Microcapsule embedding preparation method of milk-flavor essence resistant to high-temperature baking
By mixing milk flavoring with specific components and constructing a dense wall matrix to form high-temperature resistant microcapsules, the problem of flavor loss of milk flavoring during baking is solved, and flavor retention is achieved during high-temperature baking.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- GUANGDONG HENGYU BIOTECHNOLOGY CO LTD
- Filing Date
- 2026-03-23
- Publication Date
- 2026-05-12
AI Technical Summary
Traditional milk flavorings are prone to volatility and oxidation during baking, resulting in significant flavor loss and failing to achieve the desired flavor enhancement effect.
A stable first mixture is formed by uniformly mixing milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan. Then, modified chitosan, octenyl succinate starch, and sodium caseinate are dissolved in water, and sodium tripolyphosphate is added to construct a dense wall material matrix. Finally, high-temperature resistant microcapsules are formed by homogenization and vacuum freeze-drying.
It achieves efficient encapsulation and high-temperature preservation of milk flavoring, improving the flavor stability and aroma retention time of baked goods.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of flavor technology, specifically to a method for preparing a high-temperature resistant baking milk flavor by microcapsule encapsulation. Background Technology
[0002] Milk flavoring is one of the most widely used flavor additives in baked goods. It can significantly enhance the milky flavor and improve the texture of baked products, meeting consumers' demand for milky-flavored foods. However, the core flavor components of traditional milk flavorings mostly have low boiling points and poor thermal stability. During the baking process, they are prone to volatilization, oxidation, and degradation, resulting in severe loss of milky flavor, short aroma retention time, and even off-flavors, failing to achieve the expected flavor enhancement effect.
[0003] To address the aforementioned issues, existing technologies commonly employ microencapsulation to encapsulate milk flavorings. The core-shell structure formed by the encapsulation material blocks heat conduction and oxygen permeation, reducing heat loss of flavor components. Currently, commonly used microcapsule wall materials include single or composite systems such as maltodextrin, gum arabic, modified starch, and whey protein. Encapsulation processes often employ spray drying and coagulation methods. However, existing technologies still have significant shortcomings. Summary of the Invention
[0004] This invention provides a method for preparing a high-temperature resistant baking milk flavor microcapsule. The milk flavor microcapsules prepared by the method described in this application have excellent high-temperature resistance and stability, and are suitable for high-temperature baking.
[0005] The present invention solves its technical problem by adopting the following technical solution: A method for preparing a high-temperature resistant baking milk flavoring via microcapsule encapsulation includes the following steps: (1) The milk flavoring, ascorbate palmitate, sucrose fatty acid ester and pullulan polysaccharide are stirred evenly at 40~60℃ and 200~500rpm to obtain the first mixture; (2) Add modified chitosan, octenyl succinate starch and sodium caseinate to water, stir evenly at 200-500 rpm at 60-80℃, then add sodium tripolyphosphate, stir evenly at 200-500 rpm at 60-80℃ to obtain the second mixture. (3) Add the first mixture to the second mixture, stir evenly at 200-500 rpm at 40-60℃, homogenize, filter, and freeze dry under vacuum to obtain milk flavor microcapsules.
[0006] This application first mixes milk flavoring with ascorbyl palmitate, sucrose fatty acid ester, and pullulan, wherein sucrose fatty acid ester, pullulan, and ascorbyl palmitate prevent the flavoring from oxidizing and promote its compatibility with the aqueous wall material, forming a stable first mixture. Then, modified chitosan, octenyl succinate starch, and sodium caseinate are dissolved in water, and sodium tripolyphosphate is added to fully combine the wall material components, constructing a dense, high-temperature resistant wall material matrix, resulting in a second mixture. Finally, the first mixture is added to the second mixture to uniformly coat the flavoring droplets. After homogenization, the particles are further refined and the wall material is made denser. After filtering to remove impurities, vacuum freeze-drying is used to avoid flavoring volatilization and wall material damage, ultimately forming stable, high-temperature resistant milk flavoring microcapsules, achieving efficient encapsulation and high-temperature retention of the flavoring.
[0007] As a preferred embodiment of this application, the mass ratio of the milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan is 100:(8~12):(4~6):(2~5).
[0008] As a preferred embodiment of this application, the mass ratio of the modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate is (30~40):(20~30):(20~30):(800~2000):(0.5~2).
[0009] As a preferred embodiment of this application, the method for preparing the modified chitosan is as follows: Add fructooligosaccharides and trehalose to water and stir until well mixed to obtain the first mixture; Chitosan was added to an aqueous solution of citric acid and swollen at 40-60°C for 40-80 minutes. Then, the first mixture and silk fibroin were added, stirred evenly, ultrasonically treated, filtered, and dried to obtain modified chitosan.
[0010] As a preferred embodiment of this application, the mass ratio of the oligofructose, trehalose, and water is 1:(0.8~1.5):(4~10).
[0011] In a preferred embodiment of this application, the mass ratio of chitosan, citric acid aqueous solution, first mixture, and silk fibroin is 1:(8~12):(0.8~1.5):(0.3~0.5).
[0012] In a preferred embodiment of this application, the ultrasonic treatment power is 400~800W and the time is 20~60min.
[0013] In a preferred embodiment of this application, the citric acid aqueous solution contains 4-10% citric acid aqueous solution by mass.
[0014] As a preferred embodiment of this application, the mass ratio of the first mixture to the second mixture is 1:(2~5).
[0015] As a preferred embodiment of this application, the vacuum freeze drying specifically involves: first drying at a vacuum of 35~40 Pa and a temperature of -12~-9℃ for 0.5~2 hours; then drying at a vacuum of 50~55 Pa and a temperature of -8~-5℃ for 0.5~2 hours; then drying at a vacuum of 10~15 Pa and a temperature of -2~2℃ for 0.5~2 hours; and finally drying at a vacuum of 6~12 Pa and a temperature of 18~22℃ for 0.5~2 hours.
[0016] As a preferred embodiment of this application, the homogenization pressure is 28~32MPa, the temperature is 35~42℃, and the time is 8~20min.
[0017] As a preferred embodiment of this application, the milk flavoring comprises the following components in parts by weight: 8-15 parts of γ-nonanolactone, 6-12 parts of δ-decanolactone, 3-8 parts of ethyl vanillin, 2-5 parts of dimethyl butylene, 10-20 parts of whey powder, and 30-50 parts of edible vegetable oil.
[0018] As a preferred embodiment of this application, the edible vegetable oil includes olive oil and coconut oil in a mass ratio of 1:(0.2~0.6).
[0019] The beneficial effects of this invention are as follows: First, milk flavoring is mixed evenly with ascorbyl palmitate, sucrose fatty acid ester, and pullulan. Sucrose fatty acid ester, pullulan, and ascorbyl palmitate prevent the flavoring from oxidizing and promote its compatibility with the aqueous wall material, forming a stable first mixture. Then, modified chitosan, octenyl succinate starch, and sodium caseinate are dissolved in water, and sodium tripolyphosphate is added to fully combine the wall material components, constructing a dense, high-temperature resistant wall material matrix, resulting in a second mixture. Finally, the first mixture is added to the second mixture to uniformly coat the flavoring droplets. After homogenization, the particles are further refined and the wall material is made denser. After filtering to remove impurities, vacuum freeze-drying is used to avoid flavoring volatilization and wall material damage, ultimately forming stable, high-temperature resistant milk flavoring microcapsules, achieving efficient encapsulation and high-temperature retention of the flavoring. Detailed Implementation
[0020] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0021] In this invention, the technical features described in an open-ended manner include both closed-ended technical solutions composed of the listed features and open-ended technical solutions that include the listed features.
[0022] In this invention, numerical ranges are involved. Unless otherwise specified, the numerical ranges are considered continuous and include the minimum and maximum values of the range, as well as every value between the minimum and maximum values. Furthermore, when the range refers to integers, it includes every integer between the minimum and maximum values of the range. Additionally, when multiple ranges are provided to describe features or characteristics, the ranges may be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are included.
[0023] In this invention, there are no particular limitations on the specific dispersion and stirring methods.
[0024] Unless otherwise specified, all reagents or instruments used in this invention are commercially available conventional products. Unless otherwise specified, the raw materials used in each comparative example and the parallel experiments of each embodiment are the same commercially available products.
[0025] Example 1 A method for preparing a high-temperature resistant baking milk flavoring via microcapsule encapsulation includes the following steps: (1) Weigh the following raw materials according to the following mass proportions: 12 parts of γ-nonanolactone, 10 parts of δ-decanolactone, 5 parts of ethyl vanillin, 4 parts of dimethyl butylene, 14 parts of whey powder, and 45 parts of edible vegetable oil. The edible vegetable oil includes olive oil and coconut oil in a mass ratio of 1:0.5. Mix the raw materials evenly according to the proportions to obtain the milk flavoring. (2) Add fructooligosaccharides and trehalose to water and stir at 200 rpm for 20 min at 45°C to obtain the first mixture; the mass ratio of fructooligosaccharides, trehalose and water is 1:1:8.
[0026] Chitosan was added to a 5 wt% citric acid aqueous solution and swollen at 50°C for 50 min. Then, the first mixture and silk fibroin were added, and the mixture was stirred at 200 rpm for 60 min, followed by ultrasonic treatment at 500 W for 30 min. The mixture was then filtered and dried to obtain modified chitosan. The mass ratio of chitosan, citric acid aqueous solution, first mixture, and silk fibroin was 1:10:1:0.4.
[0027] (3) The milk flavoring, ascorbate palmitate, sucrose fatty acid ester and pullulan polysaccharide were mixed at 400 rpm for 30 min at 50 °C in a mass ratio of 100:8:6:5 to obtain the first mixture; (4) Add modified chitosan, octenyl succinate starch and sodium caseinate to water, stir at 40 rpm for 20 min at 70 °C, then add sodium tripolyphosphate, stir evenly at 400 rpm for 30 min at 70 °C to obtain the second mixture. The mass ratio of the modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate is 30:20:30:1000:0.5.
[0028] (5) The first mixture was added to the second mixture and stirred at 400 rpm for 60 min at 50 °C. The mixture was then added to a high-pressure homogenizer and homogenized at 30 MPa and 40 °C for 10 min. After filtration, the mixture was freeze-dried under vacuum to obtain milk flavor microcapsules. The mass ratio of the first mixture to the second mixture was 1:3.
[0029] The vacuum freeze drying process specifically involves: first drying at a vacuum of 38 Pa and a temperature of -10°C for 1 hour; then drying at a vacuum of 52 Pa and a temperature of -6°C for 1 hour; then drying at a vacuum of 12 Pa and a temperature of -0°C for 1 hour; and finally drying at a vacuum of 10 Pa and a temperature of 20°C for 1.5 hours.
[0030] Example 2 A method for preparing a high-temperature resistant baking milk flavoring via microcapsule encapsulation includes the following steps: (1) Weigh the following raw materials according to the following mass proportions: 12 parts of γ-nonanolactone, 10 parts of δ-decanolactone, 5 parts of ethyl vanillin, 4 parts of dimethyl butylene, 14 parts of whey powder, and 45 parts of edible vegetable oil. The edible vegetable oil includes olive oil and coconut oil in a mass ratio of 1:0.5. Mix the raw materials evenly according to the proportions to obtain the milk flavoring. (2) Add fructooligosaccharides and trehalose to water and stir at 200 rpm for 20 min at 45°C to obtain the first mixture; the mass ratio of fructooligosaccharides, trehalose and water is 1:1:8.
[0031] Chitosan was added to a 5 wt% citric acid aqueous solution and swollen at 50°C for 50 min. Then, the first mixture and silk fibroin were added, and the mixture was stirred at 200 rpm for 60 min, followed by ultrasonic treatment at 500 W for 30 min. The mixture was then filtered and dried to obtain modified chitosan. The mass ratio of chitosan, citric acid aqueous solution, first mixture, and silk fibroin was 1:10:1:0.4.
[0032] (3) The milk flavoring, ascorbate palmitate, sucrose fatty acid ester and pullulan polysaccharide were stirred at 400 rpm for 30 min at 50 °C in a mass ratio of 100:12:4:2 to obtain the first mixture; (4) Add modified chitosan, octenyl succinate starch and sodium caseinate to water, stir at 40 rpm for 20 min at 70 °C, then add sodium tripolyphosphate, stir evenly at 400 rpm for 30 min at 70 °C to obtain the second mixture. The mass ratio of the modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate is 30:20:30:1000:0.5.
[0033] (5) The first mixture was added to the second mixture and stirred at 400 rpm for 60 min at 50 °C. The mixture was then added to a high-pressure homogenizer and homogenized at 30 MPa and 40 °C for 10 min. After filtration, the mixture was freeze-dried under vacuum to obtain milk flavor microcapsules. The mass ratio of the first mixture to the second mixture was 1:3.
[0034] The vacuum freeze drying process specifically involves: first drying at a vacuum of 38 Pa and a temperature of -10°C for 1 hour; then drying at a vacuum of 52 Pa and a temperature of -6°C for 1 hour; then drying at a vacuum of 12 Pa and a temperature of -0°C for 1 hour; and finally drying at a vacuum of 10 Pa and a temperature of 20°C for 1.5 hours.
[0035] Example 3 A method for preparing a high-temperature resistant baking milk flavoring via microcapsule encapsulation includes the following steps: (1) Weigh the following raw materials according to the following mass proportions: 12 parts of γ-nonanolactone, 10 parts of δ-decanolactone, 5 parts of ethyl vanillin, 4 parts of dimethyl butylene, 14 parts of whey powder, and 45 parts of edible vegetable oil. The edible vegetable oil includes olive oil and coconut oil in a mass ratio of 1:0.5. Mix the raw materials evenly according to the proportions to obtain the milk flavoring. (2) Add fructooligosaccharides and trehalose to water and stir at 200 rpm for 20 min at 45°C to obtain the first mixture; the mass ratio of fructooligosaccharides, trehalose and water is 1:1:8.
[0036] Chitosan was added to a 5 wt% citric acid aqueous solution and swollen at 50°C for 50 min. Then, the first mixture and silk fibroin were added, and the mixture was stirred at 200 rpm for 60 min, followed by ultrasonic treatment at 500 W for 30 min. The mixture was then filtered and dried to obtain modified chitosan. The mass ratio of chitosan, citric acid aqueous solution, first mixture, and silk fibroin was 1:10:1:0.4.
[0037] (3) The milk flavoring, ascorbate palmitate, sucrose fatty acid ester and pullulan polysaccharide were mixed at 400 rpm for 30 min at 50 °C in a mass ratio of 100:8:6:5 to obtain the first mixture; (4) Add modified chitosan, octenyl succinate starch and sodium caseinate to water, stir at 40 rpm for 20 min at 70 °C, then add sodium tripolyphosphate, stir evenly at 400 rpm for 30 min at 70 °C to obtain the second mixture. The mass ratio of the modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate is 40:30:20:1000:2.
[0038] (5) The first mixture was added to the second mixture and stirred at 400 rpm for 60 min at 50 °C. The mixture was then added to a high-pressure homogenizer and homogenized at 30 MPa and 40 °C for 10 min. After filtration, the mixture was freeze-dried under vacuum to obtain milk flavor microcapsules. The mass ratio of the first mixture to the second mixture was 1:3.
[0039] The vacuum freeze drying process specifically involves: first drying at a vacuum of 38 Pa and a temperature of -10°C for 1 hour; then drying at a vacuum of 52 Pa and a temperature of -6°C for 1 hour; then drying at a vacuum of 12 Pa and a temperature of -0°C for 1 hour; and finally drying at a vacuum of 10 Pa and a temperature of 20°C for 1.5 hours.
[0040] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 uses an equal amount of chitosan to replace the modified chitosan, while everything else is the same.
[0041] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the preparation method of the modified chitosan in Comparative Example 2 is different from that in Example 1, but all other aspects are the same.
[0042] The preparation method of the modified chitosan in this comparative example is as follows: Chitosan was added to a 5 wt% citric acid aqueous solution, swollen at 50°C for 50 min, stirred at 200 rpm for 60 min, and ultrasonically treated at 500 W for 30 min. The mixture was then filtered and dried to obtain modified chitosan. The mass ratio of chitosan to citric acid aqueous solution was 1:10.
[0043] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the mass ratios of milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan are different, while all other components are the same.
[0044] The mass ratio of milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan in this comparative example is 100:5:10:1.
[0045] Comparative Example 4 The difference between Comparative Example 4 and Example 1 is that the mass ratios of milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan are different, while all other components are the same.
[0046] The mass ratio of milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan in this comparative example is 100:20:2:10.
[0047] Comparative Example 5 The difference between Comparative Example 5 and Example 1 is that the mass ratios of modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate are different, while all other ratios are the same.
[0048] The mass ratio of modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate in this comparative example is 20:50:10:1000:0.2.
[0049] Comparative Example 6 The difference between Comparative Example 6 and Example 1 is that the mass ratios of modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate are different, while all other ratios are the same.
[0050] The mass ratio of modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate in this comparative example is 50:5:50:1000:5.
[0051] Test case 1. Preheat the electric oven to the set temperature (200℃). Experiment with each temperature gradient separately. After the temperature stabilizes (keep warm for 10 minutes) before placing the samples in. Place each group of samples in the electric oven and set the baking time to 15 minutes. Keep the oven sealed during the baking process to avoid temperature fluctuations. After baking, remove the samples and place them in a sterile operating table to cool naturally to room temperature.
[0052] Core material leakage detection: Take 0.1g of cooled sample, add 10mL of anhydrous ethanol, ultrasonically extract for 10min (200W), centrifuge at 10000r / min and 4℃ for 10min, take the supernatant, and use HPLC to detect the peak areas of γ-nonanolactone and δ-decanolactone before and after the electric oven treatment.
[0053] High-temperature retention rate = (sum of peak areas of γ-nonanolactone and δ-decanolactone after oven treatment / sum of peak areas of γ-nonanolactone and δ-decanolactone before oven treatment) 100%.
[0054] 2. Weigh the ingredients according to the following proportions: 100g high-gluten flour, 20g white sugar, 30g butter, 20g egg, 10g deionized water, and 0.3g milk flavor microcapsules.
[0055] Mix all baking ingredients evenly and knead into a smooth dough. Let it rest and rise for 20 minutes (25℃). Roll out the dough to a thickness of 0.3cm and cut it into uniform sizes (2cm×2cm). Place the dough on a baking tray. Preheat the electric oven to the set temperature (200℃). Place three samples in each temperature gradient simultaneously and bake for 15 minutes (the standard baking time for cookies). After the temperature stabilizes, place the samples in the oven. After baking, remove the samples and let them cool naturally to room temperature to obtain the finished baked product. Take 10g of each batch of baked product, grind it to 100 mesh, place it in a 50mL sterile centrifuge tube, add 20mL of ethyl acetate, seal and ultrasonically extract for 20min (250W), centrifuge at 10000r / min and 4℃ for 15min, take the supernatant, filter it through a 0.22μm filter membrane to obtain the flavor test solution; the content of γ-nonanolactone and δ-decanolactone in the flavor test solution is detected by HPLC. Flavor retention rate = (Component content after baking / Component content before baking) × 100%.
[0056] Table 1
[0057] As can be seen from Table 1, the milk flavor microcapsules prepared by the method described in this application have excellent high temperature resistance and excellent stability, making them suitable for high temperature baking.
[0058] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. A method for preparing a high-temperature resistant baking milk flavoring by microencapsulation, characterized in that, Includes the following steps: (1) Mix the milk flavoring, ascorbate palmitate, sucrose fatty acid ester and pullulan polysaccharide evenly to obtain the first mixture; (2) Add modified chitosan, octenyl succinate starch and sodium caseinate to water, stir evenly, then add sodium tripolyphosphate and stir evenly to obtain the second mixture; (3) Add the first mixture to the second mixture, stir evenly, homogenize, filter, and freeze dry under vacuum to obtain milk flavor microcapsules.
2. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 1, characterized in that, The mass ratio of the milk flavoring, ascorbate palmitate, sucrose fatty acid ester, and pullulan is 100:(8~12):(4~6):(2~5).
3. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 1, characterized in that, The mass ratio of the modified chitosan, octenyl succinate starch, sodium caseinate, water, and sodium tripolyphosphate is (30~40):(20~30):(20~30):(800~2000):(0.5~2).
4. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 1, characterized in that, The modified chitosan is prepared by: Add fructooligosaccharides and trehalose to water and stir until well mixed to obtain the first mixture; Chitosan was added to an aqueous solution of citric acid and swollen at 40-60°C for 40-80 minutes. Then, the first mixture and silk fibroin were added, stirred evenly, ultrasonically treated, filtered, and dried to obtain modified chitosan.
5. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The mass ratio of the oligofructose, trehalose, and water is 1:(0.8~1.5):(4~10).
6. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The mass ratio of chitosan, citric acid aqueous solution, first mixture, and silk fibroin is 1:(8~12):(0.8~1.5):(0.3~0.5).
7. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The ultrasonic treatment has a power of 400~800W and a duration of 20~60min.
8. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The citric acid aqueous solution contains 4-10% citric acid by mass.
9. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The mass ratio of the first mixture to the second mixture is 1:(2~5).
10. The method for preparing high-temperature resistant baking milk flavoring via microcapsule encapsulation according to claim 4, characterized in that, The vacuum freeze drying process specifically involves: first drying at a vacuum of 35-40 Pa and a temperature of -12--9℃ for 0.5-2 hours; then drying at a vacuum of 50-55 Pa and a temperature of -8--5℃ for 0.5-2 hours; then drying at a vacuum of 10-15 Pa and a temperature of -2-2℃ for 0.5-2 hours; and finally drying at a vacuum of 6-12 Pa and a temperature of 18-22℃ for 0.5-2 hours.