Microcapsule perfume and method for preparing the same
By using a specific ratio of composite gum arabic and composite gelatin as wall materials, microcapsule flavors were prepared, solving the problems of low encapsulation rate, high cost, and poor stability in existing microcapsule flavors. This achieved efficient encapsulation and long-lasting stability of flavors, making it suitable for food, daily chemical, and textile industries.
Patent Information
- Application Number
- CN202510019390.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-07
- Publication Date
- 2025-10-21
- Estimated Expiration
- 2045-01-07
AI Technical Summary
Existing microcapsule flavor preparation processes suffer from low encapsulation rates, high costs, complex processes, and difficulty in large-scale promotion. They cannot effectively address the risk of flavor loss due to volatilization during storage, processing, and use. Furthermore, traditional flavors exhibit poor stability under high temperature and high pressure conditions, affecting product quality consistency and long-lasting fragrance effects.
Using a specific ratio of composite gum arabic and composite gelatin as wall materials, combined with essential oils, fragrances, emulsifiers and additives, microcapsule fragrances are prepared by spray drying to form a stable microcapsule structure, ensuring the stability and durability of the fragrances during storage, processing and use.
It achieves high encapsulation efficiency of microencapsulated flavors, reduces production costs, simplifies preparation processes, improves the thermal stability and antioxidant properties of flavors, ensures the long-lasting stability of aroma and reasonable particle size distribution, and is suitable for a variety of product fields.
Smart Images

Figure BDA0005230857170000203 
Figure BDA0005230857170000211 
Figure BDA0005230857170000212
Abstract
Description
Technical Field
[0001] The present invention relates to the field of essence preparation, in particular to a microcapsule essence and a preparation method thereof. Background Art
[0002] In the diverse landscape of the contemporary consumer market, fragrances, as functional additives that impart unique olfactory characteristics to products, play an indispensable and crucial role in a wide range of sectors, including food, daily chemicals, and textiles. In the food industry, precisely blended fragrances enable products like baked goods, confectionery, beverages, and dairy products to present a rich, diverse, and enticing flavor profile, catering to consumers' increasingly refined taste preferences and ultimately giving products a significant advantage in the fiercely competitive market. In the daily chemicals industry, fragrances are a core component of products like shampoo, shower gel, skincare, and even perfume. They not only create a unique sensory impression but also stimulate a pleasant olfactory experience during consumer use, becoming a key driver of product appeal to target audiences. In the textile industry, textiles treated with fragrances, such as clothing and bedding, can continuously release a pleasant aroma during daily use, effectively enhancing the comfort and sense of well-being of the living environment.
[0003] However, traditional flavors have demonstrated a series of inherent drawbacks in their practical application, severely restricting their effectiveness and industry expansion. Their primary shortcoming is their limited performance. During product storage, even in the relatively static environment of sealed packaging, driven by the flavor's inherent physical and chemical properties, molecular evaporation becomes increasingly pronounced over time. This results in a sharp decrease in aroma intensity and compromised flavor integrity by the time the product reaches the end consumer. For example, the initial addition of high-quality flavors is intended to provide consumers with a rich and mellow taste experience. However, the volatilization process during storage results in a far lower aroma intensity after opening than expected, significantly undermining the product's quality image and weakening the brand's competitiveness.
[0004] Entering the processing stage, traditional flavors face even more stringent challenges. Food processing involves complex processes such as high-temperature steaming, high-pressure treatment, and vigorous stirring. The preparation of daily chemical products involves delicate steps such as mixing multiple chemical ingredients and temperature-controlled heating. The printing, dyeing, and finishing of textile products are also accompanied by complex and dynamic physical and chemical conditions. Under such conditions, the high volatility of traditional flavors not only induces significant flavor loss and increases production costs, but also leads to increased dispersion of aroma content in the final product, making it difficult to maintain aroma consistency between different batches, posing a serious threat to product quality stability.
[0005] Furthermore, the stability defects of traditional fragrances during the use phase cannot be ignored. Taking daily chemical products as a typical example, after shampoo or shower gel is opened and used frequently in daily life, the product comes into contact with air over a large area, which accelerates the volatilization process of the fragrance, resulting in a significant reduction in the fragrance in the early and later stages of product use. After textile products have undergone multiple washing and drying cycles, the durability of the fragrance of the fragrance has declined sharply, making it difficult to maintain the pleasant fragrance atmosphere initially set for a long time, and unable to continuously meet consumers' demand for a long-lasting fragrance experience.
[0006] The innovative emergence of microencapsulation technology has opened up a new path to resolving the challenges facing traditional fragrances. Leveraging the principles of fine chemistry, this technology encapsulates fragrance molecules within tiny capsules, creating a barrier-like protective layer that effectively shields the core fragrance components from erosion and interference from external environmental factors. This allows for precise control of the fragrance's release process. While the product is in storage, the microcapsules act as a physical barrier to prevent fragrance volatilization, ensuring the product's aroma maintains a steady state. During processing, the microcapsule structure exhibits excellent tolerance, withstanding temperature ranges, pressure thresholds, and chemical fluctuations, minimizing the risk of fragrance loss. During use, as the product interacts with the external environment, such as friction, humidity gradients, and other stimuli, the microcapsules slowly and continuously release the fragrance according to a pre-set mechanism, ensuring a long-lasting fragrance effect.
[0007] Despite the significant theoretical advantages of microencapsulation technology, existing microencapsulated fragrance preparation processes currently suffer from numerous shortcomings. For one thing, most existing preparation processes exhibit suboptimal encapsulation efficiency, resulting in a significant number of fragrance ingredients failing to be effectively encapsulated during the preparation process. This results in a high risk of volatilization and loss during subsequent storage, processing, and use, hindering the full potential of microencapsulation technology. Furthermore, some preparation processes are overly complex, involving complex operating procedures, high-cost specialized equipment, and stringent reaction conditions. This not only significantly increases production costs but also places extremely high demands on the cleanliness of the production environment and the professional skills of operators, becoming a key obstacle to large-scale industrialization and popularization. Furthermore, some preparation methods utilize costly raw materials and limited supply channels, further compressing the market potential for microencapsulated fragrances.
[0008] In summary, the existing microcapsule flavor preparation technology system is difficult to meet the current market's strong demand for high-performance, low-cost, and easy-to-promote microcapsule flavor products.
[0009] Therefore, according to the above-mentioned related technologies, it is urgent to develop a microcapsule flavor and a preparation method thereof. Summary of the Invention
[0010] In view of this, the purpose of the present invention is to provide a microcapsule flavor and a preparation method thereof to meet the current market demand for high-performance, low-cost, and easy-to-promote microcapsule flavor products.
[0011] Based on the above objectives, the present invention provides a microcapsule flavor and a preparation method thereof.
[0012] A microcapsule essence is prepared from the following raw materials in parts by weight:
[0013] 30-50 parts of essential oil, 20-30 parts of spices, 15-25 parts of wall materials, 5-10 parts of emulsifier, 3-5 parts of auxiliary agents;
[0014] The essential oil is any one of lavender oil, rose essential oil, and lemon essential oil, and has the characteristics of being natural and having a pure aroma;
[0015] The spice is prepared from musk spice, sandalwood spice and gelatin;
[0016] The wall material is obtained by mixing compound gum arabic and compound gelatin in a mass ratio of 70-75:20-25;
[0017] The composite gum arabic is obtained by mixing gum arabic and modified gum arabic;
[0018] The mass ratio of gum arabic to modified gum arabic in the composite gum arabic is 68-71:2-4;
[0019] The composite gelatin is obtained by mixing gelatin and modified gelatin;
[0020] The mass ratio of gelatin to modified gelatin in the composite gelatin is 18-22:2-3;
[0021] The modified gum arabic is rose essential oil modified gum arabic;
[0022] The modified gelatin is rose essential oil modified gelatin;
[0023] The emulsifier is a nonionic emulsifier, and the nonionic emulsifier is any one of Tween-20, Tween-40, Tween-60, Tween-80, Span-20, Span-40 and Span-60.
[0024] The auxiliary agent is any one of vitamin C and vitamin E, which can prevent the oxidation and deterioration of flavors and spices and extend the shelf life of the microcapsule flavor.
[0025] The preparation process of the spices is as follows:
[0026] Gelatin is added to deionized water, stirred at 50-55°C and 200-300 rpm for 45-50 minutes, glutaraldehyde is added, the pH is adjusted to 8-9 with sodium hydroxide solution, and then compound spices are added, stirred at 300-500 rpm for 10-20 minutes for preliminary mixing, the pH value of the system is adjusted to 5-7, and the mixture is reacted in a constant temperature water bath at 35-45°C for 2-4 hours. The solution is then placed in an ultrasonic cleaner and ultrasonicated at 200-300W for 10-20 minutes. Finally, the solution is centrifuged, the precipitate is washed with deionized water for 3-5 times, and then freeze-dried at -40--30°C and a vacuum degree of 0.3-0.5 mbar for 18-24 hours to obtain the finished product.
[0027] Preferably, the usage ratio of the gelatin, deionized water, glutaraldehyde and compound spices is 5-8 g: 60-80 mL: 0.05-0.055 g: 0.05-0.08 g.
[0028] Preferably, the compound fragrance is obtained by mixing musk fragrance and sandalwood fragrance in a mass ratio of 20-25:40-45.
[0029] Preferably, the preparation process of the modified gum arabic is as follows:
[0030] Place gum arabic in a three-necked flask, slowly add distilled water, stir at 250-280 rpm for 45-50 min, add genipin, stir at 320-350 rpm for 6-9 min, adjust the system to a pH of 8-9 with anhydrous sodium carbonate, add rose essential oil, stir at 250-280 rpm for 10-15 min, react at 50-54° C. for 4-5 h, and finally centrifuge at 9000-10000 rpm for 15-18 min to obtain modified gum arabic.
[0031] Preferably, the usage ratio of gum arabic, distilled water, genipin and rose essential oil is 10-14 g:100-120 mL:0.05-0.07 g:4-5 g.
[0032] Preferably, the preparation process of the modified gelatin is as follows:
[0033] Place gelatin in a three-necked flask, add deionized water, stir at 48-53°C and 200-210 rpm for 30-40 minutes, add glutaraldehyde, stir at 300-320 rpm for 6-8 minutes, adjust the pH of the system to 8-9 with sodium hydroxide solution, add rose essential oil, react at 220-250 rpm and 45-48°C for 4-5 hours, and finally centrifuge at 4°C and 13000-15000 rpm for 12-15 minutes to obtain modified gelatin.
[0034] Preferably, the usage ratio of gelatin, deionized water, glutaraldehyde and rose essential oil is 8-10 g:80-90 mL:0.064-0.068 g:3-3.3 g.
[0035] A method for preparing a microcapsule essence comprises the following steps:
[0036] Step S1. Preparation of a mixed oil phase: Mix the essential oil and the fragrance, place them on a magnetic stirrer, and stir at a speed of 200-300 rpm for 10-15 minutes to ensure that the two are fully mixed to form a uniform mixed oil phase;
[0037] Step S2. Preparation of wall material solution: Mix the prepared wall material and deionized water, raise the temperature to 50-70°C, and stir with a magnetic stirrer at 200-300 rpm until the wall material is completely dissolved to obtain a clear, uniform wall material solution;
[0038] Step S3. Preparation of emulsified wall material solution: adding an emulsifier to the wall material solution, maintaining the magnetic stirrer speed at 200-300 rpm, stirring for 7-10 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0039] Step S4. Emulsion formation: under continuous stirring at 200-300 rpm, the mixed oil phase is added dropwise to the emulsified wall material solution. The addition is completed within 11-15 minutes to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion;
[0040] Step S5. Adding additives and stirring: Add the additives to the emulsion and continue stirring at a speed of 200-300 rpm for 30-40 min to allow the additives to fully dissolve and evenly distribute to obtain a final emulsion;
[0041] Step S6. Spray drying: Set the air inlet temperature to 180-200°C and the air outlet temperature to 80-100°C, adjust the spray pressure to 0.2-0.4 MPa, transport the emulsion to the atomizer via a peristaltic pump, and spray it into the drying tower. The hot air quickly evaporates the moisture, drying the emulsion to obtain the microencapsulated essence.
[0042] Preferably, the ratio of the wall material to deionized water in step S2 is 15-25 g: 150-200 mL.
[0043] Beneficial effects of the present invention:
[0044] The present invention provides a microcapsule flavor and a preparation method thereof. The present invention modifies the flavor with gelatin and then passes a wall material obtained by compounding composite gum arabic and composite gelatin in a specific ratio through the outer layer. The finally obtained microcapsule flavor has a long-lasting and stable aroma, a reasonable particle size distribution, good thermal stability, and strong antioxidant properties. In addition, the raw materials involved are common, the process is simple, the cost is low, and it is easy to promote, so it has broad application prospects. DETAILED DESCRIPTION
[0045] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to specific embodiments.
[0046] Example 1: A method for preparing a microcapsule flavor, comprising the following steps:
[0047] S1. Mix 20g of musk spices and 40g of sandalwood spices to obtain a composite spice;
[0048] S2. 5 g of gelatin was added to 60 mL of deionized water and stirred at 200 rpm for 45 min at 50°C. 0.05 g of glutaraldehyde was added and the pH was adjusted to 8 with sodium hydroxide solution. 0.05 g of the compound fragrance was then added and stirred at 300 rpm for 10 min for preliminary mixing. The pH of the system was adjusted to 5 and the mixture was reacted in a 35°C water bath for 2 h. The solution was then placed in an ultrasonic cleaner and sonicated at 200 W for 10 min. The solution was then centrifuged and the precipitate was washed three times with deionized water. The mixture was then freeze-dried at -40°C and a vacuum of 0.3 mbar for 18 h to obtain the fragrance.
[0049] S3. 10 g of gum arabic was placed in a three-necked flask, 100 mL of distilled water was slowly added, and the mixture was stirred at 250 rpm for 45 min. 0.05 g of genipin was added, and the mixture was stirred at 320 rpm for 6 min. The pH of the mixture was adjusted to 8 with anhydrous sodium carbonate. 4 g of rose essential oil was added, and the mixture was stirred at 250 rpm for 10 min. The mixture was reacted at 50°C for 4 h, and finally centrifuged at 9000 rpm for 15 min to obtain modified gum arabic.
[0050] S4. 8 g of gelatin was placed in a three-necked flask, 80 mL of deionized water was added, and the mixture was stirred at 48°C and 200 rpm for 30 min. 0.064 g of glutaraldehyde was added and stirred at 300 rpm for 6 min. The pH of the mixture was adjusted to 8 with sodium hydroxide solution. 3 g of rose essential oil was added and the mixture was reacted at 220 rpm and 45°C for 4 h. Finally, the mixture was centrifuged at 4°C and 13,000 rpm for 12 min to obtain modified gelatin.
[0051] S5. 68 g of gum arabic and 2 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0052] S6. 18 g of gelatin and 2 g of modified gelatin were mixed to obtain composite gelatin;
[0053] S7. 70 g of compound gum arabic and 20 g of compound gelatin were mixed to obtain a wall material;
[0054] S8. Preparation of mixed oil phase: 30 g of lavender oil was mixed with 20 g of spices, placed on a magnetic stirrer, and stirred at 200 rpm for 10 min to ensure that the two were thoroughly mixed to form a uniform mixed oil phase;
[0055] S9. Wall material solution preparation: Mix 15 g of the prepared wall material with 150 mL of deionized water, raise the temperature to 50°C, and stir at 200 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, uniform wall material solution.
[0056] S10. Preparation of emulsified wall material solution: 5 g of Tween-20 was added to the wall material solution, the magnetic stirrer speed was maintained at 200 rpm, and stirred for 7 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0057] S11. Emulsion formation: Under continuous stirring at 200 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution over a period of 11 minutes to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion.
[0058] S12 additive addition and stirring: 3g of vitamin C was added to the emulsion and stirred at 200 rpm for 30 min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0059] S13. Spray drying: Set the air inlet temperature to 180°C and the air outlet temperature to 80°C, adjust the spray pressure to 0.2 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated flavor.
[0060] Example 2: A method for preparing a microcapsule flavor, comprising the following steps:
[0061] S1. Mix 21g of musk spices and 41g of sandalwood spices to obtain a composite spice;
[0062] S2. 6 g of gelatin was added to 64 mL of deionized water and stirred at 220 rpm for 46 min at 51 ° C. 0.051 g of glutaraldehyde was added and the pH was adjusted to 8.5 with sodium hydroxide solution. 0.06 g of the compound flavor was added and initially mixed by stirring at 340 rpm for 12 min. The pH value of the system was adjusted to 5.5 and reacted in a constant temperature water bath at 37 ° C for 3 h. The solution was then placed in an ultrasonic cleaner and sonicated at 220 W for 12 min. Finally, the solution was centrifuged and the precipitate was washed four times with deionized water. The precipitate was then freeze-dried at -38 ° C and a vacuum of 0.4 mbar for 19 h to obtain the flavor.
[0063] S3. 11 g of gum arabic was placed in a three-necked flask, 104 mL of distilled water was slowly added, and the mixture was stirred at 256 rpm for 46 min. 0.054 g of genipin was added, and the mixture was stirred at 326 rpm for 7 min. The pH of the mixture was adjusted to 8.5 with anhydrous sodium carbonate. 4.2 g of rose essential oil was added, and the mixture was stirred at 256 rpm for 11 min. The mixture was reacted at 51°C for 4.5 h, and finally centrifuged at 9200 rpm for 16 min to obtain modified gum arabic.
[0064] S4. 8.4 g of gelatin was placed in a three-necked flask, and 82 mL of deionized water was added. The mixture was stirred at 49°C and 202 rpm for 32 min. 0.065 g of glutaraldehyde was added, and the mixture was stirred at 305 rpm for 7 min. The pH of the mixture was adjusted to 8.5 with sodium hydroxide solution. 3.1 g of rose essential oil was added, and the mixture was reacted at 226 rpm and 46°C for 4.5 h. Finally, the mixture was centrifuged at 4°C and 13,400 rpm for 13 min to obtain the modified gelatin.
[0065] S5. 69 g of gum arabic and 3 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0066] S6. 19 g of gelatin and 2.2 g of modified gelatin were mixed to obtain composite gelatin;
[0067] S7. 71g of compound gum arabic and 21g of compound gelatin were mixed to obtain a wall material;
[0068] S8. Preparation of mixed oil phase: 34 g of rose essential oil was mixed with 22 g of spices, placed on a magnetic stirrer, and stirred at 220 rpm for 11 min to ensure that the two were fully mixed to form a uniform mixed oil phase;
[0069] S9. Wall material solution preparation: Mix 17 g of the prepared wall material with 160 mL of deionized water, raise the temperature to 54°C, and stir at 220 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, homogeneous wall material solution.
[0070] S10. Preparation of emulsified wall material solution: 6 g of Tween-40 was added to the wall material solution, the magnetic stirrer speed was maintained at 220 rpm, and stirred for 8 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0071] S11. Emulsion formation: Under continuous stirring at 220 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution within 12 min to allow the oil phase to be evenly dispersed in the aqueous phase to form a stable emulsion;
[0072] S12 additive addition and stirring: 4g of vitamin E was added to the emulsion and stirred at 220rpm for 32min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0073] S13. Spray drying: Set the air inlet temperature to 185°C and the air outlet temperature to 84°C, adjust the spray pressure to 0.3 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated fragrance.
[0074] Example 3: A method for preparing a microcapsule flavor, comprising the following steps:
[0075] S1. Mix 22g of musk spices and 42g of sandalwood spices to obtain a composite spice;
[0076] S2. 6.5 g of gelatin was added to 68 mL of deionized water and stirred at 240 rpm for 47 min at 52°C. 0.052 g of glutaraldehyde was added and the pH was adjusted to 9 with sodium hydroxide solution. 0.07 g of the compound fragrance was then added and stirred at 380 rpm for 14 min for preliminary mixing. The pH of the system was adjusted to 6 and the mixture was reacted in a 39°C water bath for 4 h. The solution was then placed in an ultrasonic cleaner and sonicated at 240 W for 14 min. The solution was finally centrifuged and the precipitate was washed five times with deionized water. The mixture was then freeze-dried at -36°C and a vacuum of 0.5 mbar for 20 h to obtain the fragrance.
[0077] S3. 12 g of gum arabic was placed in a three-necked flask, 108 mL of distilled water was slowly added, and the mixture was stirred at 262 rpm for 47 min. 0.058 g of genipin was added, and the mixture was stirred at 332 rpm for 7 min. The pH of the mixture was adjusted to 9 with anhydrous sodium carbonate. 4.4 g of rose essential oil was added, and the mixture was stirred at 262 rpm for 12 min. The mixture was reacted at 52°C for 5 h, and finally centrifuged at 9400 rpm for 16 min to obtain modified gum arabic.
[0078] S4. 8.8 g of gelatin was placed in a three-necked flask, and 84 mL of deionized water was added. The mixture was stirred at 50°C and 204 rpm for 34 min. 0.066 g of glutaraldehyde was added, and the mixture was stirred at 310 rpm for 8 min. The pH of the mixture was adjusted to 9 with sodium hydroxide solution. 3.2 g of rose essential oil was added, and the mixture was reacted at 232 rpm and 47°C for 5 h. Finally, the mixture was centrifuged at 4°C and 13,800 rpm for 14 min to obtain the modified gelatin.
[0079] S5. 70 g of gum arabic and 4 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0080] S6. 20 g of gelatin and 2.4 g of modified gelatin were mixed to obtain composite gelatin;
[0081] S7. 72g of compound gum arabic and 22g of compound gelatin were mixed to obtain a wall material;
[0082] S8. Mixed oil phase preparation: 38g of lemon essential oil was mixed with 24g of spices, placed on a magnetic stirrer, and stirred at 240rpm for 12min to ensure that the two were thoroughly mixed to form a uniform mixed oil phase;
[0083] S9. Wall material solution preparation: Mix 19 g of the prepared wall material with 170 mL of deionized water, raise the temperature to 58°C, and stir at 240 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, homogeneous wall material solution.
[0084] S10. Preparation of emulsified wall material solution: 7 g of Tween-60 was added to the wall material solution, the magnetic stirrer speed was maintained at 240 rpm, and stirred for 9 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0085] S11. Emulsion formation: Under continuous stirring at 240 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution. The addition was completed within 13 min to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion.
[0086] S12 additive addition and stirring: 5g of vitamin C was added to the emulsion and stirred at 240 rpm for 34 min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0087] S13. Spray drying: Set the air inlet temperature to 190°C and the air outlet temperature to 88°C, adjust the spray pressure to 0.4 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated flavor.
[0088] Example 4: A method for preparing a microcapsule flavor, comprising the following steps:
[0089] S1. Mix 23g of musk fragrance and 43g of sandalwood fragrance to obtain a composite fragrance;
[0090] S2. 7 g of gelatin was added to 72 mL of deionized water and stirred at 260 rpm for 48 min at 53 ° C. 0.053 g of glutaraldehyde was added and the pH was adjusted to 8 with sodium hydroxide solution. 0.08 g of the compound fragrance was then added and stirred at 420 rpm for 16 min for preliminary mixing. The pH value of the system was adjusted to 6.5 and reacted in a constant temperature water bath at 41 ° C for 2 h. The solution was then placed in an ultrasonic cleaner and sonicated at 260 W for 16 min. Finally, the solution was centrifuged and the precipitate was washed three times with deionized water. The precipitate was then freeze-dried at -34 ° C and a vacuum of 0.3 mbar for 22 h to obtain the fragrance.
[0091] S3. 13 g of gum arabic was placed in a three-necked flask, 112 mL of distilled water was slowly added, and the mixture was stirred at 268 rpm for 48 min. 0.062 g of genipin was added, and the mixture was stirred at 338 rpm for 8 min. The pH of the mixture was adjusted to 8 with anhydrous sodium carbonate. 4.6 g of rose essential oil was added, and the mixture was stirred at 268 rpm for 13 min. The mixture was reacted at 53°C for 4 h, and finally centrifuged at 9600 rpm for 17 min to obtain modified gum arabic.
[0092] S4. 9.2 g of gelatin was placed in a three-necked flask, and 86 mL of deionized water was added. The mixture was stirred at 51°C and 206 rpm for 36 min. 0.067 g of glutaraldehyde was added, and the mixture was stirred at 315 rpm for 6 min. The pH of the mixture was adjusted to 8 with sodium hydroxide solution. 3.1 g of rose essential oil was added, and the mixture was reacted at 238 rpm and 46°C for 4 h. Finally, the mixture was centrifuged at 4°C and 14,200 rpm for 13 min to obtain modified gelatin.
[0093] S5. 69 g of gum arabic and 2 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0094] S6. 21 g of gelatin and 2.6 g of modified gelatin were mixed to obtain composite gelatin;
[0095] S7. 73g of compound gum arabic and 23g of compound gelatin were mixed to obtain a wall material;
[0096] S8. Preparation of mixed oil phase: 42 g of lavender oil was mixed with 26 g of spices, placed on a magnetic stirrer, and stirred at 260 rpm for 13 min to ensure that the two were thoroughly mixed to form a uniform mixed oil phase;
[0097] S9. Wall material solution preparation: Mix 21 g of the prepared wall material with 180 mL of deionized water, raise the temperature to 62°C, and stir at 260 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, homogeneous wall material solution.
[0098] S10. Preparation of emulsified wall material solution: 8 g of Span-20 was added to the wall material solution, the magnetic stirrer speed was maintained at 260 rpm, and stirred for 8 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0099] S11. Emulsion formation: Under continuous stirring at 260 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution. The addition was completed within 14 minutes to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion.
[0100] S12 additive addition and stirring: 3g of vitamin E was added to the emulsion and stirred at 260rpm for 36min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0101] S13. Spray drying: Set the air inlet temperature to 195°C and the air outlet temperature to 92°C, adjust the spray pressure to 0.2 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated flavor.
[0102] Example 5: A method for preparing a microcapsule flavor, comprising the following steps:
[0103] S1. Mix 24g of musk spices and 44g of sandalwood spices to obtain a composite spice;
[0104] S2. 7.5 g of gelatin was added to 76 mL of deionized water and stirred at 280 rpm for 49 min at 54 ° C. 0.054 g of glutaraldehyde was added and the pH was adjusted to 8.5 with sodium hydroxide solution. 0.075 g of the compound fragrance was added and initially mixed at 460 rpm for 18 min. The pH value of the system was adjusted to 6 and the mixture was reacted in a constant temperature water bath at 43 ° C for 3 h. The solution was then placed in an ultrasonic cleaner and ultrasonicated at 280 W for 18 min. Finally, the solution was centrifuged and the precipitate was washed four times with deionized water. The precipitate was then freeze-dried at -32 ° C and a vacuum of 0.4 mbar for 23 h to obtain the fragrance.
[0105] S3. 12 g of gum arabic was placed in a three-necked flask, 116 mL of distilled water was slowly added, and the mixture was stirred at 274 rpm for 49 min. 0.066 g of genipin was added, and the mixture was stirred at 344 rpm for 8 min. The pH of the mixture was adjusted to 8.5 with anhydrous sodium carbonate. 4.8 g of rose essential oil was added, and the mixture was stirred at 274 rpm for 14 min. The mixture was reacted at 52°C for 4.5 h, and finally centrifuged at 9800 rpm for 17 min to obtain modified gum arabic.
[0106] S4. 9.6 g of gelatin was placed in a three-necked flask, and 88 mL of deionized water was added. The mixture was stirred at 52°C and 208 rpm for 38 min. 0.065 g of glutaraldehyde was added, and the mixture was stirred at 320 rpm for 7 min. The pH of the mixture was adjusted to 8.5 with sodium hydroxide solution. 3 g of rose essential oil was added, and the mixture was reacted at 244 rpm and 47°C for 4.5 h. Finally, the mixture was centrifuged at 4°C and 14,600 rpm for 14 min to obtain the modified gelatin.
[0107] S5. 70 g of gum arabic and 3 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0108] S6. 19 g of gelatin and 2.8 g of modified gelatin were mixed to obtain composite gelatin;
[0109] S7. 74 g of compound gum arabic and 24 g of compound gelatin were mixed to obtain a wall material;
[0110] S8. Preparation of mixed oil phase: 46 g of rose essential oil was mixed with 28 g of spices, placed on a magnetic stirrer, and stirred at 280 rpm for 14 min to ensure that the two were thoroughly mixed to form a uniform mixed oil phase;
[0111] S9. Wall material solution preparation: Mix 23 g of the prepared wall material with 190 mL of deionized water, raise the temperature to 66°C, and stir at 280 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, homogeneous wall material solution.
[0112] S10. Preparation of emulsified wall material solution: 9 g of Span-40 was added to the wall material solution, the magnetic stirrer speed was maintained at 280 rpm, and stirred for 9 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0113] S11. Emulsion formation: Under continuous stirring at 280 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution within 12 min to allow the oil phase to be evenly dispersed in the aqueous phase to form a stable emulsion;
[0114] S12 additive addition and stirring: 4g of vitamin C was added to the emulsion and stirred at 280rpm for 38min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0115] S13. Spray drying: Set the air inlet temperature to 190°C and the air outlet temperature to 96°C, adjust the spray pressure to 0.3 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated flavor.
[0116] Example 6: A method for preparing a microcapsule flavor, comprising the following steps:
[0117] S1. Mix 25g of musk spices and 45g of sandalwood spices to obtain a composite spice;
[0118] S2. 8 g of gelatin was added to 80 mL of deionized water and stirred at 300 rpm for 50 min at 55 ° C. 0.055 g of glutaraldehyde was added and the pH was adjusted to 9 with sodium hydroxide solution. 0.08 g of the compound fragrance was then added and stirred at 500 rpm for 20 min for preliminary mixing. The pH value of the system was adjusted to 7 and the mixture was reacted in a constant temperature water bath at 45 ° C for 4 h. The solution was then placed in an ultrasonic cleaner and ultrasonicated at 300 W for 20 min. Finally, the solution was centrifuged and the precipitate was washed with deionized water five times. The precipitate was then freeze-dried at -30 ° C and a vacuum of 0.5 mbar for 24 h to obtain the fragrance.
[0119] S3. 14 g of gum arabic was placed in a three-necked flask, 120 mL of distilled water was slowly added, and the mixture was stirred at 280 rpm for 50 min. 0.07 g of genipin was added, and the mixture was stirred at 350 rpm for 9 min. The pH of the mixture was adjusted to 9 with anhydrous sodium carbonate. 5 g of rose essential oil was added, and the mixture was stirred at 280 rpm for 15 min. The mixture was reacted at 54°C for 5 h, and finally centrifuged at 10,000 rpm for 18 min to obtain modified gum arabic.
[0120] S4. 10 g of gelatin was placed in a three-necked flask, and 90 mL of deionized water was added. The mixture was stirred at 53°C and 210 rpm for 40 min. 0.068 g of glutaraldehyde was added, and the mixture was stirred at 320 rpm for 8 min. The pH of the mixture was adjusted to 9 with sodium hydroxide solution. 3.3 g of rose essential oil was added, and the mixture was reacted at 250 rpm and 48°C for 5 h. Finally, the mixture was centrifuged at 4°C and 15,000 rpm for 15 min to obtain the modified gelatin.
[0121] S5. 71 g of gum arabic and 4 g of modified gum arabic were mixed to obtain a composite gum arabic;
[0122] S6. 22 g of gelatin and 3 g of modified gelatin were mixed to obtain composite gelatin;
[0123] S7. 75g of compound gum arabic and 25g of compound gelatin were mixed to obtain a wall material;
[0124] S8. Preparation of mixed oil phase: 50 g of lemon essential oil was mixed with 30 g of spices, placed on a magnetic stirrer, and stirred at 300 rpm for 15 min to ensure that the two were thoroughly mixed to form a uniform mixed oil phase;
[0125] S9. Preparation of wall material solution: Mix 25 g of the prepared wall material with 200 mL of deionized water, raise the temperature to 70°C, and stir at 300 rpm using a magnetic stirrer until the wall material is completely dissolved to obtain a clear, uniform wall material solution.
[0126] S10. Preparation of emulsified wall material solution: 10 g of Span-60 was added to the wall material solution, the magnetic stirrer speed was maintained at 300 rpm, and stirred for 10 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution;
[0127] S11. Emulsion formation: Under continuous stirring at 300 rpm, the mixed oil phase was added dropwise to the emulsified wall material solution. The addition was completed within 15 min to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion.
[0128] S12 additive addition and stirring: 5g of vitamin E was added to the emulsion and stirred at 300rpm for 40min to allow the additive to fully dissolve and evenly distribute to obtain a final emulsion;
[0129] S13. Spray drying: Set the air inlet temperature to 200°C and the air outlet temperature to 100°C, adjust the spray pressure to 0.4 MPa, and transport the emulsion to the atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the final emulsion to obtain the microencapsulated flavor.
[0130] Comparative Example 1:
[0131] Compared with Example 1, this comparative example did not add "gelatin" during the preparation of the "flavor", and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, microcapsule flavor was obtained.
[0132] Comparative Example 2:
[0133] Compared with Example 1, this comparative example does not add "compound gelatin" during the preparation of the "wall material". The remaining steps and parameters are the same and will not be repeated in this comparative example. Finally, microcapsule flavor is obtained.
[0134] Comparative Example 3:
[0135] Compared with Example 1, this comparative example only replaces "modified gum arabic" with "gum arabic", and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, microcapsule flavor is obtained.
[0136] Comparative Example 4:
[0137] Compared with Example 1, this comparative example only replaces "modified gelatin" with "gelatin", and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, microcapsule flavor is obtained.
[0138] Comparative Example 5:
[0139] Compared with Example 1, this comparative example only adjusted the amount of "gum arabic" in the "compound gum arabic" from "68g" to "2g", and the amount of "modified gum arabic" in the "compound gum arabic" from "2g" to "68g". The remaining steps and parameters are the same, and will not be repeated in this comparative example. Finally, microcapsule flavor is obtained.
[0140] Comparative Example 6:
[0141] Compared with Example 1, this comparative example only adjusts the amount of "compound gum arabic" in the "wall material" from "70g" to "20g", and the amount of "compound gelatin" in the "wall material" from "20g" to "70g". The remaining steps and parameters are the same, and will not be repeated in this comparative example. Finally, microcapsule flavor is obtained.
[0142] Performance test: The following performance tests were performed on each group of microcapsule fragrance samples obtained in Examples 1 to 6 and Comparative Examples 1 to 6:
[0143] Aroma retention rate: Headspace solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) technology is used. Accurately weigh 0.5g of microencapsulated fragrance sample, place it in a sealed headspace bottle, and equilibrate it at 40°C for 30 minutes. Then, a solid phase microextraction fiber head is used to adsorb the volatile components in the headspace. The fiber head is then inserted into the gas chromatography inlet for chromatographic separation and mass spectrometry detection. The aroma retention rate is calculated by comparing the peak area of the main aroma components in the freshly prepared sample with those in the sample after 3 months and 6 months of storage. The formula is: After 3 months of storage, the aroma retention rate is ≥70% to be qualified; after 6 months of storage, the aroma retention rate is ≥50% to be qualified. The aroma retention rate of high-quality products should reach more than 60% after 6 months of storage;
[0144] Microcapsule Particle Size and Distribution: Using a laser particle size analyzer, the microcapsule flavor sample was dispersed in deionized water to form a uniform dispersion, which was then sonicated for 5 minutes to eliminate agglomerates. The dispersion was injected into the sample cell of the laser particle size analyzer. The instrument emitted a laser to illuminate the sample. By measuring the change in scattered light intensity with angle, the Mie scattering theory was used to calculate the microcapsule particle size and distribution. The volume average particle size (D[4,3]), number average particle size (D[3,2]), and particle size distribution range (D10, D50, and D90, representing the particle sizes corresponding to the cumulative volume distribution percentages of the sample reaching 10%, 50%, and 90%, respectively) were obtained. For most applications such as food and daily chemicals, a microcapsule volume average particle size (D[4,3]) of 1-100 μm is more suitable, with a D50 particle size range of 20-60 μm being more optimal. The particle size distribution span (D90-D10) should be as narrow as possible, generally required to be ≤50μm, to ensure the consistency and stability of product performance;
[0145] Thermal stability: A thermogravimetric analyzer (TGA) was used. 10 mg of microencapsulated flavor sample was placed in a ceramic crucible and heated from room temperature to 600°C at a heating rate of 10°C / min in a nitrogen atmosphere. The thermogravimetric analyzer monitors the change in sample mass with temperature in real time, and records the thermogravimetric curve (TG) and the first-order derivative thermogravimetric curve (DTG). The thermal stability of the microencapsulated flavor was evaluated by observing the temperature at which the sample began to lose weight significantly in the TG curve (initial decomposition temperature), the temperatures corresponding to key stages such as 5%, 10%, and 50% weight loss, and the peak temperature of the weight loss rate in the DTG curve. An initial decomposition temperature of ≥150°C is the basic requirement, which meets general processing and storage conditions. For some high-temperature processing or long-term exposure to high-temperature environments, an initial decomposition temperature of ≥200°C is more ideal. The temperature at 5% weight loss is ≥180°C, and the temperature at 10% weight loss is ≥220°C, which can be considered to have good thermal stability;
[0146] Antioxidant activity: Take the DPPH (1,1-diphenyl-2-picrylhydrazyl) free radical scavenging method as an example. Prepare a DPPH ethanol solution with a concentration of 0.1mmol / L, accurately weigh each group of microcapsule flavor samples, and dissolve them in ethanol to prepare a series of sample solutions with a concentration gradient (such as 0.1mg / mL, 0.2mg / mL, 0.5mg / mL, etc.). Take 2mL of DPPH solution and mix it with the sample solution, let it stand at room temperature in the dark for 30 minutes, and then measure the absorbance (A) of the mixed solution at a wavelength of 517nm. At the same time, measure the absorbance (A0) of the blank control group (containing only DPPH solution) and the background absorbance of the sample (A1, i.e., containing only sample solution). According to the formula: The free radical scavenging rate of samples at different concentrations was calculated, and the antioxidant capacity of the microencapsulated flavor was measured by the half inhibition concentration (IC50, i.e., the sample concentration corresponding to 50% of the free radical scavenging rate). The lower the IC50 value, the stronger the antioxidant activity. Taking the common antioxidant vitamin C as a reference, if the IC50 value of the microencapsulated flavor is lower than the IC50 value of vitamin C (about 0.06 mg / mL), it indicates that its antioxidant activity is strong; if the IC50 value is between 0.06-0.1 mg / mL, the antioxidant activity is moderate; if the IC50 value is greater than 0.1 mg / mL, the antioxidant activity is relatively weak.
[0147] The results are shown in Tables 1 to 4 below:
[0148] Table 1
[0149]
[0150]
[0151] Table 2
[0152] project D50 / μm Particle size distribution span (D90-D10) / μm Example 1 42 38 Example 2 48 42 Example 3 45 40 Example 4 50 45 Example 5 43 36 Example 6 52 48 Comparative Example 1 35 30 Comparative Example 2 60 55 Comparative Example 3 40 35 Comparative Example 4 46 40 Comparative Example 5 55 50 Comparative Example 6 65 60
[0153] Table 3
[0154]
[0155]
[0156] Table 4
[0157] project Temperature for 10% weight loss / ℃ DPPH free radical scavenging rate IC50 / mg / mL Example 1 230 0.052 Example 2 235 0.048 Example 3 225 0.055 Example 4 240 0.045 Example 5 232 0.050 Example 6 245 0.042 Comparative Example 1 195 0.080 Comparative Example 2 210 0.070 Comparative Example 3 215 0.065 Comparative Example 4 210 0.075 Comparative Example 5 200 0.085 Comparative Example 6 215 0.072
[0158] Data Analysis:
[0159] As can be seen from Tables 1 to 4, the microcapsule flavors prepared in Examples 1 to 6 are superior to those in Comparative Examples 1 to 6 in various performance indicators;
[0160] 1. Aroma retention rate: In Examples 1-6, the higher aroma retention rate is due to many factors. First, the addition of gelatin in the preparation process of spices plays a key role. Gelatin, as a macromolecular polymer, can form certain interactions with the volatile components in spices, such as hydrogen bonding, etc., wrapping the aroma molecules in its molecular network, slowing down the volatilization rate of the aroma. Secondly, the wall material adopts a combination of composite gum arabic and composite gelatin. This composite structure has good film-forming and barrier properties. Gum arabic itself has good hydrophilicity and can form a stable interaction with moisture, preventing external moisture from invading the interior of the microcapsule and causing hydrolysis of the aroma components; modified gum arabic and modified gelatin further optimize the performance of the wall material, and the rose essential oil modification enhances the compatibility between the wall material and the essential oil, forming a tighter wrapping structure, effectively blocking the aroma molecules from diffusing outward, thereby maintaining a high aroma retention rate after long-term storage. In addition, the rational selection and use of emulsifiers ensures the uniform mixing of the oil phase (containing essential oils and spices) and the aqueous phase (wall material solution), forming a stable emulsion and avoiding the premature release of aroma caused by local agglomeration. The antioxidant effect of the auxiliary agent vitamin C or vitamin E also indirectly protects the aroma components, preventing them from losing their aroma characteristics due to oxidation and deterioration. Comparative Example 1 does not add gelatin to prepare spices, so that the spices lack an effective binding structure inside, and the aroma molecules are more likely to volatilize and dissipate, resulting in a significant decrease in the aroma retention rate. The data after storage for 3 months and 6 months are significantly lower than those in the embodiment. For other cases of changing raw materials or processes in the comparative examples, such as changing the proportion of composite gum arabic in comparative example 5, the performance balance of the wall material as a whole is affected. When the ratio of gum arabic to modified gum arabic is out of balance, the barrier properties of the wall material are weakened, and it is impossible to effectively block the diffusion of aroma molecules, which reduces the aroma retention rate.
[0161] 2. Microcapsule particle size and distribution: In the preparation process of Examples 1-6, the parameters such as the amount of each raw material added, stirring speed, reaction temperature and time were finely controlled. These factors work together to determine the particle size and distribution of the microcapsules. During the wall material preparation stage, the dissolution, modification and mixing processes of gum arabic and gelatin are strictly carried out in accordance with specific conditions to ensure the uniformity and stability of the wall material. For example, when gum arabic is dissolved, the appropriate stirring speed (250-280rpm) and temperature (such as 50-54°C) are controlled to ensure that it is fully dispersed and does not degrade excessively. It is then mixed with modified gum arabic in a precise proportion to form a uniform composite gum arabic, which provides a good foundation for the wall material. Similarly, the preparation of composite gelatin is the same. The parameters of each step ensure that the gelatin is moderately modified and evenly mixed. During the emulsion formation process, by controlling the mixing speed of the oil phase and the emulsified wall material solution (e.g., complete dropwise addition within 10-15 minutes, stirring at 200-300 rpm), the oil droplets are evenly dispersed in the aqueous phase, preventing overly large or undersized droplets and agglomeration, thereby forming microcapsules with a relatively concentrated particle size distribution and appropriate size. A suitable particle size and narrow distribution span promote product stability in applications, such as uniform dispersion in daily chemical products, and prevent uneven particle size from affecting taste during food processing. Comparative Example 2, in which composite gelatin was not added to the wall material, compromised its structural integrity. A single-component wall material may not form a dense and uniform coating during film formation, making it difficult to control the particle size of the microcapsules during formation. This can lead to larger particle sizes (e.g., D[4,3] reaching 50 μm or even larger) and uneven distribution (D90-D10 reaching 55 μm or greater). This is because the lack of synergistic effects of the composite gelatin alters the rheological and cohesive properties of the wall material, making it unable to effectively constrain the growth and dispersion of the microcapsules. Similarly, in Comparative Example 6, the usage ratio of compound gum arabic and compound gelatin in the wall material is changed, which destroys the originally optimized balance of the wall material formula and also causes abnormalities in the particle size and distribution of microcapsules, affecting product quality and application performance.
[0162] 3. Thermal stability: The microcapsule flavors of Examples 1-6 have good thermal stability, which is mainly attributed to the unique wall material composition. The wall material constructed by composite gum arabic and composite gelatin can form a stable cross-linked network structure at high temperature. The carbohydrate groups in the gum arabic molecules and the amino acid residues in the gelatin molecules interact with each other during the heating process, enhancing the binding force between molecules. The rose essential oil modified part in the modified gum arabic and modified gelatin not only optimizes the compatibility with the aroma components, but also improves the thermal stability of the wall material to a certain extent. This may be because the chemical bonds or groups introduced by the modification change the thermal decomposition path of the wall material and increase key indicators such as the initial decomposition temperature. In addition, during the preparation process, such as the control of the reaction temperature (45-54°C) and time (4-5h) during the preparation of the wall material, the raw materials are fully reacted to form a more stable chemical structure, which further improves the overall thermal stability of the microcapsules, so that it can meet the thermal environment requirements under various processing and storage conditions. Comparative Example 3 only replaces "modified gum arabic" with "gum arabic", eliminating the structural optimization and thermal stability improvement effects brought about by the rose essential oil modification, making the wall material more susceptible to thermal decomposition at high temperatures. Because the intermolecular forces of ordinary gum arabic are relatively weak, the integrity of the wall material cannot be effectively maintained during the heating process, resulting in a decrease in the initial decomposition temperature (such as to 165°C), an early weight loss stage, and poor thermal stability. Comparative Example 5 changes the ratio of raw materials in the composite gum arabic, which also destroys the thermal stability structural foundation of the wall material. When the ratio of gum arabic to modified gum arabic is unreasonable, a stable cross-linking and mutual support structure cannot be formed at high temperatures, causing thermal stability indicators such as 5% and 10% weight loss temperatures to drop significantly, failing to reach the good levels described in the examples.
[0163] IV. Antioxidant Properties: The excellent antioxidant properties in Examples 1-6 are primarily due to the addition of vitamin C or vitamin E as additives. These, as effective antioxidants, can capture free radicals in the system, prevent free radical-induced oxidative chain reactions, and protect easily oxidized components such as unsaturated bonds in essential oils and spices. Furthermore, some components in the wall material, such as gelatin, may also have certain groups within their molecular structure that possess antioxidant activity, synergizing with the additives. Furthermore, during the rose essential oil-modified gum arabic and modified gelatin process, chemical bonds or groups with antioxidant capacity may have been introduced, further enhancing the overall antioxidant system of the microcapsules, resulting in a low DPPH free radical scavenging IC50 value and outstanding antioxidant performance. Comparative Example 1, in which gelatin was not added to prepare the spices, not only compromised aroma retention but also likely weakened the antioxidant system. The absence of gelatin deprived the spices of a potential antioxidant structural foundation, preventing them from effectively cooperating with the additives to resist oxidation. This resulted in an increased IC50 value (e.g., reaching 0.080 mg / mL) and a weakening of the antioxidant properties. In other comparative examples, the raw materials or processes were changed, such as comparative example 4 where only "modified gelatin" was replaced with "gelatin", which destroyed the original antioxidant synergistic effect of the wall material and fragrance system, reduced the free radical scavenging ability, and worsened the antioxidant performance.
[0164] In summary, Examples 1-6, through reasonable raw material formula design and precise preparation process control, have constructed a microcapsule fragrance system with excellent performance in many aspects such as aroma retention, particle size control, thermal stability and antioxidant properties. However, due to improper adjustment of key raw materials or processes in Comparative Examples 1-6, this synergistic balance was destroyed, resulting in varying degrees of deterioration of various performance indicators, which fully demonstrates the scientific nature and superiority of the microcapsule fragrance formula and preparation process of the present invention.
[0165] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Within the scope of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.
[0166] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A microcapsule flavor, characterized in that: Prepared from the following raw materials in parts by mass: 30-50 parts of essential oil, 20-30 parts of spices, 15-25 parts of wall materials, 5-10 parts of emulsifier, 3-5 parts of auxiliary agents; The essential oil is any one of lavender oil, rose essential oil, and lemon essential oil; The spice is prepared from musk spice, sandalwood spice and gelatin; The wall material is obtained by mixing compound gum arabic and compound gelatin in a mass ratio of 70-75:20-25; The composite gum arabic is obtained by mixing gum arabic and modified gum arabic; The modified gum arabic is rose essential oil modified gum arabic; The composite gelatin is obtained by mixing gelatin and modified gelatin; The modified gelatin is rose essential oil modified gelatin; The mass ratio of gum arabic to modified gum arabic in the composite gum arabic is 68-71:2-4; The mass ratio of gelatin to modified gelatin in the composite gelatin is 18-22:2-3; The preparation process of the spices is as follows: Add gelatin to deionized water, stir at 50-55°C and 200-300 rpm for 45-50 minutes, add glutaraldehyde, adjust the pH to 8-9 with sodium hydroxide solution, add compound spices, stir at 300-500 rpm for 10-20 minutes for preliminary mixing, adjust the pH value of the system to 5-7, react in a constant temperature water bath at 35-45°C for 2-4 hours, then place the solution in an ultrasonic cleaner and ultrasonicate at 200-300W for 10-20 minutes, finally centrifuge the solution, wash the precipitate with deionized water 3-5 times, and then freeze-dry at -40--30°C and a vacuum degree of 0.3-0.5 mbar for 18-24 hours to obtain the finished product; The usage ratio of gelatin, deionized water and compound spices is 5-8g:60-80mL:0.05-0.08g; The compound fragrance is obtained by mixing musk fragrance and sandalwood fragrance in a mass ratio of 20-25:40-45; The preparation process of the modified gum arabic is as follows: Place gum arabic in a three-necked flask, add distilled water, stir at 250-280 rpm for 45-50 minutes, add genipin, stir at 320-350 rpm for 6-9 minutes, adjust the pH value of the system to 8-9 with anhydrous sodium carbonate, add rose essential oil, stir at 250-280 rpm for 10-15 minutes, react at 50-54°C for 4-5 hours, and finally centrifuge at 9000-10000 rpm for 15-18 minutes to obtain modified gum arabic; The usage ratio of the gum arabic, distilled water, genipin and rose essential oil is 10-14 g:100-120 mL:0.05-0.07 g:4-5 g; The preparation process of the modified gelatin is as follows: Place gelatin in a three-necked flask, add deionized water, stir at 48-53°C and 200-210 rpm for 30-40 minutes, add glutaraldehyde, stir at 300-320 rpm for 6-8 minutes, adjust the pH of the system to 8-9 with sodium hydroxide solution, add rose essential oil, react at 220-250 rpm and 45-48°C for 4-5 hours, and finally centrifuge at 4°C and 13000-15000 rpm for 12-15 minutes to obtain modified gelatin; The usage ratio of the gelatin, deionized water, glutaraldehyde and rose essential oil is 8-10 g: 80-90 mL: 0.064-0.068 g: 3-3.3 g.
2. The microcapsule flavor according to claim 1, characterized in that The emulsifier is a non-ionic emulsifier, and the non-ionic emulsifier is any one of Tween-20, Tween-40, Tween-60, Tween-80, Span-20, Span-40 and Span-60; The auxiliary agent is any one of vitamin C and vitamin E.
3. The method for preparing the microcapsule flavor according to any one of claims 1 to 2, characterized in that: The following steps are involved: Step S1. Preparation of a mixed oil phase: Mix the essential oil and the fragrance, place them on a magnetic stirrer, and stir at a speed of 200-300 rpm for 10-15 minutes to ensure that the two are fully mixed to form a uniform mixed oil phase; Step S2. Preparation of wall material solution: Mix the prepared wall material and deionized water, raise the temperature to 50-70°C, and stir with a magnetic stirrer at 200-300 rpm until the wall material is completely dissolved to obtain a clear, uniform wall material solution; Step S3. Preparation of emulsified wall material solution: adding an emulsifier to the wall material solution, maintaining the magnetic stirrer speed at 200-300 rpm, stirring for 7-10 min to uniformly disperse the emulsifier in the wall material solution to form an emulsified wall material solution; Step S4. Emulsion formation: under continuous stirring at 200-300 rpm, the mixed oil phase is added dropwise to the emulsified wall material solution. The addition is completed within 11-15 minutes to uniformly disperse the oil phase in the aqueous phase to form a stable emulsion; Step S5. Adding additives and stirring: Add the additives to the emulsion and continue stirring at a speed of 200-300 rpm for 30-40 min to allow the additives to fully dissolve and evenly distribute to obtain a final emulsion; Step S6. Spray drying: Set the air inlet temperature to 180-200°C and the air outlet temperature to 80-100°C, adjust the spray pressure to 0.2-0.4 MPa, and deliver the emulsion to an atomizer via a peristaltic pump. Spray it into a drying tower. The hot air quickly evaporates the water, drying the emulsion to obtain the microencapsulated flavor. The usage ratio of the wall material and deionized water in step S2 is 15-25 g:150-200 mL.
Citation Information
Patent Citations
Preparation method of fragrance microcapsules for dispelling birds
CN106047482A