Transparent micro-emulsion essence and preparation method thereof
By compounding modified sophorolipids with enzymatic lecithin and using nano-zinc oxide, combined with precise pH control and gradient homogenization technology, the stability and aroma fidelity problems of transparent microemulsions were solved, and the production of transparent microemulsion flavors with high stability and long shelf life was achieved.
Patent Information
- Application Number
- CN202510844633.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-23
- Publication Date
- 2025-09-23
AI Technical Summary
It is difficult to form a stable transparent microemulsion in a water-based system with existing technology, and the essence is easily oxidized during storage, resulting in aroma deterioration, and the product transparency and stability are insufficient.
Modified sophorolipids and enzymatically hydrolyzed lecithin are used as composite emulsifiers, combined with nano zinc oxide and precise pH control, and nano-scale oil droplets are formed through three-stage gradient high-pressure homogenization and ultrasonic dispersion. Combined with online particle size and turbidity detection and selective treatment, the product is finally nitrogen-filled and packaged to ensure product stability.
The high physical stability and aroma fidelity of the transparent micro-emulsion flavor are achieved, which significantly extends the shelf life of the product and improves the control accuracy and yield of the production process.
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Figure CN120682877A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of essence preparation, in particular to a transparent micro-emulsion essence and a preparation method thereof. Background Art
[0002] Fragrances, as core ingredients that impart pleasant aromas to a wide range of products, are widely used in cosmetics, food, pharmaceuticals, and other fields. However, the direct application of many flavors, especially oil-soluble ones, in water-based systems is limited by their insolubility or low solubility. This can easily lead to product separation and turbidity, potentially compromising the uniform release and stability of the fragrance. To overcome these issues, preparing flavors into microemulsions has become an important technological approach. A microemulsion is a thermodynamically or kinetically stable, optically transparent or translucent colloidal dispersion system composed of an oil phase, an aqueous phase, a surfactant, and an optional co-surfactant, which forms spontaneously or with low energy input. The droplet size is typically in the nanometer range (e.g., 10-200 nm). This structure not only improves the dispersion of the fragrance in the aqueous phase but also helps protect the fragrance from external factors such as oxidation and volatilization, thereby extending the aroma's longevity.
[0003] Existing technologies often struggle to balance the long-term physical stability and optical clarity of microemulsions. While a variety of emulsifiers have been used in fragrance microemulsification, single emulsifiers or simple compound systems sometimes struggle to form sufficiently strong and flexible interfacial films to effectively prevent nanoscale oil droplets from austenitizing, coalescing, or flocculating during long-term storage or under varying environmental conditions (such as temperature fluctuations), leading to stratification, precipitation, or decreased transparency. In particular, achieving a highly clear and transparent appearance places higher demands on the selection and proportioning of emulsifiers, as well as the regulation of the microstructure of the entire system. However, existing technologies lack systematic optimization solutions for this purpose, sometimes relying on empirical screening and lacking in-depth consideration of the synergistic mechanisms of multiple components.
[0004] When it comes to the chemical stability and aroma fidelity of flavors, existing technologies focus primarily on the emulsification process itself, with insufficient attention paid to the initial quality of the raw materials and subsequent antioxidant protection throughout the entire process. Flavor molecules, especially those from natural sources, contain numerous chemical components that are susceptible to oxidation or hydrolysis. If the flavor raw materials themselves have already undergone a certain degree of degradation (e.g., high peroxide or acid values), or if active substances such as oxygen are not effectively isolated during preparation and storage, then even if a physically stable microemulsion is formed, the characteristic aroma of the flavor may deteriorate over time, producing an off-flavor, significantly shortening the product's effective shelf life and sensory acceptability. Summary of the Invention
[0005] The purpose of the present invention is to provide a transparent microemulsion essence and a preparation method thereof, which solves the problems in the prior art of essence microemulsions, such as poor physical stability, insufficient transparency, easy deterioration of fragrance, imprecise production process control, and difficulty in ensuring product purity and safety.
[0006] To achieve the above objectives, the present invention is implemented through the following technical solutions: A transparent micro-emulsifying essence, which is composed of the following components by mass percentage: Fragrance base 15-25%; Modified sophorolipids 1.2-1.8%; Enzymatic lecithin 0.6-1.2%; Deionized water 65-75%; Propylene glycol 5-8%; Nano zinc oxide 0.01-0.03%.
[0007] Furthermore, the flavor base is the core functional oil phase. Modified sophorolipids and enzymatically hydrolyzed lecithin are combined as a composite emulsifier. Utilizing their differences in hydrophilic-lipophilic balance (HLB) and molecular structure, they can form a more stable and flexible interfacial film at the oil-water interface, effectively reducing interfacial tension and forming an O / W microemulsion with extremely small and evenly distributed particles.
[0008] Preferably, the flavor base is selected from at least one of fat-soluble citrus flavors, fat-soluble floral flavors or fat-soluble fruit flavors, and the acid value of the flavor base is less than or equal to 2.0 mgKOH / g, and the peroxide value is less than or equal to 0.5 mmol / kg.
[0009] Furthermore, the selection of a specific type of fat-soluble flavor ensures its good compatibility with the O / W microemulsion system, avoiding the damage these degradation products may cause to the microemulsion interface membrane or trigger subsequent adverse chemical reactions, thereby ensuring the fidelity of the final product aroma and the stability of the microemulsion structure.
[0010] Preferably, the pH value of the transparent micro-emulsifying essence is 6.5-7.5, and food-grade nitrogen is filled into the transparent micro-emulsifying essence to form a protective atmosphere, wherein the oxygen content is less than or equal to 0.5%.
[0011] Furthermore, controlling the pH value in the near-neutral range of 6.5-7.5 is beneficial to maintaining the optimal emulsifying properties of the selected composite emulsifier, and slowing down the hydrolysis rate of certain ester components in the flavor, thereby maintaining the aroma characteristics.
[0012] A method for preparing a transparent micro-emulsifying essence comprises the following steps: Step 1, the additive selection step, comprises: Raw materials must be inspected and accepted, with the peroxide value of the flavor base being less than or equal to 0.5mmol / kg, and the total microbial count of the emulsifier being less than or equal to 50CFU / g; adding an external additive, wherein the external additive comprises 5-8% propylene glycol and 0.01-0.03% nano zinc oxide; Step 2, a pre-mixing step, comprises: Oil phase pretreatment: dynamically mixing the flavor base and the modified sophorolipid at a temperature of 45-55° C. for 25-35 minutes to form an oil phase mixture; Preparation of aqueous phase: Disperse enzymatically hydrolyzed lecithin in deionized water, adjust the pH to 6.5-7.5, and cool the aqueous phase mixture to 20-25°C; Step 3, emulsification step, comprising: Colostrum formation: the oil phase mixture and the water phase mixture are mixed in a volume ratio of 1:3 to 1:5, and then subjected to a three-stage gradient high-pressure homogenization process; Ultrafine dispersion: After the colostrum is formed, the nano zinc oxide is added and ultrasonic dispersion is performed, wherein the ultrasonic power density is 250-350W / cm 2 , processing time is 4-6 minutes; Step 4, optional processing step, including: Online detection of turbidity and particle size of intermediate products, where the qualified range of turbidity is 15-25 NTU and the qualified range of particle size D50 is 70-90 nm; If the turbidity and particle size of the intermediate product are qualified, the intermediate product is filtered through a 100-mesh filter and then proceeds to step 5; If the turbidity or particle size test of the intermediate product fails, 0.3-0.5% of polyglycerol ricinoleate is added to the intermediate product, followed by filtering through a 100-mesh filter, and then returning the filtered product to step 3 for secondary emulsification treatment; Step 5: Final inspection and warehousing steps, including: The product was subjected to an accelerated stability test, wherein after 90 days of storage at 40°C, the peroxide value was less than or equal to 3.0 mmol / kg; The product is packed with nitrogen, wherein the nitrogen filling pressure is 0.10-0.15MPa, and the residual oxygen in the package is less than or equal to 0.3%.
[0013] Furthermore, the mechanism of step 1 lies in source quality control, ensuring that the raw materials entering the system have high chemical stability and microbial safety, laying the foundation for the subsequent formation of stable microemulsions.
[0014] The innovation of step 2 lies in the refined independent pretreatment of the oil phase and the water phase. The heating and mixing of the oil phase promotes the dissolution and activation of the emulsifier, while the pH adjustment and cooling of the water phase optimize the hydration state of the emulsifier and protect heat-sensitive components, thereby improving the subsequent emulsification efficiency.
[0015] Step 3 is the core emulsification step. The three-stage gradient high-pressure homogenization applies energy step by step to more gently and efficiently reduce the oil droplet size to the nanometer level to form colostrum. Nano-zinc oxide is then added and ultrasonic dispersion is performed. The ultrasonic cavitation effect is used to ensure the uniform dispersion of nanoparticles without destroying the formed colostrum structure. This is the key to ensuring the transparency and stability of the final product.
[0016] The innovation of step 4 lies in its closed-loop quality control and dynamic adjustment mechanism. Turbidity and particle size are monitored online, and qualified products are filtered and forwarded to the next stage to ensure purity. Unqualified products are supplemented with an emulsifier (polyglycerol polyricinoleate, which may improve the system by changing the interfacial film properties or aiding emulsification) and filtered to remove coarse particles before being returned for re-emulsification. This selective treatment significantly improves the process's tolerance and yield.
[0017] Step 5 verifies the long-term storage performance of the product through accelerated stability testing, and nitrogen-filled packaging isolates oxygen to the greatest extent possible to ensure the quality of the product during its shelf life.
[0018] Preferably, the three-stage gradient high-pressure homogenization treatment in step 3 includes: First-stage homogenization treatment, with a homogenization pressure of 75-85 MPa, and 2-3 cycles; Secondary homogenization treatment, with a homogenization pressure of 45-55 MPa, and 2-3 cycles; Three-stage homogenization treatment, with a homogenization pressure of 25-35 MPa and 1-2 cycles; In addition, after the homogenization treatment, a pulsed negative pressure degassing treatment is implemented, wherein the negative pressure range is -0.07 to -0.09 MPa and the pulse frequency is 1-3 Hz.
[0019] Furthermore, the three-stage gradient high-pressure homogenization utilizes a multi-stage process, progressing from high to low pressure. Its mechanism is to more finely and gently break up oil droplets through progressively decreasing shear strength. The high-pressure stage primarily breaks up large oil droplets, while the subsequent lower pressure stages further refine the droplets and optimize the particle size distribution.
[0020] Pulsed negative pressure degassing: Degassing is performed immediately after each homogenization stage. Its mechanism is to promptly remove tiny bubbles that may be introduced or dissolved in the liquid due to the intense shear and turbulence during homogenization. Compared to continuous negative pressure, pulsed negative pressure can effectively degas while reducing excessive system disturbance and excessive solvent volatilization. This combined process is crucial for achieving microemulsified flavors with high clarity and physical stability.
[0021] Preferably, the secondary emulsification treatment in step 4 includes increasing the homogenization pressure by 10-15%, and the nano zinc oxide is added within 5-8 minutes after the secondary homogenization treatment is completed.
[0022] Furthermore, the homogenization pressure is increased by 10-15%: The homogenization pressure is appropriately increased during the secondary emulsification. The mechanism may be to overcome the insufficient initial emulsification or the changes in system properties (such as viscosity and interfacial tension) after the addition of co-emulsifiers, and to provide sufficient energy to ensure that the oil droplets can be effectively broken and dispersed to achieve the qualified particle size and turbidity.
[0023] Preferably, the additive selection step in step 1 further includes conducting a qualification review of the raw material supplier and conducting a pesticide residue test on the raw material, wherein the pesticide residue content is less than or equal to 0.01 mg / kg.
[0024] Furthermore, supplier qualification review: its mechanism is to ensure the batch stability and overall quality level of the purchased raw materials from the source by evaluating the supplier's production capacity, quality management system, etc., which is a preventive quality assurance measure.
[0025] Pesticide Residue Testing: Naturally sourced raw materials, such as flavor bases, are tested for pesticide residues, with strict limits set (≤0.01mg / kg). This ensures the safety of the final product for consumption or contact, while also preventing potential pesticide residues from adversely affecting the stability or sensory properties of the microemulsion. This comprehensive quality control, which goes beyond conventional physical and chemical indicators, reflects the high standards of product quality and safety.
[0026] Preferably, the emulsification step in step 3 is carried out in a controlled production environment, and the controlled production environment monitoring includes: The residual microorganisms on the surface of the equipment are less than or equal to 10 CFU / cm 2 ; The conductivity of process water is less than or equal to 5μS / cm.
[0027] Furthermore, the control of microbial residues on the surface of the equipment: its mechanism is to prevent the production equipment from becoming a source of microbial contamination, to prevent microorganisms and their metabolites from entering the product, causing product corruption, demulsification or the generation of unpleasant odors, and to ensure the microbial safety and stability of the product.
[0028] Conductivity control of process water: The conductivity of deionized water is a key indicator of its purity. Low conductivity (≤5μS / cm) indicates extremely low levels of ionic impurities in the water. This is done to prevent these ions (especially multivalent metal ions) from reacting with emulsifiers (e.g., precipitation, reduced emulsifying activity), or from altering the pH and ionic strength of the system, which could interfere with the formation and stability of the microemulsion.
[0029] Preferably, the final inspection and warehousing step in step 5 further includes a 100-day storage verification of the nitrogen-filled packaged product, wherein the dielectric constant fluctuation is less than or equal to 0.5.
[0030] Furthermore, 100-day storage verification: by storing the product at room temperature or under specific conditions for a longer period of time, the stability of the product during its actual shelf life can be more comprehensively evaluated.
[0031] Dielectric constant fluctuation monitoring: As a colloidal dispersion system, the dielectric constant of a microemulsion is closely related to its internal structure (such as oil droplet size, interfacial properties, and continuous phase properties). When a microemulsion undergoes structural changes, such as droplet coalescence, phase separation, or austenitization, resulting in increased or nonuniform particle size, the overall dielectric properties of the system can change. Therefore, it is important to monitor the fluctuation of the dielectric constant during storage. Minimal fluctuations (≤0.5) indicate that the microemulsion's microstructure remains highly stable.
[0032] Preferably, the filtering operation through a 100-mesh filter in step 4 has the following specific parameters: a 100-mesh metal filter is used, and the filtering flow rate is controlled at 0.5-1.2 m 3 / h, the filtration pressure difference is 0.05-0.15MPa.
[0033] Furthermore, a 100-mesh metal filter screen with a specific pore size is selected to effectively remove trace insoluble impurities, incompletely dispersed agglomerates, or large oil droplet aggregates formed before reprocessing of unqualified products. This improves the clarity and uniformity of the final product and creates better conditions for secondary emulsification. Metal materials may also be considered for their durability and ease of cleaning.
[0034] Convection velocity (0.5-1.2m 3 The flow rate (flow / h) and differential pressure (0.05-0.15 MPa) are controlled to ensure filtration efficiency and operational safety. Excessively high flow rates or differential pressures can damage the filter screen, cause the filter cake to compact too quickly and clog the filter screen, or create excessive shear forces on the microemulsion droplets, causing structural damage.
[0035] In summary, the present invention includes at least one of the following beneficial technical effects: 1. This invention achieves excellent physical stability and a highly clear appearance in a transparent microemulsion flavor through the synergistic effect of modified sophorolipids and enzymatically hydrolyzed lecithin, combined with a specific ratio of nano-zinc oxide and precise pH control. Compared to existing technologies, which often suffer from poor emulsion stability and insufficient transparency due to improper emulsifier selection or component incompatibility, this invention significantly enhances the long-term uniformity and visual quality of microemulsions.
[0036] 2. The present invention implements strict quality control standards from the raw material selection stage, specifically limiting the peroxide value and acid value of the flavor base and the microbial indicators of the emulsifier, supplemented by nitrogen inertization technology during the production process. This series of measures effectively inhibits the oxidation and hydrolysis reactions of the flavor components, thereby maximizing the preservation of the flavor's inherent aroma characteristics and significantly extending the product's shelf life. Existing technologies that fail to pay sufficient attention to the initial quality of raw materials and antioxidant measures can easily lead to product degradation and a shortened shelf life. The present invention overcomes these deficiencies through source control and process assurance.
[0037] 3. The present invention innovatively constructs a preparation process that integrates three-stage gradient high-pressure homogenization, pulsed negative pressure degassing, online quality monitoring, and selective rework. This refined emulsification process and dynamic feedback adjustment mechanism ensure the uniform and small particle size of the microemulsion and the high stability of the system, thereby improving the control accuracy and yield of the production process. Compared with the problems of relatively extensive homogenization parameter settings in traditional processes, lack of real-time quality feedback and effective correction measures, resulting in large differences between product batches and high energy consumption, the present invention promotes the stability and efficiency of transparent microemulsion flavor production.
[0038] 4. The present invention systematically implements quality and safety assurance measures throughout the entire preparation process, including key control points such as the qualification review of raw material suppliers, strict monitoring of pesticide residues, maintenance of the cleanliness of the emulsification production environment, and precision filtration of the final product. These integrated control links ensure that the final transparent micro-emulsified flavor has higher purity and safety in use. The existing technology may have weak links in the whole-chain quality and safety management, which easily lead to the introduction of impurities or pollutants. The present invention improves the overall quality and safety standards of the product through multi-dimensional purification and rigorous control. BRIEF DESCRIPTION OF THE DRAWINGS
[0039] Figure 1 Schematic diagram of the method of the present invention. DETAILED DESCRIPTION
[0040] The following is combined with Figure 1 , the present invention is described in further detail.
[0041] The present invention provides a transparent micro-emulsion essence and a preparation method thereof Example
[0042] This embodiment provides a preparation method of a transparent microemulsification essence.
[0043] Prepare 1000g of transparent micro-emulsifying essence, the components of which are calculated by mass percentage: Fat-soluble citrus flavor (acid value 1.0 mgKOH / g, peroxide value 0.2 mmol / kg): 20%; Modified sophorolipids: 1.5%; Enzymatically hydrolyzed lecithin: 0.9%; Propylene glycol: 6.5%; Nano zinc oxide: 0.02%; Deionized water: 71.08%.
[0044] The preparation steps are as follows: Step 1: Additive selection steps: The selected fat-soluble citrus flavoring raw materials were inspected and tested to ensure their peroxide value was less than or equal to 0.5 mmol / kg. Modified sophorolipids and enzymatically hydrolyzed lecithin (used as an emulsifier) were inspected and tested to ensure their total microbial count was less than or equal to 50 CFU / g. The above components were weighed according to the formula, with propylene glycol and nano-zinc oxide prepared as external additives. All raw materials met the requirement of pesticide residue content less than or equal to 0.01 mg / kg.
[0045] Step 2: Pre-mixing process: Oil phase pretreatment: 200 g of fat-soluble citrus flavor was mixed with 15 g of modified sophorolipid and dynamically stirred at 50° C. for 30 minutes to form a uniform oil phase mixture.
[0046] Preparation of aqueous phase: Disperse 9 g of enzymatically hydrolyzed lecithin in 710.8 g of deionized water, add 65 g of propylene glycol, stir thoroughly to dissolve, adjust the pH value of the aqueous phase mixture to 7.0, and then cool the aqueous phase mixture to 22.5°C for use.
[0047] Step 3: Emulsification step: Colostrum Formation: The oil phase mixture obtained from the pretreatment was mixed with the aqueous phase mixture at a volume ratio of 1:4, followed by a three-stage gradient high-pressure homogenization process. Homogenization parameters were: Level 1 homogenization pressure of 80 MPa, three cycles; Level 2 homogenization pressure of 50 MPa, three cycles; Level 3 homogenization pressure of 30 MPa, two cycles. Immediately following homogenization, pulsed negative pressure degassing was performed at a negative pressure of -0.08 MPa and a pulse frequency of 2 Hz.
[0048] Ultrafine dispersion: After the three-stage gradient high-pressure homogenization treatment to form colostrum, add 0.2g of nano zinc oxide and continue ultrasonic dispersion treatment. The ultrasonic power density is controlled at 300W / cm 2 The emulsification step is carried out in a controlled production environment to ensure that the residual microbial count on the equipment surface is less than or equal to 10 CFU / cm 2 , the conductivity of the process water (deionized water) used is less than or equal to 5μS / cm.
[0049] Step 4: Optional processing steps: The turbidity and particle size D50 of the intermediate product were tested online. In this embodiment, the test results were: turbidity 20 NTU, particle size D50 80 nm, both within the qualified range (turbidity 15-25 NTU, particle size D50 70-90 nm).
[0050] The qualified intermediate product was filtered through a 100-mesh metal filter, and the filtration flow rate was controlled at 0.85m 3 / h, the filtration pressure difference is 0.10MPa.
[0051] If the online test fails, 0.3-0.5% (by total amount) of polyglycerol ricinoleate is added to the intermediate product, which is then filtered through a 100-mesh metal filter. The filtered product is then returned to step 3 for secondary emulsification. The homogenization pressure during the secondary emulsification is increased by 10-15% compared to the initial emulsification, and nano zinc oxide is added within 5-8 minutes after the secondary homogenization of the secondary emulsification is completed.
[0052] Step 5: Final inspection and warehousing steps: The filtered product underwent accelerated stability testing. After 90 days of storage at 40°C, the peroxide value was found to be less than or equal to 3.0 mmol / kg. The product was packaged in a nitrogen-filled container at a pressure of 0.125 MPa, ensuring that the residual oxygen content in the package was less than or equal to 0.3%. The final product pH was 7.0. After 100 days of storage, the dielectric constant fluctuation of the packaged product was verified to be less than or equal to 0.5. The product has a clear appearance and a pure aroma.
[0053] Example 2 This embodiment provides a preparation method of a transparent microemulsification essence.
[0054] Prepare 1000g of transparent micro-emulsifying essence, the components of which are calculated by mass percentage: Fat-soluble floral flavor (acid value 0.8mgKOH / g, peroxide value 0.15mmol / kg): 15%; Modified sophorolipids: 1.2%; Enzymatically hydrolyzed lecithin: 0.6%; Propylene glycol: 5%; Nano zinc oxide: 0.01%; Deionized water: 78.19%.
[0055] The preparation steps are as follows: Step 1: Additive selection steps: The selected fat-soluble floral flavoring ingredients were inspected to ensure their peroxide values met the requirements. Modified sophorolipids and enzymatically hydrolyzed lecithin were inspected to ensure their total microbial counts met the requirements. The above components were weighed according to the recipe. All raw materials met the pesticide residue limit requirements.
[0056] Step 2: Pre-mixing process: Oil phase pretreatment: 150 g of fat-soluble floral essence was mixed with 12 g of modified sophorolipids and dynamically stirred at 45° C. for 25 minutes to form an oil phase mixture.
[0057] Preparation of aqueous phase: Disperse 6 g of enzymatically hydrolyzed lecithin in 781.9 g of deionized water, add 50 g of propylene glycol, stir thoroughly to dissolve, adjust the pH value of the aqueous phase mixture to 6.5, and then cool the aqueous phase mixture to 20°C for use.
[0058] Step 3: Emulsification step: Colostrum Formation: The oil phase mixture obtained from the pretreatment was mixed with the aqueous phase mixture at a volume ratio of 1:3, followed by a three-stage gradient high-pressure homogenization process. Homogenization parameters were: Level 1 homogenization pressure of 75 MPa, two cycles; Level 2 homogenization pressure of 45 MPa, two cycles; Level 3 homogenization pressure of 25 MPa, one cycle. Immediately following homogenization, pulsed negative pressure degassing was performed at a negative pressure of -0.07 MPa and a pulse frequency of 1 Hz.
[0059] Ultrafine dispersion: After the three-stage gradient high-pressure homogenization process to form colostrum, add 0.1g of nano zinc oxide and continue ultrasonic dispersion treatment. The ultrasonic power density is controlled at 250W / cm 2 The emulsification step was carried out in a controlled production environment that met the requirements.
[0060] Step 4: Optional processing steps: The turbidity and particle size D50 of the intermediate product were detected online. In this embodiment, the test results were: turbidity 15 NTU, particle size D50 70 nm, both within the qualified range.
[0061] The qualified intermediate product was filtered through a 100-mesh metal filter, and the filtration flow rate was controlled at 0.5m 3 / h, the filtration pressure difference is 0.05MPa.
[0062] If the online test fails, feed, filter and secondary emulsification treatment are performed according to the method described.
[0063] Step 5: Final inspection and warehousing steps: The filtered product underwent accelerated stability testing and nitrogen-filled packaging, and all indicators met the requirements. The final product had a pH of 6.5, and residual oxygen in the packaging was less than or equal to 0.5%. The dielectric constant fluctuation met the requirements after 100 days of storage. The product also had a clear and transparent appearance.
[0064] Example 3 This embodiment provides a preparation method for a transparent microemulsification essence, using the upper limit parameters of the range.
[0065] Prepare 1000g of transparent micro-emulsifying essence, the components of which are calculated by mass percentage: Fat-soluble fruity flavor (acid value 1.5mgKOH / g, peroxide value 0.3mmol / kg): 25%; Modified sophorolipids: 1.8%; Enzymatically hydrolyzed lecithin: 1.2%; Propylene glycol: 8%; Nano zinc oxide: 0.03%; Deionized water: 63.97%.
[0066] The preparation steps are as follows: Step 1: Additive selection steps: The selected fat-soluble fruit flavoring ingredients were inspected to ensure their peroxide values met the requirements. Modified sophorolipids and enzymatically hydrolyzed lecithin were inspected to ensure their total microbial counts met the requirements. The above components were weighed according to the recipe. All raw materials met the pesticide residue limit requirements.
[0067] Step 2: Pre-mixing process: Oil phase pretreatment: 250 g of fat-soluble fruit flavor was mixed with 18 g of modified sophorolipid, and the mixture was dynamically stirred at 55° C. for 35 minutes to form an oil phase mixture.
[0068] Preparation of aqueous phase: Disperse 12 g of enzymatically hydrolyzed lecithin in 639.7 g of deionized water, add 80 g of propylene glycol, stir thoroughly to dissolve, adjust the pH value of the aqueous phase mixture to 7.5, and then cool the aqueous phase mixture to 25°C for use.
[0069] Step 3: Emulsification step: Colostrum Formation: The oil phase mixture obtained from the pretreatment was mixed with the aqueous phase mixture at a volume ratio of 1:5, followed by a three-stage gradient high-pressure homogenization process. Homogenization parameters were: Level 1 homogenization pressure of 85 MPa, three cycles; Level 2 homogenization pressure of 55 MPa, three cycles; Level 3 homogenization pressure of 35 MPa, two cycles. Immediately following homogenization, pulsed negative pressure degassing was performed at a negative pressure of -0.09 MPa and a pulse frequency of 3 Hz.
[0070] Ultrafine dispersion: After the three-stage gradient high-pressure homogenization treatment to form colostrum, add 0.3g nano zinc oxide and continue ultrasonic dispersion treatment. The ultrasonic power density is controlled at 350W / cm 2 The emulsification step was carried out in a controlled production environment that met the requirements.
[0071] Step 4: Optional processing steps: The turbidity and particle size D50 of the intermediate product were detected online. In this embodiment, the test results were: turbidity 25 NTU, particle size D50 90 nm, both within the qualified range.
[0072] The qualified intermediate product was filtered through a 100-mesh metal filter, and the filtration flow rate was controlled at 1.2 m 3 / h, the filtration pressure difference is 0.15MPa.
[0073] If the online test fails, feed, filter and secondary emulsification treatment are performed according to the method described.
[0074] Step 5: Final inspection and warehousing steps: The filtered product underwent accelerated stability testing and nitrogen-filled packaging, and all indicators met the requirements. The final product had a pH of 7.5, and residual oxygen in the packaging was less than or equal to 0.5%. The dielectric constant fluctuation met the requirements after 100 days of storage. The product also had a clear and transparent appearance.
[0075] Comparative Example 1: Compared with Example 1, the difference is: The formula does not contain enzymatic lecithin (original dosage 0.9%) and nano zinc oxide (original dosage 0.02%). To maintain the total weight unchanged, the amount of deionized water was increased from 71.08% to 72.00%.
[0076] In step 2, the pH of the aqueous phase was not adjusted to 7.0. The pH of the aqueous phase depended on the natural state of the enzymatically hydrolyzed lecithin (removed here) and propylene glycol dissolved in deionized water. All other steps were the same as in Example 1.
[0077] Comparative Example 2: Compared with Example 1, the difference is: The fat-soluble citrus flavor raw material used in step 1 has a peroxide value of 1.8 mmol / kg (0.2 mmol / kg in Example 1, and required to be less than or equal to 0.5 mmol / kg).
[0078] In step 5, the final inspection and storage step, the product is not packed with nitrogen, but is packed in a normal air environment. The rest is the same as in Example 1.
[0079] Comparative Example 3: Compared with Example 1, the difference is: In the colostrum formation in step 3, a three-stage gradient high-pressure homogenization process is not used, but a single-stage high-pressure homogenization process is used, with the homogenization pressure set at 50 MPa and 5 cycles.
[0080] In the colostrum formation in step 3, pulsed negative pressure degassing was not performed after the homogenization treatment.
[0081] In step 4, no online turbidity and particle size testing of the intermediate product is performed, and therefore no selective treatment (such as addition of polyglycerol ricinoleate and secondary emulsification) based on the test results is performed. All materials treated in step 3 are directly subjected to subsequent filtration (if any). All other steps are the same as in Example 1.
[0082] Comparative Example 4: Compared with Example 1, the difference is: In step 1, the additive selection step, the raw materials used were not specifically tested for pesticide residues to ensure that the content was less than or equal to 0.01 mg / kg, but regular commercially available raw materials were used.
[0083] The emulsification step in step 3 is carried out in a normal production workshop environment, without special control of the residual microorganisms on the surface of the equipment (which may be higher than 10 CFU / cm 2 ) and the conductivity of the process water (which may be higher than 5μS / cm).
[0084] In step 4, the step of filtering the qualified intermediate product (or not tested according to comparative example 3) through a 100-mesh metal filter was omitted. The rest was the same as in Example 1.
[0085] Experiment 1: Evaluation of the effects of specific emulsification systems and pH control on the physical stability and appearance of microemulsion flavors Experimental steps: Sample preparation: Samples were prepared according to the formulations and processes of Example 1, Example 2, and Example 3, and were labeled as Group 1.1, Group 1.3, and Group 1.5, respectively.
[0086] Following the design of Comparative Example 1, i.e., based on the formulations and processes of Examples 1, 2, and 3, respectively, except that enzymatically hydrolyzed lecithin and nano-zinc oxide were omitted from each formulation (their weights were supplemented with deionized water), and pH adjustment was not performed during the aqueous phase pretreatment step. Corresponding samples were prepared and labeled Group 1.2 (corresponding to Example 1), Group 1.4 (corresponding to Example 2), and Group 1.6 (corresponding to Example 3).
[0087] Initial status evaluation (0 days): Appearance observation: Place the freshly prepared samples of each group (Group 1.1 to Group 1.6) in a clean, transparent colorimetric tube and observe their clarity and transparency with the naked eye under good light. Record the presence of turbidity, opalescence, stratification, or precipitation.
[0088] Turbidity measurement: Using a calibrated turbidimeter, take an appropriate amount of thoroughly mixed sample and measure its turbidity value (NTU) according to the instrument operating procedures. Repeat the measurement three times for each sample and record the average value.
[0089] Particle Size Analysis: Using a dynamic light scattering particle size analyzer, take an appropriate amount of sample (dilute with deionized water that meets the instrument's requirements, if necessary) and determine its average particle size (D50) and polydispersity index (PDI, if provided by the instrument). Repeat the measurement three times for each sample and record the average value.
[0090] Accelerated stability test: Each sample group was divided into two parts and sealed separately. One part was stored at room temperature (25±2℃, protected from light), and the other part was placed in a constant temperature incubator (40±2℃, protected from light) for accelerated aging test.
[0091] Remove samples at set time points (e.g., day 7, day 15, day 30). Samples stored at 40°C must first be returned to room temperature.
[0092] Repeat the appearance observation and turbidity measurement in step 2. Particle size analysis can be performed at the end of the experiment (e.g., day 30), or at additional intermediate measurement points as needed.
[0093] Table 1: Physical stability and appearance evaluation data of microemulsion flavor Sample group number Initial appearance (0 days) Initial turbidity (NTU, 0 days) Initial D50 (nm, 0 days) Appearance after 30 days (25℃) Turbidity after 30 days (NTU, 25℃) D50 after 30 days (nm, 25℃) Appearance after 30 days (40℃) Turbidity after 30 days (NTU, 40℃) D50 after 30 days (nm, 40℃) Group 1.1 Clear and transparent, no opalescence 18.5 78 Clear and transparent, no obvious changes 19.2 80 Clear and transparent, slightly opalescent 23.8 85 Group 1.2 Slightly opalescent, slightly turbid 45.3 185 Obvious turbidity, with trace sediment at the bottom 68.7 250 Severe turbidity, obvious stratification 155.0 Greater than 500 (or unmeasurable) Group 1.3 Clear and transparent, no opalescence 16.2 72 Clear and transparent, no obvious changes 17.0 75 Clear and transparent, slightly opalescent 21.5 81 Group 1.4 Obvious opalescence, relatively turbid 52.8 210 Turbidity increases, and sediment is visible 81.3 310 Severe stratification, obvious oil-water separation Greater than 200 (or unmeasurable) N / A Group 1.5 Clear and transparent, no opalescence 23.1 88 Clear and transparent, no obvious changes 24.5 91 Clear and transparent, slightly opalescent 29.3 98 Group 1.6 Slightly opalescent, with visible graininess 60.1 245 Severe turbidity, with a lot of sediment at the bottom 110.5 380 Severe demulsification, oil phase floating Greater than 200 (or unmeasurable) N / A Summary of experimental results and mechanism analysis: The experimental results clearly demonstrate that samples from Groups 1.1, 1.3, and 1.5, i.e., transparent microemulsion flavors prepared according to the technical solutions of the present invention, all exhibited an excellent clear and transparent appearance in their initial state, with low turbidity and a small, uniform average particle size. More importantly, after 30 days of accelerated aging storage at room temperature and 40°C, these samples showed minimal changes in physical stability and appearance. Only a slight increase in turbidity or opalescence was observed under accelerated conditions, while the overall structure remained intact. This fully demonstrates the effectiveness of the specific component combinations and process parameters described in this invention for constructing highly stable, transparent microemulsion systems.
[0094] In contrast, samples in Groups 1.2, 1.4, and 1.6 exhibited high turbidity and large particle size in their initial state, due to the lack of enzymatic lecithin and nano-zinc oxide in the formula, and the lack of precise control of the aqueous phase pH. Their appearance showed varying degrees of turbidity or opalescence. In subsequent stability tests, the aging rate of these comparative samples was significantly accelerated, especially under high temperature conditions of 40°C. Severe turbidity, stratification, precipitation, and even demulsification were common. Their turbidity increased sharply, and the particle size increased significantly or could not be accurately measured due to system damage. This reveals that the stability of the microemulsion system is greatly reduced after the loss of key components and key process control points.
[0095] This experimental result is highly consistent with the technical concept of the present invention. The present invention uses a modified sophorolipid and enzymatically hydrolyzed lecithin compound as the core emulsifier, based on the complementarity of the two in terms of hydrophilic-lipophilic balance and molecular structure. This compound system can form a more tightly arranged, more stable and elastic interfacial film at the oil-water interface, thereby effectively reducing the interfacial energy and promoting the formation of an O / W microemulsion with smaller particle size and more uniform distribution.
[0096] Experiment 2: Evaluation of the effects of raw material quality control and antioxidant measures on the chemical stability and aroma retention of microemulsion flavors Experimental steps: Sample preparation: Samples were prepared according to the formulations and processes of Examples 1, 2, and 3, and labeled as Group 2.1, Group 2.3, and Group 2.5, respectively. These samples all used a flavor base that met the low peroxide value requirements of the present invention and were packaged in a nitrogen-filled manner.
[0097] Following the design of Comparative Example 2, which is based on the formulations and processes of Examples 1, 2, and 3, respectively, but using a flavor base with a peroxide value significantly higher than the preferred range described herein (for example, using the same type of flavor base as in the Examples but with a peroxide value of 1.5-2.0 mmol / kg), and omitting nitrogen flushing during the final packaging step, but instead packaging under normal air, corresponding samples were prepared and labeled Group 2.2 (corresponding to Example 1), Group 2.4 (corresponding to Example 2), and Group 2.6 (corresponding to Example 3).
[0098] Initial status evaluation (0 days): Peroxide Value (PV) Determination: Take freshly prepared samples from each group (Groups 2.1 to 2.6) and determine their initial PV according to standard methods (e.g., GB5009.227). Repeat the measurement 2-3 times for each sample and record the average value.
[0099] Aroma Evaluation: Invite 3-5 trained professional aroma assessors to conduct independent sensory evaluations of each group of fresh samples, recording the aroma's main characteristics, intensity, purity, and the presence of any unpleasant odors.
[0100] Accelerated aging test: Take an appropriate amount of samples from each group, seal them, and place them in a constant temperature incubator at 40±2℃ and store them away from light for 90 days.
[0101] Evaluation of condition after aging (90 days): Peroxide Value (PV) Determination: Remove the aged sample and allow it to return to room temperature. Determine its PV using the standard method. Repeat the measurement 2-3 times for each sample and record the average value.
[0102] Aroma Evaluation: The same professional aroma assessors were invited to conduct independent sensory evaluations of the aged samples. Changes in aroma characteristics, attenuation of intensity, decrease in purity, and any new unpleasant odors (such as rancid or stale aromas) were recorded.
[0103] Table 2: Evaluation data of chemical stability and aroma retention of microemulsion flavor Sample group number Initial flavor base PV Initial sample PV (0 day) Initial aroma description (0 days) Sample PV after 90 days (40℃) Aroma description after 90 days (40℃) Group 2.1 0.2 0.28 Fresh citrus fragrance, pure, no odor 2.1 The main citrus aroma still exists, slightly dull, with no obvious odor Group 2.2 1.8 1.95 Citrus scent, but a little greasy, barely acceptable 10.5 Obvious rancid oil smell, citrus aroma is almost covered, and the aroma is seriously deteriorated Group 2.3 0.15 0.22 Elegant floral fragrance, fresh and natural 1.8 The main body of the floral fragrance is clear, the intensity is slightly reduced, and there is no unpleasant odor Group 2.4 1.7 1.88 Floral fragrance, but with a slightly stale background, the aroma is not fresh enough 9.8 The floral aroma is seriously distorted, accompanied by a significant pungent and sour smell, which is unacceptable Group 2.5 0.3 0.35 Sweet and fruity, full and pleasant 2.5 The fruity characteristics are still there, the sweetness is slightly reduced, and the overall taste is acceptable. Group 2.6 1.9 2.10 Fruity, but not fresh enough, with a hint of unpleasant odor molecules 11.2 The fruity aroma has almost disappeared, replaced by a strong smell of oil and unpleasant chemical smell Summary of experimental results and mechanism analysis: The experimental results significantly demonstrate the crucial role of raw material quality control and antioxidant measures in maintaining the chemical stability and aroma quality of microemulsifier flavors. Samples in Groups 2.1, 2.3, and 2.5, prepared using a flavor base with a low initial peroxide value and packaged in nitrogen-filled packaging, showed relatively small increases in peroxide value after 90 days of high-temperature accelerated aging. While the aroma profile may have slightly changed, the main aroma was maintained, with no significant degradation. This demonstrates that the measures employed in this invention can effectively slow the oxidative degradation of microemulsifier flavors.
[0104] In stark contrast, samples in Groups 2.2, 2.4, and 2.6, due to the use of flavor bases with high initial peroxide values and the lack of nitrogen filling, had initially high PV values. During accelerated aging, these PV values rose sharply, far exceeding acceptable levels. Sensory evaluation results echoed this finding, showing that these comparative samples exhibited significant aroma deterioration after aging, including unpleasant odors such as rancid oil and staleness, almost completely destroying their original characteristic aroma. This directly demonstrates that neglecting initial raw material quality control and lacking effective antioxidant measures can lead to a sharp decline in product chemical stability and a loss of aroma quality.
[0105] The technical advantage of this invention lies in its forward-looking quality control concept. The peroxide value (PV) in a flavor base is a key indicator of its initial oxidation level. A low PV indicates a low content of primary oxidation products, such as hydroperoxides, generated by the oxidation of unsaturated fatty acids or terpenes. These primary oxidation products are not only inherently unstable and prone to further decomposition to produce small molecules with unpleasant odors, such as aldehydes, ketones, and acids, but they also trigger free radical chain reactions, accelerating subsequent oxidation processes.
[0106] Experiment 3: Evaluation of the Effect of Refined Preparation Process on the Uniformity and Production Stability of Microemulsified Flavor Experimental steps: Sample preparation: Samples were prepared according to the formulations and processes of Examples 1, 2, and 3, with three independent batches prepared under each condition (e.g., labeled as Groups 3.1A, 3.1B, and 3.1C; Groups 3.3A, 3.3B, and 3.3C; and Groups 3.5A, 3.5B, and 3.5C). These samples were prepared using a three-stage gradient high-pressure homogenization process, pulsed negative pressure degassing, online quality monitoring, and selective reprocessing.
[0107] Comparative Example 3 was designed based on the formulations of Examples 1, 2, and 3, except that the homogenization step was changed to a single-stage high-pressure homogenization (e.g., 50 MPa, 5 cycles). Pulsed negative pressure degassing was omitted, and online turbidity and particle size testing of the intermediate product, along with potential reprocessing, was omitted. Similarly, three independent batches were prepared under each condition (e.g., labeled as Groups 3.2A, 3.2B, and 3.2C; Groups 3.4A, 3.4B, and 3.4C; and Groups 3.6A, 3.6B, and 3.6C).
[0108] Initial status evaluation (0 days): Appearance observation (bubbles): Place freshly prepared samples from each batch (Group 3.1A to Group 3.6C) in clean, transparent colorimetric tubes. Carefully observe whether there are any visible residual bubbles in the samples and record the amount of bubbles (e.g., none, trace, small amount, or large amount).
[0109] Turbidity measurement: Using a calibrated turbidimeter, measure the turbidity value (NTU) of each batch of samples. Repeat the measurement three times for each batch of samples and record the average value.
[0110] Particle Size Analysis: Use a dynamic light scattering particle size analyzer to determine the average particle size (D50) and polydispersity index (PDI, if available). Repeat the measurement three times for each batch of samples, and record the average value.
[0111] Data analysis and batch-to-batch consistency assessment: Calculate the mean and standard deviation of turbidity and D50 obtained under each process condition (e.g., group 3.1, including batches 3.1A, 3.1B, and 3.1C) to assess batch-to-batch consistency.
[0112] For the comparative samples, since there was no online monitoring or rework mechanism, the quality of their final products directly reflected the simplified process. For the example samples, their online monitoring and selective rework mechanism (although rework was not specifically triggered in this experimental design, the existence of this mechanism itself is part of the process) is intended to ensure the qualified rate and consistency of the final products.
[0113] Table 3: Data on the impact of different preparation processes on the initial properties and batch consistency of microemulsion flavors Sample group number (batch) Appearance bubbles (0 days) Initial turbidity (NTU, 0 days) Initial D50 (nm, 0 days) Group 3.1A none 18.1 77 Group 3.1B trace 19.0 80 Group 3.1C none 18.6 79 Group 3.1 (mean ± SD) Trace / none 18.57±0.45 78.67±1.53 Group 3.2A More 55.3 190 Group 3.2B Small amount 68.1 235 Group 3.2C More 61.5 210 Group 3.2 (mean ± SD) More / less 61.63±6.40 211.67±22.55 Group 3.3A none 15.8 71 Group 3.3B none 16.5 73 Group 3.3C trace 16.1 72 Group 3.3 (mean ± SD) Trace / none 16.13±0.35 72.00±1.00 Group 3.4A Small amount 62.7 220 Group 3.4B More 75.0 270 Group 3.4C Small amount 69.3 240 Group 3.4 (mean ± SD) Small amount / large amount 69.00±6.16 243.33±25.17 Group 3.5A none 22.5 87 Group 3.5B trace 23.8 90 Group 3.5C none 23.0 89 Group 3.5 (mean ± SD) Trace / none 23.10±0.66 88.67±1.53 Group 3.6A More 70.2 255 Group 3.6B Small amount 81.9 300 Group 3.6C More 77.4 280 Group 3.6 (mean ± SD) More / less 76.50±5.92 278.33±22.55 Summary of experimental results and mechanism analysis: The results of this test clearly demonstrate the significant improvement in the quality uniformity and production stability of microemulsion flavors through refined preparation processes. Using the three-stage gradient high-pressure homogenization, pulsed negative pressure degassing, and integrated online quality monitoring and selective rework mechanisms described in this invention (e.g., Groups 3.1, 3.3, and 3.5), each batch of samples produced exhibited low initial turbidity and a small average particle size, with minimal standard deviation between batches. This demonstrates highly consistent product characteristics and a stable and controllable production process. Furthermore, virtually no residual bubbles were observed in these samples, ensuring the product's excellent appearance.
[0114] In contrast, the comparative samples (e.g., Groups 3.2, 3.4, and 3.6) using a simplified process, due to the use of a single-stage high-pressure homogenizer without degassing, and the lack of online monitoring and rework quality assurance, exhibited significantly higher turbidity and particle size than the example samples, and significantly increased batch-to-batch variability (standard deviation). This indicates that the simplified process struggles to consistently achieve the desired microemulsification effect, resulting in poor product quality consistency. Furthermore, a high number of residual bubbles were commonly observed in the comparative samples, impacting the product's visual quality and potential physical stability.
[0115] The advantageous mechanism of the process of the present invention lies in its multi-faceted synergistic effects. First, the three-stage gradient high-pressure homogenization achieves a more gentle and efficient crushing and refinement of the oil droplets by applying shear force step by step from high pressure to low pressure. The high-pressure stage is mainly responsible for coarse crushing, while the subsequent lower pressure stages help to further reduce the particle size and optimize the particle size distribution, avoiding local overheating that may be caused by a single excessive energy input or causing excessive shearing of the already formed tiny droplets and unnecessary aggregation, thereby more stably obtaining nano-scale droplets within the target range. Secondly, the pulsed negative pressure degassing technology is implemented immediately after each stage of homogenization. Its mechanism is to use the negative pressure environment to promote the rapid precipitation and removal of tiny bubbles dissolved in the liquid or involved due to shearing.
[0116] Experiment 4: Evaluation of the impact of comprehensive quality and safety assurance measures on the purity and safety of microemulsified flavors Experimental steps: Sample preparation: Samples were prepared according to the formulations and processes of Examples 1, 2, and 3, and are labeled Group 4.1, Group 4.3, and Group 4.5, respectively. The preparation of these samples strictly adhered to the quality and safety measures described in this invention, including the use of raw materials screened for pesticide residues, emulsification in a cleanliness-controlled environment, the use of process water with acceptable conductivity, and precision filtration of the final product.
[0117] Following the design of Comparative Example 4, which is based on the formulations and processes of Examples 1, 2, and 3, key quality and safety controls were omitted or relaxed during the preparation process: Regular, commercially available raw materials that had not been screened for specific pesticide residues were used; emulsification was performed in a standard workshop environment, without specific controls for residual microorganisms on equipment surfaces or the conductivity of process water; and the final product was not subjected to a 100-mesh metal filter for precision filtration. Corresponding samples were prepared and labeled Group 4.2 (corresponding to Example 1), Group 4.4 (corresponding to Example 2), and Group 4.6 (corresponding to Example 3).
[0118] Initial status evaluation (0 days): Microbiological testing: Take an appropriate amount of freshly prepared samples from each group (Groups 4.1 to 4.6) and, under aseptic conditions, perform a total aerobic bacterial count (CFU / g or CFU / mL) according to national standards or pharmacopoeia methods. Perform the test in parallel for each sample, and record the average value.
[0119] Visible impurities inspection: Place an appropriate amount of sample in a clean, transparent container. Observe carefully with the naked eye under good lighting conditions to check for insoluble particles, flocculent matter, or other visible foreign matter. Observation can be supplemented with a low-power microscope, and record the observation results.
[0120] Record and compare: Record the actual conductivity of process water during sample preparation (expected ≤ 5 μS / cm) and the monitoring results of microbial residues on the surface of production equipment (expected ≤ 10 CFU / cm 2 ).
[0121] For comparative samples, since no special control is performed, the general conductivity range of the conventional process water used (usually higher than 5μS / cm) and the general microbial background level of the general workshop environment can be recorded as a reference.
[0122] Table 4: Data on the impact of different quality safety control levels on the purity of microemulsifier essence Sample group number Pesticide residue control in raw materials Production environment control Finished product filtration Total number of microorganisms (CFU / g, 0 day) Visible impurities (0 days) Group 4.1 yes Yes (high cleanliness) Yes (100 mesh) 15 No obvious insoluble matter or foreign matter was found Group 4.2 No (regular) No (ordinary workshop) no 280 Occasionally tiny particles are seen, slightly impure Group 4.3 yes Yes (high cleanliness) Yes (100 mesh) 12 No obvious insoluble matter or foreign matter was found Group 4.4 No (regular) No (ordinary workshop) no 350 A small amount of fine suspended matter can be seen Group 4.5 yes Yes (high cleanliness) Yes (100 mesh) 18 No obvious insoluble matter or foreign matter was found Group 4.6 No (regular) No (ordinary workshop) no 310 There is a small amount of sediment at the bottom that is barely noticeable Summary of experimental results and mechanism analysis: The results of this experiment strongly demonstrate the critical role of the comprehensive quality and safety assurance measures described in this invention in enhancing the purity and potential safety of transparent microemulsified essences. Samples from Groups 4.1, 4.3, and 4.5, thanks to rigorous quality control across multiple stages, including raw material screening, production environment control, and finished product processing, had significantly lower total microbial counts than the control samples, and their appearance showed no obvious visible impurities, demonstrating a higher degree of purity. This is directly attributable to systematic risk prevention and control measures.
[0123] In contrast, samples in Groups 4.2, 4.4, and 4.6, due to a lack of targeted raw material pesticide residue screening (increasing the potential risk of chemical contaminants), production in an environment with less stringent cleanliness controls (increasing the chance of microbial contamination), and the omission of the final precision filtration step (failure to remove tiny particles or aggregates that may have been introduced during the production process), had significantly higher total microbial counts and exhibited varying degrees of visible impurities or impurities. These discrepancies highlight the need for comprehensive quality and safety control throughout the entire supply chain.
[0124] This invention utilizes a multi-layered approach to ensuring product purity and safety. First, auditing raw material suppliers and controlling specific indicators in key ingredients like flavors (such as the pesticide residues indirectly reflected in this example) are the first line of defense in mitigating the introduction of harmful substances at the source. Second, rigorous monitoring of the cleanliness of the emulsification production environment, including controlling microbial residues on equipment surfaces and using high-purity process water (such as low-conductivity deionized water), minimizes the chance of contamination from external microorganisms and inorganic / organic impurities during the production process, creating the foundation for producing products with a low microbial load.
[0125] 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 transparent micro-emulsification essence, characterized in that: The components are as follows by mass percentage: Fragrance base 15-25%; Modified sophorolipids 1.2-1.8%; Enzymatic lecithin 0.6-1.2%; Deionized water 65-75%; Propylene glycol 5-8%; Nano zinc oxide 0.01-0.03%.
2. A transparent micro-emulsifier essence according to claim 1, characterized in that The flavor base is selected from at least one of fat-soluble citrus flavors, fat-soluble floral flavors, or fat-soluble fruit flavors. The acid value of the flavor base is less than or equal to 2.0 mgKOH / g, and the peroxide value is less than or equal to 0.5 mmol / kg.
3. A transparent micro-emulsifier essence according to claim 1, characterized in that: The pH value of the transparent micro-emulsifying essence is 6.5-7.
5. Food-grade nitrogen is filled into the transparent micro-emulsifying essence to form a protective atmosphere, wherein the oxygen content is less than or equal to 0.5%.
4. A method for preparing a transparent micro-emulsifying essence, applied to a transparent micro-emulsifying essence according to any one of claims 1 to 3, characterized in that: The following steps are involved: Step 1, the additive selection step, comprises: Raw materials must be inspected and accepted, with the peroxide value of the flavor base being less than or equal to 0.5mmol / kg, and the total microbial count of the emulsifier being less than or equal to 50CFU / g; adding an external additive, wherein the external additive comprises 5-8% propylene glycol and 0.01-0.03% nano zinc oxide; Step 2, a pre-mixing step, comprises: Oil phase pretreatment: dynamically mixing the flavor base and the modified sophorolipid at a temperature of 45-55° C. for 25-35 minutes to form an oil phase mixture; Preparation of aqueous phase: Disperse enzymatically hydrolyzed lecithin in deionized water, adjust the pH to 6.5-7.5, and cool the aqueous phase mixture to 20-25°C; Step 3, emulsification step, comprising: Colostrum formation: the oil phase mixture and the water phase mixture are mixed in a volume ratio of 1:3 to 1:5, and then subjected to a three-stage gradient high-pressure homogenization process; Ultrafine dispersion: After the colostrum is formed, the nano zinc oxide is added and ultrasonic dispersion is performed, wherein the ultrasonic power density is 250-350W / cm 2 , processing time is 4-6 minutes; Step 4, optional processing step, including: Online detection of turbidity and particle size of intermediate products, where the qualified range of turbidity is 15-25 NTU and the qualified range of particle size D50 is 70-90 nm; If the turbidity and particle size of the intermediate product are qualified, the intermediate product is filtered through a 100-mesh filter and then proceeds to step 5; If the turbidity or particle size test of the intermediate product fails, 0.3-0.5% of polyglycerol ricinoleate is added to the intermediate product, followed by filtering through a 100-mesh filter, and then returning the filtered product to step 3 for secondary emulsification treatment; Step 5: Final inspection and warehousing steps, including: The product was subjected to an accelerated stability test, wherein after 90 days of storage at 40°C, the peroxide value was less than or equal to 3.0 mmol / kg; The product is packed with nitrogen, wherein the nitrogen filling pressure is 0.10-0.15MPa, and the residual oxygen in the package is less than or equal to 0.3%.
5. A method for preparing a transparent micro-emulsifier essence according to claim 4, characterized in that: The three-stage gradient high-pressure homogenization treatment in step 3 includes: First-stage homogenization treatment, with a homogenization pressure of 75-85 MPa, and 2-3 cycles; Secondary homogenization treatment, with a homogenization pressure of 45-55 MPa, and 2-3 cycles; Three-stage homogenization treatment, with a homogenization pressure of 25-35 MPa and 1-2 cycles; In addition, after the homogenization treatment, a pulsed negative pressure degassing treatment is implemented, wherein the negative pressure range is -0.07 to -0.09 MPa and the pulse frequency is 1-3 Hz.
6. A method for preparing a transparent micro-emulsifier essence according to claim 4, characterized in that: The secondary emulsification treatment in step 4 includes increasing the homogenization pressure by 10-15%, and the nano zinc oxide is added within 5-8 minutes after the secondary homogenization treatment is completed.
7. A method for preparing a transparent micro-emulsifier essence according to claim 4, characterized in that: The additive selection step in step 1 further includes conducting a qualification review of the raw material supplier and conducting a pesticide residue test on the raw material, wherein the pesticide residue content is less than or equal to 0.01 mg / kg.
8. A method for preparing a transparent micro-emulsifier essence according to claim 4, characterized in that: The emulsification step in step 3 is carried out in a controlled production environment, and the controlled production environment monitoring includes: The residual microorganisms on the surface of the equipment are less than or equal to 10 CFU / cm 2 ; The conductivity of process water is less than or equal to 5μS / cm.
9. A method for preparing a transparent micro-emulsifier essence according to claim 4, characterized in that: The final inspection and warehousing step in step 5 further includes a 100-day storage verification of the nitrogen-filled packaged product, wherein the dielectric constant fluctuation is less than or equal to 0.
5.
10. The method for preparing a transparent micro-emulsifier essence according to claim 4, wherein: The specific parameters of the filtration operation through the 100-mesh filter in step 4 are: using a 100-mesh metal filter, the filtration flow rate is controlled at 0.5-1.2m 3 / h, the filtration pressure difference is 0.05-0.15MPa.