Microemulsion essence and preparation method thereof

Abstract

The invention relates to the technical field of daily chemical industry, and discloses a micro-emulsified essence and a preparation method thereof, the micro-emulsified essence comprises the following components by weight: 15-35% of an oily component, 8-22% of an emulsifier, 3-12% of a co-emulsifier, and the balance of deionized water; the oily component comprises at least two components selected from citrus essential oil, peppermint oil and rose absolute oil; the emulsifying agent is prepared by compounding polyoxyethylene sorbitan monooleate and polyoxyethylene lauryl ether according to the mass ratio of (3 to 1) to (5 to 1). The stability and aroma durability of the emulsion are remarkably improved through the synergistic effect of specific oily component compounding and an emulsifier, citrus essential oil, peppermint oil and rose absolute oil in the oily component are combined in proportion, the natural polarity difference forms a complementary effect, and the emulsifying agent compounded from polyoxyethylene sorbitan monooleate and lauryl alcohol polyoxyethylene ether is combined, so that the stability and aroma durability of the emulsion are remarkably improved. The system is still kept stable under high-temperature and high-shear conditions.

Description

Technical Field

[0001] The present invention relates to the technical field of daily chemical industry, in particular to a micro-emulsified essence and a preparation method thereof. Background Art

[0002] In food, cosmetics, and daily chemical products, the use of flavors is crucial to the sensory experience of the product. Traditional flavors are mostly in liquid form, but due to their high volatility and poor stability, they often lead to uneven aroma release and are prone to stratification or deterioration in high temperature or humid environments, affecting the product's performance and shelf life. To improve the stability of flavors in various environmental conditions, a microemulsified flavor is needed.

[0003] Microemulsified flavors encapsulate oily flavor ingredients in an emulsion system and utilize the effects of emulsifiers and co-emulsifiers to form a nano-scale oil droplet dispersion system. This structure can not only effectively delay the volatilization of the aroma, but also improve the stability of the flavor under different environmental conditions. The existing microemulsified flavor preparation technology still has some shortcomings. Some products are prone to emulsion stratification under high temperature and high shear conditions, and the aroma release rate is difficult to control, resulting in premature loss of aroma during storage, affecting the product's aroma persistence. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the present invention provides a micro-emulsified flavor and a preparation method thereof, which solve the deficiencies of the prior art in terms of stability, aroma persistence and release control of micro-emulsified flavors.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: A micro-emulsified flavor, composed of the following components by weight percentage: Oily component 15-35%, emulsifier 8-22%, co-emulsifier 3-12%, the balance is deionized water; The oily component comprises at least two components selected from citrus essential oil, peppermint oil, and rose absolute; The emulsifier is prepared by compounding polyoxyethylene sorbitan monooleate and lauryl alcohol polyoxyethylene ether in a mass ratio of 3:1-5:1; the auxiliary emulsifier is a mixture of propylene glycol and isopropyl myristate in a mass ratio of 1:0.3-1:0.6.

[0006] By adopting the above technical solution: the micro-emulsified essence significantly improves the stability of the emulsion and the persistence of the fragrance through the synergistic effect of the compounding of specific oily ingredients and the emulsifier. The citrus essential oil, peppermint oil and rose absolute in the oily ingredients are combined in proportion, and their natural polarity differences form a complementary effect. The emulsifier is combined with polyoxyethylene sorbitan monooleate and lauryl polyoxyethylene ether. By precisely controlling the HLB value, the system remains stable under high temperature and high shear conditions. The co-emulsifier composed of propylene glycol and isopropyl myristate further reduces the interfacial tension and ensures that the oil droplets are evenly dispersed to the nanometer level.

[0007] Preferably, among the oily components, citrus essential oil accounts for 40-65% of the total weight of the oily components, peppermint oil accounts for 15-30%, and rose absolute accounts for 10-25%, and the sum of the three accounts for more than 92% of the total weight of the oil phase components.

[0008] Preferably, the HLB value of the polyoxyethylene sorbitan monooleate is 14.5-16.5, the HLB value of the lauryl alcohol polyoxyethylene ether is 12.0-13.5, and the comprehensive HLB value after the two are compounded is controlled at 13.8-15.2.

[0009] Preferably, the composition further comprises an antioxidant accounting for 0.05-0.3% of the total mass of the composition, wherein the antioxidant is a compound of vitamin E and tea polyphenols, and the mass ratio of the two is 1:0.8-1:1.2.

[0010] Preferably, a method for preparing a microemulsified flavor, used for the microemulsified flavor, comprises the following steps: S1, oil phase pretreatment: ultrasonically treating the oily component at 45-50° C. for 15-20 minutes, with an ultrasonic frequency of 28-35 kHz; S2. Emulsification system construction: The pretreated oily component is shear-emulsified with the emulsifier and co-emulsifier at a speed of 800-1200 r / min for 8-12 minutes, and the system temperature is maintained at 40-45°C; S3. Preparation of aqueous phase: Preheat deionized water to 50-55°C, add the remaining emulsifier components, and stir and disperse at 400-600 r / min for 5-8 minutes; S4. Primary emulsification: inject the oil phase into the water phase at a flow rate of 0.8-1.2 L / min, and homogenize at a high speed of 2000-2500 r / min for 10-15 minutes, controlling the emulsification temperature at 55-60°C; S5, high pressure homogenization: perform three-stage gradient homogenization at a pressure of 18-35 MPa, with the first stage pressure being 18-22 MPa, the second stage pressure being 25-28 MPa, and the third stage pressure being 30-35 MPa. The processing time for each stage is 2-4 minutes. S6, aging treatment: the emulsion was allowed to stand and mature at 35-38°C for 2-3 hours, and then filtered through a 200-mesh ultrafiltration membrane; S7, finished product preparation: cooling the filtered emulsion to 25-30°C to obtain the micro-emulsified flavor; S8. Low-temperature spray drying: spray-dry the finished product under the conditions of air inlet temperature of 85-95°C, air outlet temperature of 45-50°C, and atomization pressure of 0.8-1.2 MPa to obtain microcapsule flavor powder with a moisture content of ≤3%.

[0011] Preferably, the shear rate of the shear emulsification in S2 is 8-12 m / s, and the auxiliary emulsifier is added three times at intervals of 3-5 minutes during the emulsification process, and the amount added each time is 30%-40% of the total amount of the remaining auxiliary emulsifier.

[0012] Preferably, the S4 medium- and high-speed homogenizer adopts a double-layer stator and rotor structure, with an upper rotor gap of 0.2-0.5 mm, a lower rotor gap of 0.1-0.3 mm, and a rotor linear speed of 15-20 m / s.

[0013] Preferably, in the three-stage gradient homogenization of S5, a transition period of 2-3 minutes is set between two adjacent stages, and the pressure is gradually increased at a pressure increase rate of 3-5 MPa / min.

[0014] Preferably, during the aging treatment in S6, stirring is performed at a low speed of 200-300 r / min for 2-3 minutes every 30 minutes, and the inclination angle of the stirring blade is 15-25°.

[0015] Preferably, the method further comprises performing a microcapsule stability test after S8, wherein the test conditions are storage at 40° C. and 75% relative humidity for 30 days, the microcapsule structure has no obvious damage, and the flavor release rate is ≤5%.

[0016] The present invention provides a micro-emulsified essence and a preparation method thereof. It has the following beneficial effects: 1. In the present invention, the microemulsified flavor significantly improves the stability and aroma persistence of the emulsion through the synergistic effect of the specific oily ingredients and the emulsifier. The citrus essential oil, peppermint oil and rose absolute in the oily ingredients are combined in proportion, and their natural polarity differences form a complementary effect. The emulsifier is combined with polyoxyethylene sorbitan monooleate and lauryl alcohol polyoxyethylene ether, and the HLB value is precisely controlled to ensure that the system remains stable under high temperature and high shear conditions. The co-emulsifier composed of propylene glycol and isopropyl myristate further reduces the interfacial tension, ensuring that the oil droplets are evenly dispersed to the nanometer level.

[0017] 2、The application adopts a preparation method combining three-stage gradient homogenization and low-speed curing process to realize accurate control of oil droplet particle size and optimization of structural stability, three-stage gradient homogenization avoids structural damage caused by one-time high pressure by gradually increasing the pressure, and in combination with a double-layer stator structure, the oil droplet particle size is stably maintained at 50-100 nm and uniformly distributed, periodic low-speed stirring in the curing process promotes the migration of emulsifier molecules to the interface to form a dense protective film to prevent particle aggregation, the spray drying process is carried out at low temperature to retain active ingredients of the essence, the obtained microcapsule powder has a water content of ≤3%, a concentrated particle size distribution, and a D90 / D10 value of less than 1.4.

[0018] 3、The application ensures the long-term stability of the product in extreme environments through antioxidant compounding and microcapsule stability testing, vitamin E and tea polyphenol are compounded in proportion to synergistically inhibit oxidation, so that the peroxide value of the essence after being stored at 40℃ and 75% humidity for 30 days is less than 0.02%, the microcapsule structure is tested under high temperature and high humidity, the wall material has no obvious rupture or moisture absorption phenomenon, and the essence release rate is ≤5%, achieving accurate control of the essence release rate ≤5% / 30 days, while the complete wall material structure blocks the penetration of water and oxygen. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 The application provides a microemulsified essence preparation method flowchart. Figure 2 The application provides an emulsified essence production process flowchart. DETAILED DESCRIPTION

[0020] The technical solutions of the application will be described below in conjunction with the accompanying drawings of the specification. Obviously, the described embodiments are only a part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the application.

[0021] The application provides a microemulsified essence, which is composed of the following components in percentage by weight: 15-35% of an oily component, 8-22% of an emulsifier, 3-12% of a co-emulsifier, and the balance of deionized water; The oily component comprises at least two components selected from the group consisting of citrus essential oil, mint oil, and rose absolute oil. The emulsifier is compounded from polyoxyethylene sorbitan monooleate and lauryl alcohol polyoxyethylene ether at a mass ratio of 3:1-5:1; the co-emulsifier is a mixture of propylene glycol and isopropyl myristate, and the mass ratio of the two is 1:0.3-1:0.6.

[0022] Specifically, citrus essential oil, peppermint oil and rose absolute are natural plant extracts with unique aromatic smells that can give the product a pleasant olfactory experience. The volatility of different oily components varies greatly (for example, citrus essential oil is highly volatile, while rose absolute is less volatile). Through compounding, multi-level release of aroma can be achieved. Compounding of multiple oily components can balance the intensity and persistence of aroma, avoiding the problem of monotonous aroma or rapid volatilization caused by a single component; emulsifiers can form a stable interfacial film between the oil phase and the water phase, reducing the possibility of separation of the two phases. , which can improve the stability of the emulsion and prevent stratification or demulsification; the co-emulsifier further improves the stability and uniformity of the emulsion by reducing the oil-water interfacial tension, among which viscosity is adjusted: propylene glycol, as a hydrophilic substance, can adjust the viscosity of the system and increase fluidity; isopropyl myristate, as a hydrophobic component, helps the oil phase to be better dispersed, which can significantly improve the long-term stability of the emulsion and extend the storage time; deionized water, as a continuous phase, provides sufficient medium to dilute the oily components and emulsifier to form a stable water-in-oil emulsion.

[0023] Among the oily components, citrus essential oil accounts for 40-65% of the total weight of the oily components, peppermint oil accounts for 15-30%, and rose absolute oil accounts for 10-25%. The total of the three accounts for more than 92% of the total weight of the oil phase components.

[0024] Specifically, citrus essential oil is characterized by freshness and rich fruity aroma, and is the dominant aroma source in the formula. It also has certain antibacterial and antioxidant properties, which can enhance the stability of the product. A high proportion (40%-65%) ensures the dominant position of the citrus aroma, and is paired with other low-volatile ingredients (such as rose absolute oil) to form a layered aroma. Peppermint oil has a relatively strong aroma, and when paired with citrus essential oil, it can play a balancing role, avoiding the monotony of a single citrus aroma. At the same time, it has antibacterial, anti-inflammatory and soothing effects, and is suitable for use in cosmetics or skin care products. Rose absolute oil is a low-volatile ingredient that can continue to play a role in the later stage of aroma release, prolong the durability of the aroma, enhance the aftertaste of the aroma, and make the overall aroma richer and longer-lasting.

[0025] The HLB value of polyoxyethylene sorbitan monooleate is 14.5-16.5, and the HLB value of lauryl alcohol polyoxyethylene ether is 12.0-13.5. The comprehensive HLB value of the two after compounding is controlled at 13.8-15.2.

[0026] Specifically, the HLB value is used to measure the hydrophilicity and lipophilicity of surfactants. The higher the HLB value, the stronger the hydrophilicity, and the lower the HLB value, the stronger the lipophilicity. By compounding emulsifiers with different HLB values, the comprehensive HLB value can be adjusted to adapt to the polarity requirements of specific oily components, thereby achieving a more stable emulsification system. Polyoxyethylene sorbitan monooleate has strong hydrophilicity and is suitable for dispersion in the aqueous phase to form a stable interfacial film. At the same time, it can effectively reduce the oil-water interfacial tension and promote the dispersion of the oil phase in the aqueous phase. Lauryl polyoxyethylene ether has certain hydrophilicity and lipophilicity and is suitable for medium-polarity oily components. The combination of polyoxyethylene sorbitan monooleate can make up for the shortcomings of a single emulsifier under certain conditions.

[0027] The composition also includes an antioxidant accounting for 0.05-0.3% of the total weight of the composition. The antioxidant is a compound of vitamin E and tea polyphenols, and the mass ratio of the two is 1:0.8-1:1.2.

[0028] Specifically, antioxidants are substances that can inhibit or delay oxidation reactions and are used to protect oily ingredients from oxidative degradation. Vitamin E is a fat-soluble antioxidant that can effectively capture free radicals and prevent the occurrence of oil oxidation chain reactions. Tea polyphenols are water-soluble antioxidants that can form a synergistic effect with vitamin E to further enhance antioxidant capacity. By adjusting the compounding ratio, the oxidation characteristics of different oily ingredients can be flexibly responded to. For example, for highly volatile and easily oxidized citrus essential oils, the proportion of vitamin E can be appropriately increased; while for rose absolute oil, which is highly polar and not easily oxidized, the proportion of tea polyphenols can be increased.

[0029] Please see the attached Figure 1 A method for preparing a micro-emulsified flavor, which is used for the above-mentioned micro-emulsified flavor, comprises the following steps: S1. Oil phase pretreatment: ultrasonically treat the oily components at 45-50°C for 15-20 minutes at an ultrasonic frequency of 28-35kHz; S2. Emulsification system construction: The pretreated oily component is shear-emulsified with the emulsifier and co-emulsifier at a speed of 800-1200 r / min for 8-12 minutes, and the system temperature is maintained at 40-45°C; S3. Water phase preparation: preheat deionized water to 50-55°C, add the remaining emulsifier components, and stir and disperse at 400-600 rpm for 5-8 minutes; S4. Primary emulsification: inject the oil phase into the water phase at a flow rate of 0.8-1.2 L / min, and homogenize at a high speed of 2000-2500 r / min for 10-15 minutes, controlling the emulsification temperature at 55-60°C; S5, high pressure homogenization: three-stage gradient homogenization at a pressure of 18-35 MPa, the first stage pressure is 18-22 MPa, the second stage pressure is 25-28 MPa, and the third stage pressure is 30-35 MPa, and the processing time of each stage is 2-4 minutes; S6, aging treatment: the emulsion is left to stand and age at 35-38°C for 2-3 hours, and then filtered through a 200-mesh ultrafiltration membrane; S7, product preparation: the filtered emulsion is cooled to 25-30°C to obtain a microemulsified fragrance; S8, low-temperature spray drying: the product is spray dried at an inlet temperature of 85-95°C, an outlet temperature of 45-50°C, and an atomization pressure of 0.8-1.2 MPa to obtain a microcapsule fragrance powder with a water content of ≤3%.

[0030] Please refer to the attached Figure 1 In S2, the shear rate of shear emulsification is 8-12 m / s, and the co-emulsifier is added in three times with an interval of 3-5 minutes, and the amount of each addition is 30%-40% of the total amount of the remaining co-emulsifier.

[0031] Specifically, the shear force can destroy the oil-water interface, making the oil droplets more uniformly dispersed in water, and the shear force can accelerate the migration of emulsifier molecules to the oil-water interface to form a stable interface film. Within the shear rate range of 8-12 m / s, sufficient shear force can be ensured to refine the particles, and the system will not be overheated or the emulsifier will not be excessively consumed due to too high shear rate; by adding the co-emulsifier in several times, the properties of the oil-water interface can be gradually adjusted to avoid premature solidification or instability of the interface film caused by one-time addition. After each addition of co-emulsifier, a certain time is needed to allow it to fully diffuse and cooperate with the emulsifier in the system to form a stable interface film. An interval of 3-5 minutes is sufficient for the co-emulsifier to be uniformly dispersed and play a role, while avoiding incomplete emulsification due to too short interval or reduced efficiency due to too long interval; by gradually increasing the concentration of co-emulsifier, the needs of the emulsion at different stages can be better met.

[0032] Please refer to the attached Figure 1 In S4, the high-speed homogenization adopts a double-layer stator-rotor structure, the upper rotor gap is 0.2-0.5 mm, the lower rotor gap is 0.1-0.3 mm, and the rotor linear speed is 15-20 m / s.

[0033] Specifically, the double-layer stator-rotor structure realizes the gradual refinement of oil droplets through two shear actions. The upper rotor is responsible for the preliminary crushing of large oil droplets, and the lower rotor further refines the particles. At the same time, the design of the double-layer structure can ensure that the oil droplets are sufficiently sheared and dispersed at different stages, avoiding the problems of local overheating or uneven shearing.

[0034] Please refer to the attached Figure 1In the three-stage gradient homogenization of S5, a transition period of 2-3 minutes is set between adjacent stages, and the pressure is gradually increased at a pressure increase rate of 3-5 MPa / min.

[0035] Specifically, three-stage gradient homogenization refers to the gradual refinement of emulsion particles and enhancement of their stability through three homogenization processes at different pressure levels. A 2-3 minute transition period is set after each stage of homogenization to allow the emulsion system sufficient time to rebalance and reduce local instability caused by rapid pressure increase. During the transition period, the particles in the emulsion can be further dispersed and form a stable interfacial film, reducing the risk of particle aggregation in the subsequent homogenization process. Through transition period adjustment, the emulsion particle size distribution after each stage of homogenization is ensured to be more uniform, providing a better foundation for the next stage of homogenization.

[0036] Please see the attached Figure 1 During the aging process of S6, the mixture was stirred at a low speed of 200-300 r / min for 2-3 minutes every 30 minutes, and the inclination angle of the stirring blade was 15-25°.

[0037] Specifically, aging refers to the process of allowing the emulsion to stand or gently stir for a period of time after preparation to further stabilize the emulsion and achieve optimal performance. This aging process improves the long-term stability of the emulsion, optimizes particle size distribution and interfacial film properties, and ensures uniform dispersion of functional ingredients (such as aroma). During the aging process, particles in the emulsion may slowly settle due to gravity. Brief, low-speed stirring every 30 minutes can effectively prevent stratification. An appropriate stirring speed is sufficient to redisperse any settled particles without damaging the emulsion structure.

[0038] Please see the attached Figure 1 It also includes a microcapsule stability test after S8. The test conditions are 40°C and 75% relative humidity for 30 days. The microcapsule structure has no obvious damage and the flavor release rate is ≤5%.

[0039] Specifically, the microcapsule stability test is a process of evaluating the physical integrity and functional performance of microcapsules under specific environmental conditions (such as temperature, humidity, etc.). The microcapsule stability test can verify the structural stability and aroma controlled release ability of the microcapsules during storage and use, ensuring that the product can meet long-term preservation and functional requirements in actual applications; 40°C and 75% relative humidity are high temperature and high humidity environments, which can accelerate the aging process of microcapsules, thereby quickly verifying their performance under normal storage conditions.

[0040] Example 1: 1. Technical solution: 1. Group distribution ratio: Oily ingredients: 25% (citrus essential oil 60%, peppermint oil 25%, rose absolute 15%) Emulsifier: 15% (polyoxyethylene sorbitan monooleate: lauryl alcohol polyoxyethylene ether = 4:1) Co-emulsifier: 8% (propylene glycol: isopropyl myristate = 1:0.5) Antioxidant: 0.1% (Vitamin E:Tea Polyphenols = 1:1) Balance: deionized water 2. Preparation process: S1. Oil phase pretreatment: The oily components were ultrasonically treated at 48°C for 18 minutes (frequency 30 kHz).

[0041] S2. Emulsification system construction: shear emulsification at 1000 r / min for 10 minutes (shear rate 10 m / s), adding co-emulsifier (35% each time) three times with an interval of 4 minutes, and maintaining the temperature at 42°C.

[0042] S3. Preparation of aqueous phase: Preheat deionized water to 52°C and stir at 500 rpm for 6 minutes.

[0043] S4. Primary emulsification: inject the oil phase into the water phase at 1.0 L / min, and homogenize at 2200 rpm for 12 min (double-layer stator and rotor: upper gap 0.3 mm, lower gap 0.2 mm, linear speed 18 m / s), temperature 58°C.

[0044] S5. High-pressure homogenization: three-stage gradient homogenization (20 MPa → 27 MPa → 33 MPa, 3 minutes per stage, pressure increase rate 4 MPa / min).

[0045] S6. Aging treatment: standing at 36°C for 2.5 hours, filtering through a 200-mesh ultrafiltration membrane, stirring at a low speed of 250 r / min for 2.5 minutes every 30 minutes (blade tilt angle 20°).

[0046] S7. Finished product preparation: Cool to 25-30°C to obtain micro-emulsified flavor.

[0047] S8. Low-temperature spray drying: inlet air 90℃, outlet air 48℃, atomization pressure 1.0MPa, to obtain microcapsule flavor powder with a moisture content of ≤3%.

[0048] 3. Technical effects: Particle size control: 80-120nm (D90 / D10=1.4), three-stage gradient homogenization process significantly refines droplets.

[0049] Stability: Zeta potential absolute value 38mV, no stratification during centrifugation (the stratification rate of the traditional process is 22%).

[0050] Entrapment rate and sustained release: 93.5% embedding rate, 30-day release rate ≤3%, composite emulsifier (HLB14.5+12.0) synergistically improves the polarity matching of the oil phase.

[0051] Example 2: 1. Technical solution: 1. Group distribution ratio: Oily ingredients: 30% (citrus essential oil 65%, peppermint oil 20%, rose absolute 15%) Emulsifier: 20% (polyoxyethylene sorbitan monooleate: lauryl alcohol polyoxyethylene ether = 5:1) Co-emulsifier: 10% (propylene glycol: isopropyl myristate = 1:0.6) Antioxidant: 0.2% (Vitamin E:Tea Polyphenols = 1:1.2) Balance: deionized water 2. Preparation process: S1. Oil phase pretreatment: ultrasonic treatment at 50°C for 20 minutes (frequency 35 kHz).

[0052] S2. Construction of emulsification system: shear emulsification at 1200 r / min for 12 minutes (shear rate 12 m / s), adding co-emulsifier (40% each time) three times with 5-minute intervals, and maintaining the temperature at 45°C.

[0053] S4. Primary emulsification: 1.2 L / min oil phase injection, 2500 rpm high-speed homogenization for 15 minutes (double-layer stator and rotor: upper layer gap 0.5 mm, lower layer 0.3 mm, linear speed 20 m / s).

[0054] S5. High-pressure homogenization: three-stage gradient homogenization (22 MPa → 28 MPa → 35 MPa, 4 minutes per stage, pressure increase rate 5 MPa / min).

[0055] S6. Aging treatment: let it stand at 38°C for 3 hours, stirring it at a low speed of 300 r / min for 3 minutes every 30 minutes (blade inclination angle 25°).

[0056] S8, low temperature spray drying: inlet air 95℃, outlet air 45℃, atomization pressure 1.2MPa.

[0057] 3. Technical effects: Particle size and stability: 70-130nm (D90 / D10=1.5), Zeta potential -35mV, dynamic aging process inhibits particle aggregation.

[0058] Antioxidant performance: 30-day release rate ≤2.5%, vitamin E and tea polyphenols synergistically resist oxidation and inhibit flavor degradation.

[0059] Example 3: 1. Technical solution: 1. Group distribution ratio: Oily ingredients: 18% (citrus essential oil 50%, peppermint oil 30%, rose absolute 20%) Emulsifier: 10% (polyoxyethylene sorbitan monooleate: lauryl alcohol polyoxyethylene ether = 3:1) Co-emulsifier: 5% (propylene glycol: isopropyl myristate = 1:0.3) Antioxidant: 0.05% (Vitamin E:Tea Polyphenols = 1:0.8) Balance: deionized water 2. Preparation process: S1. Oil phase pretreatment: ultrasonic treatment at 45°C for 15 minutes (frequency 28 kHz).

[0060] S2. Emulsification system construction: shear emulsification at 800 r / min for 8 minutes (shear rate 8 m / s), adding co-emulsifier three times with an interval of 3 minutes (30% each time), and maintaining the temperature at 40°C.

[0061] S4. Primary emulsification: 0.8 L / min oil phase injection, 2000 rpm high-speed homogenization for 10 minutes (double-layer stator and rotor: upper layer gap 0.2 mm, lower layer 0.1 mm, linear speed 15 m / s).

[0062] S5. High-pressure homogenization: three-stage gradient homogenization (18 MPa → 25 MPa → 30 MPa, 2 minutes per stage, pressure increase rate 3 MPa / min).

[0063] S6. Aging treatment: let it stand at 35°C for 2 hours, stirring it at a low speed of 200 r / min for 2 minutes every 30 minutes (blade inclination angle 15°).

[0064] S8, low-temperature spray drying: inlet air 85℃, outlet air 50℃, atomization pressure 0.8MPa.

[0065] 3. Technical effects: Emulsion particle size: 90-140nm (D90 / D10=1.6); Zeta potential absolute value: 32mV; Process adaptability: Under low oil phase (18%) conditions, the composite emulsifier (HLB14.5+12.0) still achieved a 94.1% embedding rate; sustained-release performance: 30-day release rate ≤4%, and optimized spray drying parameters (inlet air 85°C) reduced the loss of heat-sensitive components.

[0066] Comparative example (traditional process): 1. Technical solution: Component allocation ratio: oily ingredients 25% (citrus essential oil 60%, peppermint oil 25%, rose absolute oil 15%), emulsifier 15% (single emulsifier Tween 80), co-emulsifier 8% (propylene glycol).

[0067] 2. Preparation process: single-stage homogenization (25 MPa x 10 minutes), omitting ultrasonic treatment and dynamic ripening.

[0068] 3. Experimental results: Emulsion particle size: 220-280 nm (D90 / D10 = 2.1); Zeta potential absolute value: 28 mV; Centrifugal stability: slight stratification; Microcapsule release rate: 10% within 30 days.

[0069] I. Comparison of experimental results and analysis 1. Test items and standards Test item Test standard Instrument model Particle size distribution GB / T 19077-2016 Malvern Zetasizer Zeta potential ISO 13099-2012 Nanoparticle size analyzer Centrifugal stability GB / T 11543-2008 Centrifuge TG16-WS Embedding rate Gas chromatography (GB / T 31124) Agilent 7890B 2. Comparison of experimental results Index Example 1 Example 2 Example 3 Comparative example Average particle size (nm) 85 95 78 220 Zeta potential (mV) -38 -35 -40 -18 Centrifugal layering rate (%) 0 0 0 22 Embedding rate (%) 93.5 91.8 94.1 68.3 30-day release rate (%) 4.2 4.8 3.9 19.7 3. Experimental verification and summary Three-stage gradient homogenization: the average particle size of Examples 1-3 is ≤95 nm, while the particle size distribution uniformity of the Comparative Example is increased by more than 60%.

[0070] Dynamic ripening stirring: the Zeta potential absolute value of the example is ≥35 mV, the centrifugal stability is 100%, and the stratification rate of the traditional process is 22%.

[0071] Compound emulsifier compounding: the embedding rate is ≥91.8%, and the Comparative Example is only 68.3%, and the HLB synergistic effect improves the oil-water compatibility.

[0072] Particle size control (50-150 nm) meets the food / cosmetic nanoemulsion standard (GB / T19077-2016); Microcapsule slow-release performance (release rate ≤5%) adapts to long-acting fragrance needs, such as skin care slow-release fragrance and food controlled-release flavoring agent.

[0073] 4. Conclusion: The present application refines the droplets through gradient homogenization, enhances the interface stability through dynamic ripening, and precisely matches the oil phase polarity through compound emulsifier, solving the problems of uneven particle size, easy stratification and low embedding rate in traditional microemulsion process.

[0074] Example 4: Production process flow of emulsified fragrance Please refer to the attached Figure 2 : I. Raw material preparation stage First, incoming raw materials undergo incoming inspection to ensure they meet relevant quality standards. Once qualified, they are properly stored in designated areas (raw material storage). Prior to use, raw materials are checked and issued according to the production plan. Pre-processing, including filtering, dissolving, and cooling, is performed based on specific needs to ensure smooth processing in subsequent steps.

[0075] 2. Critical Control Point CCP2: Weighing and Preparation Entering the critical control point CCP2, we begin to weigh and prepare the flavor. This stage is divided into three main parts: 1. Oil phase preparation: Accurately weigh and mix the oil components according to the formula.

[0076] 2. Preparation of water phase: prepare water-soluble ingredients in proportion.

[0077] 3. Preparation of pigment solution: The pigment solution is mixed with the oil phase and water phase after high-speed stirring to form colostrum.

[0078] During this process, we strictly verify whether the amount of food additives added complies with the national standard GB2760 to ensure product safety and compliance.

[0079] Subsequently, the prepared oil phase, water phase and pigment solution are mixed and colostrum stirred to fully disperse the components and prepare for the next step of homogenization.

[0080] 3. Homogenization and Inspection After the colostrum is stirred, it is homogenized, where high pressure or mechanical shearing forces are used to further refine the particles, making the emulsion more uniform and stable. The homogenized product undergoes rigorous product inspection to ensure that it meets quality standards.

[0081] IV. Critical Control Point CCP3: Filtration and Packaging If the product passes inspection, proceed to CCP3 for filtration. Use a 100-mesh filter or, if necessary, remove residue based on the recipe to ensure the emulsion is pure and free of impurities. At the same time, inspect the packaging materials to ensure they meet hygiene and specification requirements. Next, complete the following steps: Filling and weighing: quantitatively filling the emulsion into the container.

[0082] · Cap: Seal the container to prevent contamination.

[0083] Packaging: labeling, sealing, boxing, packaging, and finally storage of finished products.

[0084] 5. Disposal of defective products If a product is found to be unqualified at any stage of the inspection, the unqualified product review and disposal procedure will be initiated to analyze the cause and take corrective measures to ensure that the problem is resolved in a timely manner.

[0085] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A microemulsified flavor, characterized in that: By weight percentage, it is composed of the following components: Oily component 15-35%, emulsifier 8-22%, co-emulsifier 3-12%, the balance is deionized water; The oily component comprises at least two components selected from citrus essential oil, peppermint oil, and rose absolute; The emulsifier is prepared by compounding polyoxyethylene sorbitan monooleate and lauryl alcohol polyoxyethylene ether in a mass ratio of 3:1-5:1; The auxiliary emulsifier is a mixture of propylene glycol and isopropyl myristate, and the mass ratio of the two is 1:0.3-1:0.

6.

2. A microemulsified flavor according to claim 1, characterized in that, Among the oily components, citrus essential oil accounts for 40-65% of the total weight of the oily components, peppermint oil accounts for 15-30%, and rose absolute accounts for 10-25%, and the sum of the three accounts for more than 92% of the total weight of the oil phase components.

3. A microemulsified flavor according to claim 1, characterized in that, The HLB value of the polyoxyethylene sorbitan monooleate is 14.5-16.5, and the HLB value of the lauryl alcohol polyoxyethylene ether is 12.0-13.

5. The comprehensive HLB value of the compounded polyoxyethylene sorbitan monooleate is controlled at 13.8-15.

2.

4. A micro-emulsified flavor according to claim 1, characterized in that, The composition also includes an antioxidant accounting for 0.05-0.3% of the total weight of the composition. The antioxidant is a compound of vitamin E and tea polyphenols, and the mass ratio of the two is 1:0.8-1:1.

2.

5. A method for preparing a microemulsified flavor, characterized in that: A micro-emulsified flavor according to any one of claims 1 to 4, comprising the following steps: S1. Oil phase pretreatment: ultrasonically treat the oily components at 45-50°C for 15-20 minutes at an ultrasonic frequency of 28-35kHz; S2. Emulsification system construction: The pretreated oily component is shear-emulsified with the emulsifier and co-emulsifier at a speed of 800-1200 r / min for 8-12 minutes, and the system temperature is maintained at 40-45°C; S3. Preparation of aqueous phase: Preheat deionized water to 50-55°C, add the remaining emulsifier components, and stir and disperse at 400-600 r / min for 5-8 minutes; S4. Primary emulsification: inject the oil phase into the water phase at a flow rate of 0.8-1.2 L / min, and homogenize at a high speed of 2000-2500 r / min for 10-15 minutes, controlling the emulsification temperature at 55-60°C; S5, high pressure homogenization: perform three-stage gradient homogenization at a pressure of 18-35 MPa, with the first stage pressure being 18-22 MPa, the second stage pressure being 25-28 MPa, and the third stage pressure being 30-35 MPa. The processing time for each stage is 2-4 minutes. S6, aging treatment: the emulsion was allowed to stand and mature at 35-38°C for 2-3 hours, and then filtered through a 200-mesh ultrafiltration membrane; S7, finished product preparation: cooling the filtered emulsion to 25-30°C to obtain the micro-emulsified flavor; S8. Low-temperature spray drying: spray dry the finished product under the conditions of air inlet temperature of 85-95°C, air outlet temperature of 45-50°C, and atomization pressure of 0.8-1.2MPa to obtain microcapsule flavor powder with a moisture content of ≤3%.

6. The method for preparing a micro-emulsified flavor according to claim 5, characterized in that: The shear rate of the shear emulsification in S2 is 8-12 m / s, and the co-emulsifier is added three times with an interval of 3-5 minutes during the emulsification process, and the amount added each time is 30%-40% of the total amount of the remaining co-emulsifier.

7. The method for preparing a microemulsified flavor according to claim 5, characterized in that: The S4 medium- and high-speed homogenizer adopts a double-layer stator and rotor structure, with an upper rotor gap of 0.2-0.5mm, a lower rotor gap of 0.1-0.3mm, and a rotor linear speed of 15-20m / s.

8. The method for preparing a micro-emulsified flavor according to claim 5, characterized in that: In the three-stage gradient homogenization of S5, a transition period of 2-3 minutes is set between two adjacent stages, and the pressure is gradually increased at a pressure increase rate of 3-5 MPa / min.

9. The method for preparing a micro-emulsified flavor according to claim 5, characterized in that: During the aging process of S6, the mixture is stirred at a low speed of 200-300 r / min for 2-3 minutes every 30 minutes, and the inclination angle of the stirring blade is 15-25°.

10. The method for preparing a micro-emulsified flavor according to claim 5, characterized in that: It also includes a microcapsule stability test after S8. The test conditions are storage at 40°C and 75% relative humidity for 30 days. There is no obvious damage to the microcapsule structure and the flavor release rate is ≤5%.

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