. Each sample was tested three times, and the average value was taken. The test results were filled in Table 1.
[0047] (2) Flavor release test Twenty healthy persons with normal sense of smell and taste and who had not recently suffered from cold, rhinitis and other diseases were selected as test persons. 5 g of sample was dispersed in 100 mL of deionized water to obtain a sample dispersion. A blank control solution without adding sample was set. The filter paper disc was soaked in the sample dispersion for 5 minutes and then taken out. The test persons put the soaked filter paper disc into their mouths and recorded the time when the cool taste 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.
[0048] Table 1 Test results of samples of Examples 1-11 and Comparative Examples 1-2 Combined with Table 1, it can be seen that in Examples 1-3, after 3 days, the antibacterial rate of Escherichia coli is 99.87% and above, and the antibacterial rate of Staphylococcus aureus is 99.85% and above. After 21 days, the antibacterial rate of Escherichia coli is 97.79% and above, and the antibacterial rate of Staphylococcus aureus is 97.84% and above, indicating that the cooling composite prepared by the present application has good antibacterial performance and long-term antibacterial performance; the release duration of Examples 1-3 is 45 minutes or more, indicating that the cooling composite prepared by the present application has good long-term release performance and stability.
[0049] In Example 4 and Example 5, when preparing the peppermint essential oil spheres, the mass ratio of the peppermint starch composite powder to the sodium alginate is not within the range defined in the present application. When the content of the peppermint starch composite powder is too much, the spheres are difficult to form, and the viscosity of the system also decreases, the coating of the peppermint starch composite powder is incomplete, part of the essential oil is exposed and volatilized, the embedding rate decreases, and the overall stability of the system also decreases, which affects both the antibacterial performance and the release performance; when the content of the peppermint starch composite powder is too little, due to the presence of porous starch and the excessively high concentration of sodium alginate, the viscosity of the system increases rapidly, making it difficult to evenly disperse the system, and the peppermint essential oil spheres are also difficult to form, adhesion occurs, and the embedding performance decreases, affecting the stability of the system, so the performance of Example 4 and Example 5 are both reduced.
[0050] In the preparation of peppermint essential oil pellets in Examples 6 and 7, the mass ratio of chitosan to calcium chloride in the solidifying solution was not within the range specified in the present application. When the content of calcium chloride was too low, Ca 2+ When the content of calcium chloride is insufficient, ion exchange is difficult to occur, the formed calcium alginate skeleton is weak, and the embedding rate of the core material is difficult to further increase, resulting in a decrease in the content of menthol essential oil; when the content of calcium chloride is too high, excessive Ca 2+ This will reduce the stability of the essential oil globules, causing the core material to overflow and the stability of the system to decrease, so the performance of both Example 6 and Example 7 is reduced.
[0051] In Example 8 and Example 9, when preparing the menthol complex, the mass ratios of menthol, silica microspheres and dopamine hydrochloride are not within the range specified in the present application. When the content of dopamine is too little, it is difficult to further coat the silica microspheres loaded with menthol, and it is difficult for menthol to further achieve the performance of slow release, and it is difficult to further improve the stability of menthol. When the content of dopamine is too much, the silica microspheres loaded with menthol are over-coated, resulting in excessive particle size, which affects the overall uniformity and dispersibility of the system, and reduces the release effect of menthol. Therefore, the performance of Example 8 and Example 9 are both reduced.
[0052] In Example 10, when preparing the peppermint essential oil pellets, the porous starch was replaced with ordinary rice starch. The surface area of the rice starch that was not treated with a composite enzyme was difficult to further increase, so that the loading rate of the peppermint essential oil decreased, and it was difficult to further improve the antibacterial performance and release performance of the system. Therefore, the performance of Example 10 was reduced.
[0053] The menthol complex of Example 11 does not have dopamine added, and the silica microspheres without dopamine added are difficult to be further coated. Menthol is quickly released from the silica microspheres, causing the menthol to be quickly inactivated, so the performance of Example 11 is reduced.
[0054] In Comparative Example 1, the peppermint essential oil pellets are replaced with an equal amount of peppermint starch composite powder. Only the peppermint powder composite starch is added to the system without being coated, which causes the peppermint essential oil to be released quickly and evaporate quickly, making it difficult to achieve long-term sustained release performance, and it is also difficult to further improve the antibacterial performance of the system. Therefore, the performance of Comparative Example 1 is reduced.
[0055] In Comparative Example 2, the menthol complex was replaced with ordinary menthol. The uncoated menthol evaporated quickly in the system and quickly lost its activity. Therefore, it was difficult for menthol to play a long-term release role, which also affected the long-term antibacterial performance of the system. Therefore, the performance of Comparative Example 2 was reduced.
[0056] 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 composite, characterized in that: The composition includes the following components by mass: 40-50 parts of sw-23, 28-32 parts of peppermint essential oil globules, 22-26 parts of menthol complex, 13-15 parts of potassium sorbate, 8-12 parts of sodium bicarbonate; The raw materials of the peppermint essential oil pellets include peppermint essential oil, porous starch, sodium alginate and chitosan.
2. A cooling agent composite according to claim 1, characterized in that: The porous starch is prepared by the following method: The citric acid-disodium hydrogen phosphate buffer solution is mixed with rice starch to obtain a starch suspension and stirred, alpha-amylase and saccharifying enzyme are added and stirred, and then a sodium hydroxide solution is added to inactivate the mixed enzyme to stop the reaction, centrifugation washing, freeze drying, and grinding to obtain porous starch.
3. A cooling agent composite according to claim 1, characterized in that: The peppermint essential oil spheres are prepared by the following method: The porous starch is mixed with peppermint essential oil, and the mixture is centrifuged and washed after magnetic stirring. The precipitate is recovered after centrifugation again, and freeze-dried to obtain starch-composite peppermint essential oil powder. The peppermint starch composite powder, sodium alginate and water are mixed and stirred to obtain a mixed system, chitosan is mixed with a calcium chloride solution to obtain a solidified liquid, the mixed system is added to the solidified liquid for solidification, and the mixture is filtered, washed and dried to obtain peppermint essential oil pellets.
4. A cooling agent composite according to claim 3, characterized in that: The mass ratio between the starch composite peppermint essential oil powder and the sodium alginate is (3.5-3.9):
1.
5. The cooling agent composite according to claim 3, characterized in that: The mass ratio of chitosan to calcium chloride in the solidifying liquid is (1.3-1.5):
1.
6. The cooling agent composite according to claim 1, characterized in that: The menthol complex comprises menthol, silicon dioxide and dopamine hydrochloride.
7. A cooling agent composite according to claim 6, characterized in that: The menthol complex is prepared by the following method: The hexadecyltrimethylammonium bromide is mixed with water, heated and stirred, then ammonia water is added, stirring is continued, n-hexane and ethyl orthosilicate are added, stirring for reaction, centrifugation is performed to collect the product, and the product is washed and dried, the system is mixed with concentrated hydrochloric acid and anhydrous ethanol, reflux extraction is performed under magnetic stirring to remove the hexadecyltrimethylammonium bromide, and the product is washed and dried to obtain silica microspheres; menthol is mixed with anhydrous ethanol, silica microspheres are added, ultrasonic dispersion is performed, and then dopamine hydrochloride is added under stirring, stirring is continued, and tris(hydroxymethyl)aminomethane is added to react, after the reaction is completed, the product is centrifuged and collected, washed, and dried to obtain a menthol complex.
8. A cooling agent composite according to claim 7, characterized in that: The mass ratio of the menthol, silicon dioxide and dopamine is 1:1:(0.35-0.45).
9. A method for preparing the cooling agent composite according to any one of claims 1 to 8, characterized in that: The steps include: The cooling agent complex is obtained by mixing SW-23, peppermint essential oil globules, menthol complex, potassium sorbate and sodium bicarbonate.