Cooling agent compound and preparation method thereof

Abstract

The invention relates to a cooling agent composition and a preparation method thereof. The cooling agent composition comprises a composite wall material microcapsule, sw-23, limonene, potassium sorbate and an antioxidant, the composite wall material microcapsule comprises menthol, shea butter, candelilla wax and a water phase. The cooling agent compound disclosed by the invention has the effects of improving the flavor release performance of the cooling agent compound, and having good antibacterial activity and long-acting stability.

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. They are often used in food additives.

[0003] Cooling agents are usually composed of menthol as the main substance. Menthol is a left-handed, colorless needle-shaped crystal that is soluble in ethanol and miscible with oils. It has a cool, fresh, and pleasant mint aroma with a sweet, thorny smell, giving people a cool feeling. The aroma is penetrating, and the taste is also fresh, sweet, and cool. With the increase in demand for a cool taste, menthol is generally compounded with other cooling agents to enhance the coolness and flavor of the cooling agent. However, menthol and other cooling agents are not resistant to high temperatures and are easily volatile. They have poor stability at room temperature and a short duration of coolness, so there is room for improvement. Summary of the invention

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

[0005] 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 compound comprises a composite wall material microcapsule, SW-23, limonene, potassium sorbate and an antioxidant. The composite wall material microcapsule comprises a menthol compound, shea butter, candelilla wax and an aqueous phase.

[0006] By adopting the above technical scheme, menthol is easily released, resulting in the loss of menthol effective ingredients. Menthol is embedded to prepare composite wall material microcapsules, so that the stability of the prepared menthol is improved, and menthol can be slowly released, thereby prolonging the duration of the cooling flavor. Menthol also has good antibacterial properties. The composite wall material microcapsules are prepared, so that the cooling agent composition has long-lasting antibacterial properties.

[0007] Preferably, the composite wall material microcapsule is prepared by the following method: After mixing shea butter, candelilla wax and menthol complex, heating and stirring in a water bath condition to obtain an oil phase; adding the oil phase to the water phase, and then shearing and dispersing to obtain a pre-emulsion, homogenizing the pre-emulsion to obtain a nanoemulsion, cooling the nanoemulsion to obtain a particle dispersion, centrifuging the particle dispersion, and then washing, centrifuging again, and drying to obtain a composite wall material microcapsule.

[0008] By adopting the above technical scheme, wood oil is added to the base of candelilla wax and used as a packaging carrier after mixing to destroy the highly ordered crystalline structure of a single solid lipid, thereby effectively increasing the loading capacity and stability of the microcapsule for the menthol complex and further improving the thermal stability of the microcapsule, thereby further improving the overall stability of the system.

[0009] Preferably, the mass ratio of the shea butter, candelilla wax and menthol complex is 1:3:(4.1-4.3).

[0010] By adopting the above technical solution, the mass ratio of the shea butter, candelilla wax and menthol complex is preferably within the above range, which can further improve the stability of the prepared composite wall material microcapsules.

[0011] Preferably, the aqueous phase comprises sodium starch octenylsuccinate and water.

[0012] By adopting the above technical scheme, sodium starch octenyl succinate is a modified starch obtained by esterification reaction between a starch derivative and octenyl succinic anhydride. The modified starch introduces a hydrophobic octenyl group, thereby making the starch amphiphilic, reducing the aggregation of starch particles, and being able to be evenly dispersed in the emulsion system, so that the emulsion has good fluidity and effectively improves the loading rate of the menthol complex for the composite wall material microcapsule.

[0013] Preferably, the mass ratio between the oil phase and sodium starch octenyl succinate is (0.68-0.72):1.

[0014] By adopting the above technical solution, preferably the mass ratio between the oil phase and the sodium starch octenyl succinate is within the above range, which can further improve the overall stability of the prepared composite wall material microcapsules.

[0015] Preferably, the menthol complex comprises menthol, activated carbon and corn starch.

[0016] By adopting the above technical solution, corn starch particles are mainly composed of straight-chain starch and amylopectin, and form starch complexes with menthol through hydrophobic interaction, thereby improving the stability of menthol. After the activated carbon and menthol are compounded, the menthol is encapsulated in the gaps of the activated carbon, making the menthol more stable in the system and improving the persistence of the flavor of the menthol during subsequent release. At the same time, the thermal stability of menthol is improved. After the activated carbon, corn starch and menthol are compounded, the stability of menthol is synergistically promoted.

[0017] Preferably, the mass ratio of the corn starch, activated carbon and menthol is 1:1.2:(0.9-1.3).

[0018] By adopting the above technical solution, preferably the mass ratio of menthol, corn starch and activated carbon is within the above range, which can further improve the stability of the prepared menthol complex.

[0019] Preferably, the menthol complex is prepared by the following method: The menthol is heated and melted, and then the activated carbon is mixed with the melted menthol, and the composite menthol is obtained after stirring. The corn starch is mixed with water to obtain a corn starch solution, which is shaken and treated in a boiling water bath to completely dissolve the corn starch. After cooling, the composite menthol is added to the corn starch solution, shaken, ultrasonicated, and freeze-dried to obtain a menthol complex.

[0020] 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 combination comprises the following steps: The composite wall material microcapsule, SW-23, limonene, potassium sorbate and antioxidant are mixed to obtain a cooling agent composition.

[0021] In summary, the present application includes at least one of the following beneficial technical effects: 1. The menthol complex is encapsulated in the microcapsule. After the menthol complex is encapsulated, the stability of menthol in the system can be effectively improved, and the phenomenon of rapid inactivation of menthol can be reduced. In addition, menthol can be slowly released, thereby prolonging the duration of the cooling flavor. In addition, menthol has good antibacterial properties, and can play a synergistic antibacterial role with SW-23, and has a long-lasting antibacterial effect, so that the stability and performance of the cooling agent composition are improved; 2. When preparing the composite wall material microcapsule, the menthol complex is encapsulated in sodium starch octenyl succinate to stabilize menthol in an amorphous form for a long time, thereby improving the thermal stability and loading capacity of menthol, prolonging the storage performance of menthol, and achieving the effect of long-term release of flavor; 3. Corn starch and activated carbon are added to the menthol complex. The corn starch and menthol form a starch complex through hydrophobic interaction, which further improves the stability of menthol. After the activated carbon and menthol are compounded with each other, the flavor release performance of menthol can be further improved, so that the cool feeling can be released for a long time, achieving the effect of preserving the fragrance. DETAILED DESCRIPTION

[0022] The present application is further described in detail below with reference to the embodiments: Description of raw materials: All raw materials in the examples are commercially available, and the antioxidant is sodium D-isoascorbate (CAS No.: 7378-23-6).

[0023] Example 1 Preparation of menthol complex: 11.62 g of menthol (CAS No.: 89-78-1) was heated to 40°C to melt the menthol, and then 15.48 g of activated carbon was mixed with the melted menthol, and the composite menthol was obtained after stirring. 12.9 g of corn starch (CAS No.: 9005-25-8) was mixed with 150 g of distilled water to obtain a corn starch solution, which was shaken and treated in a boiling water bath for 1 hour to completely dissolve the corn starch. After cooling to 40°C, the composite menthol was added to the corn starch solution, which was sealed and shaken, and then ultrasonicated for 30 minutes, and then placed in a temperature environment of 4°C for 24 hours, and finally freeze-dried at a temperature of -20°C to obtain a menthol complex.

[0024] Preparation of composite wall material microcapsules: 6.17 g of shea butter (CAS No.: 91080-23-8), 18.52 g of candelilla wax (CAS No.: 8006-44-8) and 25.31 g of menthol complex were mixed, and heated in a water bath at 80°C and stirred for 2 h until the lipid was completely dissolved to obtain an oil phase; 29.77 g of sodium starch glycolate (CAS No.: 66829-29-6) was mixed with 70 g of deionized water, stirred and hydrated, and then stirred in a water bath at 90°C for 2 h to obtain an aqueous phase; 2 0.23 g of the oil phase was added to the aqueous phase, and then a high-speed dispersant was used to shear and disperse at a speed of 10000 r / min for 1 min to obtain a pre-emulsion, the pre-emulsion was homogenized under a pressure of 800 bar to obtain a nanoemulsion, the nanoemulsion was cooled to 25°C to obtain a particle dispersion, the particle dispersion was centrifuged at a speed of 8000 r / min for 25 min, and then washed with deionized water and centrifuged again, the washing and centrifugation were repeated 3 times, and the mixture was dried in a vacuum drying oven at 38°C for 18 h to obtain composite wall material microcapsules.

[0025] Preparation of cooling agent composition: A cooling agent composition was obtained by mixing 13 g of composite wall material microcapsules, 60 g of SW-23 (CAS No.: 51115-67-4), 14 g of limonene (CAS No.: 138-86-3), 10 g of potassium sorbate (CAS No.: 24634-61-5) and 3 g of an antioxidant.

[0026] Example 2 Preparation of menthol complex: 14.86 g of menthol was heated to 40° C. to melt the menthol, and then 13.71 g of activated carbon was mixed with the melted menthol, and the composite menthol was obtained after stirring. 11.43 g of corn starch was mixed with 150 g of distilled water to obtain a corn starch solution, which was shaken and treated in a boiling water bath for 1 hour to completely dissolve the corn starch. After cooling to 40° C., the composite menthol was added to the corn starch solution, which was sealed and shaken, and then ultrasonicated for 30 minutes, and then placed in a temperature environment of 4° C. for 24 hours, and finally freeze-dried at a temperature of -20° C. to obtain a menthol complex.

[0027] Preparation of composite wall material microcapsules: 6.02 g of shea butter, 18.07 g of candelilla wax and 25.91 g of menthol complex were mixed, heated and stirred in a water bath at 80° C. for 2 h until the lipid was completely dissolved to obtain an oil phase; 29.07 g of sodium starch octenylsuccinate was mixed with 70 g of deionized water, stirred and hydrated, and then stirred in a water bath at 90° C. for 2 h to obtain an aqueous phase; 20.93 g of the oil phase was added to the aqueous phase, and then a high-speed dispersant was used for shear dispersion at a speed of 10000 r / min for 1 min to obtain a pre-emulsion, the pre-emulsion was homogenized under a pressure of 800 bar to obtain a nanoemulsion, the nanoemulsion was cooled to 25° C. to obtain a particle dispersion, the particle dispersion was centrifuged at a speed of 8000 r / min for 25 min, the aqueous phase was removed, and then washed with deionized water, centrifuged again, the washing and centrifugation were repeated 3 times, and the composite wall material microcapsules were dried in a vacuum drying oven at 38° C. for 18 h.

[0028] Preparation of cooling agent composition: A cooling agent composition was obtained by mixing 19 g of composite wall material microcapsules, 46 g of SW-23, 18 g of limonene, 12 g of potassium sorbate and 5 g of an antioxidant.

[0029] Example 3 Preparation of menthol complex: 13.33 g of menthol was heated to 40° C. to melt the menthol, and then 14.55 g of activated carbon was mixed with the melted menthol, and stirred to obtain a composite menthol. 12.12 g of corn starch was mixed with 150 g of distilled water to obtain a corn starch solution, which was shaken and treated in a boiling water bath for 1 hour to completely dissolve the corn starch. After cooling to 40° C., the composite menthol was added to the corn starch solution, which was sealed and shaken, and then ultrasonicated for 30 minutes, and then placed at a temperature of 4° C. for 24 hours, and finally freeze-dried at a temperature of -20° C. to obtain a menthol complex.

[0030] Preparation of composite wall material microcapsules: 6.1 g of shea butter, 18.29 g of candelilla wax and 25.61 g of menthol complex were mixed, heated and stirred in a water bath at 80° C. for 2 h until the lipid was completely dissolved to obtain an oil phase; 20.59 g of sodium starch octenylsuccinate was mixed with 70 g of deionized water, stirred and hydrated, and then stirred in a water bath at 90° C. for 2 h to obtain an aqueous phase; 29.41 g of the oil phase was added to the aqueous phase, and then a high-speed dispersant was used for shear dispersion at a speed of 10000 r / min for 1 min to obtain a pre-emulsion, the pre-emulsion was homogenized under a pressure of 800 bar to obtain a nanoemulsion, the nanoemulsion was cooled to 25° C. to obtain a particle dispersion, the particle dispersion was centrifuged at a speed of 8000 r / min for 25 min, the aqueous phase was removed, and then washed with deionized water, centrifuged again, the washing and centrifugation were repeated 3 times, and the composite wall material microcapsules were dried in a vacuum drying oven at 38° C. for 18 h.

[0031] Preparation of cooling agent composition: A cooling agent composition was obtained by mixing 16 g of composite wall material microcapsules, 53 g of SW-23, 16 g of limonene, 11 g of potassium sorbate and 4 g of an antioxidant.

[0032] Example 4 Example 4 is based on Example 3. The difference between Example 4 and Example 3 is that in Example 4, when preparing the menthol complex, 14.81 g of corn starch, 17.78 g of activated carbon and 7.41 g of menthol are used.

[0033] Example 5 Example 5 is based on Example 3. The difference between Example 5 and Example 3 is that in Example 5, when preparing the menthol complex, 10.26 g of corn starch, 12.31 g of activated carbon and 17.43 g of menthol are used.

[0034] Example 6 Example 6 is based on Example 3. The difference between Example 6 and Example 3 is that in Example 6, no corn starch is added when preparing the menthol complex.

[0035] Example 7 Example 7 is based on Example 3. The difference between Example 7 and Example 3 is that in Example 7, no activated carbon is added when preparing the menthol complex.

[0036] Example 8 Example 8 is based on Example 3. The difference between Example 8 and Example 3 is that in Example 8, when preparing the oil phase, 6.41 g of shea butter, 19.23 g of candelilla wax and 24.36 g of menthol complex are used.

[0037] Example 9 Example 9 is based on Example 3. The difference between Example 9 and Example 3 is that in Example 9, when preparing the oil phase, 5.81 g of shea butter, 17.44 g of candelilla wax and 26.75 g of menthol complex are used.

[0038] Example 10 Example 10 is based on Example 3. The difference between Example 10 and Example 3 is that in Example 10, 30.3 g of sodium starch octenyl succinate and 19.7 g of oil phase are used in preparing composite wall material microcapsules.

[0039] Embodiment 11 Example 11 is based on Example 3. The difference between Example 11 and Example 3 is that in Example 11, 28.57 g of sodium starch octenyl succinate and 21.43 g of oil phase are used in preparing composite wall material microcapsules.

[0040] Comparative Example 1 Comparative Example 1 is based on Example 3. In Comparative Example 1, when preparing the composite wall material microcapsules, the menthol complex is replaced with ordinary menthol.

[0041] Comparative Example 2 Comparative Example 2 is based on Example 3. In Comparative Example 2, when preparing the composite wall material microcapsules, the composite wall material microcapsules are replaced with menthol.

[0042] 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.

[0043] (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.

[0044] Table 1 Test results of samples of Examples 1-11 and Comparative Examples 1-2 Combined with Table 1, it can be seen that the antibacterial properties of Examples 1-3 are all x and above, indicating that the cooling agent combination prepared in the present application has good antibacterial properties, and the concentrations of Examples 1-3 are all x and above, indicating that the cooling agent composition prepared in the present application has good flavor release intensity.

[0045] In Example 4 and Example 5, when preparing the menthol complex, the mass ratio of corn starch, activated carbon and menthol is not within the range specified in the present application. When the menthol content is too low, the menthol content on the surface of the activated carbon is low, and there are many voids on the surface of the activated carbon. It is also difficult to further improve the composite rate with corn starch, and the corn starch also has certain voids. When the menthol content is too high, the composite between menthol and corn starch and activated carbon reaches saturation, and it is difficult to further improve the binding rate between the various systems in the menthol complex, making it difficult to further improve the stability. Therefore, the various performances of Example 4 and Example 5 are reduced.

[0046] In Example 6, when preparing the menthol complex, no corn starch was added, and only the menthol and the activated carbon were combined, which made it difficult to further combine with the menthol to form a starch complex. The stability of the menthol complex was difficult to improve, and therefore, the performance of Example 6 was reduced.

[0047] In Example 7, when preparing the menthol complex, no activated carbon was added, and the menthol was difficult to be further encapsulated, and the stability of menthol was difficult to be further improved. Therefore, the performance of Example 7 was reduced.

[0048] In Example 8 and Example 9, when preparing the oil phase of the composite wall material microcapsule, the mass ratio of shea butter, candelilla wax and menthol complex is not within the range defined in the present application. When the content of the menthol complex is too much or too little, the embedding rate of the menthol complex is affected, and it is difficult to obtain a stable composite wall material microcapsule. Therefore, the performance of Example 8 and Example 9 is reduced.

[0049] In Example 10 and Example 11, when preparing composite wall material microcapsules, the mass ratio between sodium starch octenyl succinate and the oil phase is not within the range specified in the present application. When the content of sodium starch octenyl succinate is too little, the oil phase is difficult to emulsify, resulting in reduced stability of the prepared nanoemulsion; when the content of sodium starch octenyl succinate is too much, it is difficult to increase the loading amount of the menthol complex, and therefore, the performance of Example 10 and Example 11 is reduced.

[0050] In comparative example 1, when preparing composite wall material microcapsules, the menthol complex was replaced with ordinary menthol. Ordinary menthol is difficult to combine to form a complex with hydrophobic properties and is also difficult to further encapsulate. Therefore, the performance of the cooling agent complex of comparative example 1 is reduced.

[0051] In Comparative Example 2, the composite wall material microcapsules were replaced with ordinary menthol. Ordinary menthol easily loses its activity, and its stability is difficult to be further improved, and it is also difficult to achieve long-term antibacterial performance. Therefore, the performance of Comparative Example 2 is reduced.

[0052] 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: Including composite wall microcapsules, sw-23, limonene, potassium sorbate and antioxidants The composite wall material microcapsule comprises menthol, shea butter, candelilla wax and a water phase.

2. The cooling agent composite according to claim 1, characterized in that: The composite wall material microcapsules are prepared by the following method: After mixing shea butter, candelilla wax and menthol complex, heating and stirring in a water bath condition to obtain an oil phase; adding the oil phase to the water phase, and then shearing and dispersing to obtain a pre-emulsion, homogenizing the pre-emulsion to obtain a nanoemulsion, cooling the nanoemulsion to obtain a particle dispersion, centrifuging the particle dispersion, and then washing, centrifuging again, and drying to obtain a composite wall material microcapsule.

3. A cooling agent composite according to claim 2, characterized in that: The mass ratio of the shea butter, candelilla wax and menthol is 1:3:(4.1-4.3).

4. The cooling agent composite according to claim 2, characterized in that: The aqueous phase comprises sodium starch octenyl succinate and water.

5. A cooling agent composite according to claim 4, characterized in that: The mass ratio between the oil phase and sodium starch octenyl succinate is (0.68-0.72):

1.

6. The cooling agent composite according to claim 1, characterized in that: The menthol complex comprises menthol, activated carbon and corn starch.

7. The cooling agent composite according to claim 6, characterized in that: The mass ratio of the corn starch, activated carbon and menthol is 1:1.2:(0.9-1.3).

8. A cooling agent composite according to claim 6, characterized in that: The menthol complex is prepared by the following method: The menthol is heated and melted, and then the activated carbon is mixed with the melted menthol, and the composite menthol is obtained after stirring. The corn starch is mixed with water to obtain a corn starch solution, which is shaken and treated in a boiling water bath to completely dissolve the corn starch. After cooling, the composite menthol is added to the corn starch solution, shaken, ultrasonicated, and freeze-dried to obtain a menthol complex.

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 composite wall material microcapsule, SW-23, limonene, potassium sorbate and antioxidant are mixed to obtain a cooling agent composition.

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