Pericarpium citri reticulatae soda water and preparation method thereof
Through gas-liquid phase collaborative stability technology and intelligent packaging system, the problem of flavor dissipation and sweet-acid ratio imbalance in tangerine peel soda water is solved, achieving the durability of flavor and accurate prediction of shelf life, and improving the quality stability and energy efficiency of the product.
Patent Information
- Application Number
- CN202510684620.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-26
- Publication Date
- 2025-08-08
AI Technical Summary
Traditional carbonated beverages have significant technical defects in the retention of volatile flavor ingredients. The flavor dissipation, sweet and sour ratio imbalance and insufficient shelf life prediction accuracy of the product leads to rapid attenuation of the aroma components and blurred taste levels during storage, making it difficult to meet consumer demand.
The gas-phase-liquid phase collaborative stability technology is used to embed tangerine peel essential oil molecules, combine the headspace protection of nitrogen/carbon dioxide mixed gas, and use core-shell controlled release microspheres to achieve the timing release of sour and sweetener, and track environmental parameters in real time through an intelligent packaging system, and optimize production energy consumption in combination with a closed-loop control process.
Effectively inhibit the dissipation and oxidative degradation of volatile ingredients, realize the durability of the aroma of tangerine peel, simulate the natural taste level of freshly soaked tangerine peel water, improve the reliability of shelf life prediction and product quality stability, and reduce energy consumption.
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Figure CN120436267A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of food processing, in particular to tangerine peel soda water and a preparation method thereof. Background Art
[0002] Traditional carbonated beverages have significant technical deficiencies in retaining volatile flavor components. Terpenes, which are rich in plant materials such as tangerine peel, can easily escape through the gas-liquid interface in a high-pressure carbonation system and undergo oxidation reactions with dissolved oxygen, causing the aroma components to decay rapidly during storage. Existing technologies typically use single encapsulation or static gas protection methods, but they cannot take into account the dual losses of physical escape and chemical degradation, and they do not solve the problem of diffusion rate imbalance caused by molecular weight differences between sweeteners and acidulants. As a result, the taste of the product gradually becomes blurred during the shelf life, making it difficult to meet consumer demand for flavor persistence.
[0003] In industrial production, the conflict between flavor stability and process energy efficiency is particularly prominent. Conventional dispersion processes rely on energy-intensive mechanical stirring, making it difficult to achieve uniform distribution of functional components. Variations in raw material batches further exacerbate quality fluctuations. Furthermore, traditional packaging lacks dynamic sensing of the storage environment, and shelf life predictions rely on empirical formulas that cannot accurately account for the impact of temperature and humidity fluctuations on the product, resulting in significant deviations in shelf life determinations. These shortcomings severely hinder the market competitiveness of high-value-added beverages like tangerine peel soda water. Summary of the Invention
[0004] In view of the deficiencies in the prior art, the present invention provides a tangerine peel soda water and a preparation method thereof, which solves the problems in the prior art of tangerine peel soda water such as flavor loss, unbalanced sweetness and sourness ratio, and insufficient shelf life prediction accuracy.
[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: a tangerine peel soda water and a preparation method thereof, comprising the following components by volume percentage: Tangerine peel extract 0.8-1.5% v / v Natural sweetener 5-7°Bx Acidulant 0.3-0.8% w / v Carbonated water balance Hydroxypropyl-β-cyclodextrin 0.02-0.05% w / v The headspace in the bottle is filled with nitrogen / carbon dioxide mixed gas with a volume ratio of 6:4-8:2 Time-controlled release microspheres containing an acid controlled release shell layer and a sweet controlled release core layer 0.3-0.8% w / w Mineral salts 0.06-0.15% w / v The bottle body is printed with pH-responsive ink, and the bottle cap is integrated with an NFC temperature and humidity sensor.
[0006] Preferably, the headspace mixed gas pressure is 0.10-0.20 MPa, and the residual oxygen content is ≤0.6% v / v.
[0007] Preferably, in the time-controlled release microspheres, the thickness of the acid-controlled release shell layer is 30-50 μm, and the particle size of the sweet-controlled release core layer is 20-60 μm.
[0008] Preferably, the mineral salt is a mixture of sodium bicarbonate, magnesium hydrogen phosphate and potassium chloride in a mass ratio of 5:2:1-7:3:1.
[0009] Preferably, the pH responsive ink comprises 0.05-0.15% w / v of methyl red and 0.02-0.08% w / v of bromocresol green.
[0010] A method for preparing tangerine peel soda water comprises the following steps: (a) Tangerine peel pretreatment and low-temperature extraction; (b) gas-liquid synergistic stabilization treatment; (c) Preparation of time-controlled release microspheres; (d) Mixing and chaotic dispersion; (e) Integration of aseptic filling and dynamic monitoring; (f) Closed-loop control of process parameters.
[0011] Preferably, in step (b): The molar ratio of hydroxypropyl-β-cyclodextrin to tangerine peel essential oil is 1:2-1:4, the stirring temperature is 35-45° C., and the stirring time is 90-150 min.
[0012] Preferably, in step (b): Gas replacement adopts two-stage filling, first injecting CO2 to a pressure of 0.05-0.10MPa, and then injecting N2 to a total pressure of 0.12-0.18MPa.
[0013] Preferably, in step (c): The acid controlled-release shell layer was coated using a fluidized bed with an inlet air temperature of 40-50°C, a HPMCP ethanol solution concentration of 8-12% w / v, and a spraying rate of 2-4 mL / min.
[0014] Preferably, in step (d): The ultrasonic dispersion parameters are: basic frequency 18-22 kHz, random perturbation amplitude 0.05-2.5 kHz, power 300-500 W, and time 4-8 min.
[0015] The present invention provides a tangerine peel soda water and a preparation method thereof, which has the following beneficial effects: 1. The present invention uses a gas-liquid phase collaborative stabilization technique to embed tangerine peel essential oil molecules into the cyclodextrin cavity, while simultaneously utilizing a nitrogen / carbon dioxide gas mixture for headspace protection, creating a dual-locking mechanism. This technology effectively inhibits the escape and oxidative degradation of volatile components, allowing the product to maintain its natural tangerine peel aroma throughout its shelf life, thus overcoming the bottleneck of traditional carbonated beverages that are prone to flavor decay.
[0016] 2. This invention utilizes core-shell controlled-release microspheres, which utilize gradient crosslinking and a shear-responsive structure, to achieve sequential release of the acidulant and sweetener. Upon consumption, the sourness first activates the taste buds, followed by the gradual sweetness, mimicking the natural texture of freshly brewed tangerine peel water and resolving the technical challenge of an imbalance in the sweet-sour ratio over time.
[0017] 3. This invention integrates an NFC chip and pH-responsive ink in an intelligent packaging system, enabling real-time tracking of environmental parameters and product status through dual-signal coupling. Combined with a temperature-humidity correction model, this system dynamically optimizes shelf life prediction logic, significantly improving the reliability of shelf life determination and providing consumers with intuitive quality judgment.
[0018] 4. This invention utilizes a closed-loop control process to dynamically adjust key parameters based on online test data. Combined with ultrasonic chaotic dispersion technology, this reduces energy consumption while improving component distribution uniformity. This system effectively mitigates the impact of raw material batch variations on product quality, creating an environmentally friendly, low-cost, and highly stable manufacturing model. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 A diagram showing the steps of the method of the present invention. DETAILED DESCRIPTION
[0020] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings in the present specification. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0021] Please see the attached Figure 1 The embodiment of the present invention provides a tangerine peel soda water, comprising the following components by volume percentage: Tangerine peel extract 0.8-1.5% v / v Natural sweetener 5-7°Bx Acidulant 0.3-0.8% w / v Carbonated water balance Hydroxypropyl-β-cyclodextrin 0.02-0.05% w / v The headspace in the bottle is filled with nitrogen / carbon dioxide mixed gas with a volume ratio of 6:4-8:2 Time-controlled release microspheres containing an acid controlled release shell layer and a sweet controlled release core layer 0.3-0.8% w / w Mineral salts 0.06-0.15% w / v The bottle body is printed with pH-responsive ink, and the bottle cap is integrated with an NFC temperature and humidity sensor.
[0022] Example 1 Raw materials and process parameters Tangerine peel pretreatment Tangerine peel crushing mesh: 500 mesh Extraction temperature: 90℃ Tangerine peel extract concentration: 1.2% v / v Gas-liquid synergistic stabilization Hydroxypropyl-β-cyclodextrin (HP-β-CD): 0.035% w / v N2 / CO2 mixing ratio: 7:3 Headspace pressure: 0.15MPa Time-controlled release microspheres Acid controlled release shell thickness: 40 μm Sweet controlled release core particle size: 40μm HPMCP spraying rate: 3mL / min Mixing Ultrasonic fundamental frequency: 20kHz Random perturbation amplitude: 1.25kHz Dispersion time: 6 minutes Filling and monitoring Filling temperature: 7℃ CO2 gas capacity: 1.9vol Mineral salt ratio: sodium bicarbonate: magnesium hydrogen phosphate: potassium chloride = 6:2.5:1 Example 2 Raw materials and process parameters Tangerine peel pretreatment Tangerine peel crushing mesh size: 400 mesh (not limited by the claim, but must meet the lower limit of extraction efficiency) Extraction temperature: 85℃ Tangerine peel extract concentration: 0.8% v / v Gas-liquid synergistic stabilization HP-β-CD: 0.02% w / v N2 / CO2 mixing ratio: 6:4 Headspace pressure: 0.10MPa Time-controlled release microspheres Acid controlled release shell thickness: 30 μm Sweet controlled release core particle size: 20μm HPMCP spraying rate: 2mL / min Mixing Ultrasonic fundamental frequency: 18kHz Random perturbation amplitude: 0.05kHz Dispersion time: 4 minutes Filling and monitoring Filling temperature: 5°C (not limited by the claims, but must meet the low temperature filling requirements) CO2 gas capacity: 1.6vol Mineral salt ratio: sodium bicarbonate: magnesium hydrogen phosphate: potassium chloride = 5:2:1 Example 3 Raw materials and process parameters Tangerine peel pretreatment Tangerine peel crushing mesh: 600 mesh Extraction temperature: 95℃ Tangerine peel extract concentration: 1.5% v / v Gas-liquid synergistic stabilization HP-β-CD: 0.05% w / v N2 / CO2 mixing ratio: 8:2 Headspace pressure: 0.20MPa Time-controlled release microspheres Acid controlled release shell thickness: 50 μm Sweet controlled release core particle size: 60μm HPMCP spraying rate: 4mL / min Mixing Ultrasonic fundamental frequency: 22kHz Random perturbation amplitude: 2.5kHz Dispersion time: 8 minutes Filling and monitoring Filling temperature: 8℃ CO2 gas capacity: 2.2vol Mineral salt ratio: sodium bicarbonate: magnesium hydrogen phosphate: potassium chloride = 7:3:1 Comparative Example 1 Compared with Example 1, the difference is: Hydroxypropyl-β-cyclodextrin (HP-β-CD) was removed and the unencapsulated tangerine peel extract was directly added.
[0023] Cancel the N2 / CO2 mixed gas headspace replacement and only use normal pressure air environment filling.
[0024] The remaining process parameters are exactly the same as those in Example 1.
[0025] Comparative Example 2 Compared with Example 1, the difference is: The headspace mixed gas was changed to pure CO2 (N2 / CO2 volume ratio = 0:10, which exceeds the range of 6:4-8:2 in the claims).
[0026] The CO2 gas capacity is increased to 2.5 vol (exceeding the upper limit of 1.6-2.2 vol in the claims).
[0027] The remaining process parameters are exactly the same as those in Example 1.
[0028] Comparative Example 3 Compared with Example 1, the difference is: The time-controlled release microsphere preparation step was omitted, and citric acid powder and erythritol were directly mixed (without forming a core-shell structure).
[0029] Ultrasonic dispersion cancels random frequency disturbances and uses only a fixed frequency of 20kHz.
[0030] The remaining process parameters are exactly the same as those in Example 1.
[0031] Comparative Example 4 Compared with Example 1, the difference is: Dynamic monitoring components are cancelled: pH response ink is not printed on the bottle body, and the bottle cap does not have an integrated NFC temperature and humidity sensor.
[0032] The mineral salt ratio is adjusted to sodium bicarbonate:magnesium hydrogen phosphate:potassium chloride = 9:1:1 (beyond the range of 5:2:1-7:3:1 in the claims).
[0033] The remaining process parameters are exactly the same as those in Example 1.
[0034] Comparative Example 5 Compared with Example 1, the difference is: Only a single technique of HP-β-CD embedding or N2 / CO2 mixed gas is retained: HP-β-CD embedding (0.035% w / v) was retained, but headspace gas replacement (exposure to air) was abolished.
[0035] Alternatively, the N2 / CO2 mixed gas headspace (7:3) was retained but HP-β-CD was removed.
[0036] The remaining process parameters are exactly the same as those in Example 1.
[0037] Test Example 1: Comparison of flavor retention and residual oxygen content Description of experimental steps Sample grouping: Experimental group: Example 1 (containing HP-β-CD embedding + N2 / CO2 mixed headspace) Control group: Comparative Example 1 (no embedding + air headspace) Comparative Example 2 (Pure CO2 headspace + over-limit gas capacity 2.5vol) Comparative Example 5 (retaining only HP-β-CD or only N2 / CO2 headspace) Storage conditions: Temperature: 25℃±1℃ Humidity: 60%±5%RH Store in the dark, and each group of samples was repeated 3 times (n=3).
[0038] Detection time point: 0 days (initial), 30 days, 60 days, and 90 days after filling.
[0039] Headspace gas chromatography (HS-GC) detection: Instrument: Agilent 7890B gas chromatograph equipped with FID detector parameter: Chromatographic column: HP-5 (30m×0.32mm×0.25μm) Inlet temperature: 250°C Column temperature program: 50°C (2 min) → 10°C / min → 200°C (5 min) Headspace injection: equilibrium temperature 80°C, equilibrium time 30 min operate: Take 2 mL of sample and inject it into the headspace bottle, seal it and then balance it.
[0040] Automatic sampling was performed and the peak areas of limonene and citral were integrated.
[0041] Retention rate calculation: Retention rate (%) = (peak area on day t / initial peak area) × 100 Residual oxygen detection: Instrument: LGA laser headspace analyzer parameter: Detection wavelength: 760nm (O2 characteristic absorption peak) Sampling frequency: 3 times / bottle, take the average value Experimental data table Table 1 Comparative data of flavor retention rate and residual oxygen content in Test Example 1 The rate of decrease in retention rate within the same group was nonlinear (e.g., Comparative Example 2 decreased by 18.3% between 30 and 60 days and by 16.6% between 60 and 90 days).
[0042] Fluctuations in residual oxygen levels (e.g., in Comparative Example 2, the oxygen level suddenly increased after 60 days, possibly due to changes in CO2 solubility) The limonene retention rate of Example 1 (81.3%) at 90 days was significantly higher than that of Comparative Example 1 (23.9%) and Comparative Example 5-B (47.8%).
[0043] Comparative Example 2 (excessive CO2) has a higher initial retention rate, but due to the high pressure, the packaging penetration is intensified and the attenuation is accelerated in the later stage.
[0044] When Comparative Example 5-A / B was used alone for embedding or headspace, the retention rate was between that of Example 1 and Comparative Example 1, proving that both the double locks are indispensable.
[0045] Test Example 2: Comparative Experiment on Dynamic Stability of Sweetness-Sourness Ratio and Sensory Evaluation Description of experimental steps Sample grouping: Experimental group: Example 1 (containing core-shell controlled-release microspheres + chaotic dispersion) Control group: Comparative Example 3 (direct mixing of sour / sweet powder + fixed frequency dispersion) Comparative Example 5-A (HP-β-CD encapsulation only, no microspheres) Comparative Example 5-B (N2 / CO2 headspace only, no microspheres) Storage conditions: Temperature: 25℃±1℃, humidity: 60%±5%RH, store away from light.
[0046] Each group of samples was repeated for 3 bottles (n=3), and the detection time points were: 0 days, 30 days, 60 days, and 90 days.
[0047] Electronic tongue detection: Instrument: Insent Electronic Tongue (Model TS-5000Z) Sensor configuration: Acid sensor (CA): sensitive to citric acid Sweetness sensor (GLU): sensitive to erythritol Test parameters: Sample pretreatment: Centrifuge (4000 rpm, 10 min) and take the supernatant Detection time: 120 seconds / sample, data acquisition frequency 10Hz Data processing: Sweetness-acid ratio (Brix / TA) = GLU response value (mV) / CA response value (mV) Fluctuation value = |Current sweetness-sourness ratio - Initial sweetness-sourness ratio| Sensory evaluation: Blind test design: 50 healthy subjects (25-45 years old) without taste disorders Scoring criteria: 1 point: Mixed sweet and sour taste without any layers 3 points: Sweet and sour can be distinguished but not obvious 5 points: Clear "sour → sweet" progression Testing process: The samples were randomly numbered and provided after being refrigerated at 4°C (10 mL / cup).
[0048] The subjects rinsed their mouths and tasted the food in turn, with an interval of 5 minutes.
[0049] Record the median score of each sample.
[0050] Experimental data table Table 2 Comparative data of sweetness-sourness ratio dynamic stability and sensory score of test example 2 The sweetness-sour ratio of Comparative Example 3 dropped suddenly at 30 days (1.85→1.62), and then gradually decreased after 60 days (1.41→1.28).
[0051] Sensory score fluctuations: Example 1 scored 4.1 points at 90 days, but Comparative Example 5-A scored 3.0 points during the same period (non-linear relationship).
[0052] Example 1: The sweet-sour ratio slowly decreased (Δ=0.09 after 90 days), and the sensory score was always >4 points, proving that the core-shell structure effectively delayed the imbalance.
[0053] Comparative Example 3: The uncontrolled release of sour / sweet ingredients diffused rapidly, with a Δ of 0.57 after 90 days and a sensory score collapse (1.7 points).
[0054] Comparative Example 5-A / B: The performance of the control group lacking synergistic effect is between Example 1 and Comparative Example 3, confirming the synergistic relationship between microspheres and encapsulation / headspace.
[0055] The sweet-sour ratio of Comparative Example 5-B at day 0 (1.83) was slightly higher than that of Example 1 (1.82), which may be due to the faster initial release of the unencapsulated sour components.
[0056] Test Example 3: Shelf Life Prediction Error and Color Indication Consistency Verification Experiment Description of experimental steps Sample grouping: Experimental group: Example 1 (containing NFC chip + pH response ink) Control group: Comparative Example 4 (no dynamic monitoring component) Storage conditions: High temperature and high humidity group: 40℃±1℃, 75%±3%RH Normal temperature group: 25℃±1℃, 60%±5%RH Each group of samples was repeated for 3 bottles (n=3), and the detection time points were: 0 days, 15 days, 30 days, and 60 days.
[0057] Shelf life prediction model: Example 1 Model: A temperature-humidity correction model based on the Arrhenius equation, combined with the following parameters: Reference conditions: 25°C / 60%RH, reference shelf life: 180 days Temperature coefficient Q 10 =2.8 (reaction rate doubles for every 10°C increase in temperature) Humidity correction factor β = 0.65 (for every 10% increase in humidity, the shelf life decay rate increases by 65%) Comparative Example 4 model: A conventional linear attenuation model is used, based only on the empirical temperature coefficient k=0.015 (without humidity correction).
[0058] Actual shelf life determination: Failure criteria: Flavor retention rate <70% (HS-GC detection of limonene and citral) Sweetness-sourness ratio fluctuation value>0.25 (electronic tongue detection) Visible precipitation or off-flavor (sensory evaluation) Testing frequency: Sampling and testing are carried out weekly until any failure criteria is triggered.
[0059] Color indication consistency check: Chromaticity analysis: Use a colorimeter to measure the Lab* value of the ink, divided into three stages: Yellow (pH 4.1-4.5): L85-90, a-5~0, b*70-80 Orange (pH 3.8-4.0): L75-80, a10-15, b*50-60 Red (pH 3.5-3.7): L 60-65, a 25-30, b* 30-40 pH verification: After sampling, use a pH meter to detect the actual value and compare it with the color stage.
[0060] Experimental data table Table 3 Comparison of shelf life prediction error and color indication The temperature-humidity correction model of Example 1 has a prediction error of ≤6% under high temperature and high humidity conditions, which is significantly better than the linear model of Comparative Example 4 (error>38%).
[0061] In Comparative Example 4, the predicted value under 75% RH conditions seriously deviates from the actual value (the error reaches 41.9%) because the influence of humidity is ignored.
[0062] In Example 1, the measured pH value at stage 3 (red) of the high temperature group was 3.6-3.7, which was basically consistent with the theoretical range (3.5-3.7), but there was an instrument error of ±0.1.
[0063] The measured pH value of stage 1 (yellow) in the normal temperature group was 4.2-4.4, which matched the theoretical value (4.1-4.5), but a single sample had a pH value of 4.4 (close to the upper limit).
[0064] In Example 1, at 25°C / 60% RH, one bottle has an actual shelf life of 181 days (predicted 180 days), with an error of +0.6%, reflecting the robustness of the model to batch differences.
[0065] In Comparative Example 4, the actual shelf life was 21.2% shorter than the predicted value in the room temperature group because humidity was not monitored, proving the necessity of humidity correction.
[0066] Test Example 4: Process Stability and Energy Consumption Comparison Experiment Description of experimental steps Sample grouping: Experimental group: Example 1 (closed-loop control process) Control group: Comparative example 5 (open-loop control, no feedback regulation) Production batch settings: Produce 10 batches (100L each) continuously and record the key parameters: HP-β-CD embedding efficiency (HPLC detection) Microsphere particle size distribution (D10 / D50 / D90) Ultrasonic dispersion energy consumption (kWh / kg microspheres) Detection method: Embedding rate detection: Three samples were randomly selected from each batch to test the limonene embedding efficiency (HPLC peak area integration method) Coefficient of variation (CV value) = (standard deviation / mean) × 100% Particle size analysis: Laser particle size analyzer (Malvern Mastersizer 3000) was used to measure the particle size distribution of microspheres. Span value = (D90-D10) / D50 Energy consumption monitoring: The power quality analyzer (Fluke435-II) records the real-time power during the ultrasonic dispersion stage. Unit energy consumption = total power consumption (kWh) / microsphere processing capacity (kg) Data collection: Production interval: 2 hours between each batch (equipment cooled to room temperature) Environmental control: Workshop temperature 25℃±2℃, humidity 50%±10% Experimental data table Table 4 Comparison of process stability and energy consumption The CV value of Example 1 fluctuates between 3.2% and 4.5% (affected by differences in raw material batches), but the fluctuation of Comparative Example 5 is greater (8.7% to 12.3%).
[0067] Energy consumption data: Example 1 is 0.48-0.55 kWh / kg, and Comparative Example 5 is 0.65-0.74 kWh / kg (due to the lack of chaotic dispersion optimization, energy consumption increased by 30-40%).
[0068] Comparison of key parameters: Particle size span: Example 1 has an average of 0.87 (range 0.79-0.95), reflecting uniform dispersion; The average value of Comparative Example 5 was 1.50 (range 1.34-1.63), with obvious agglomeration.
[0069] The maximum CV of Example 1 is 4.5%, which meets the quality control requirements (≤5%). The CV value of Comparative Example 5 is greater than 8%, which is beyond the acceptable range.
[0070] The CV value of Batch 7 of Comparative Example 5 increased suddenly (12.3%), which was due to the loss of control of the HP-β-CD addition rate due to the lack of closed-loop regulation.
[0071] The energy consumption of batch 5 in Example 1 was slightly higher (0.55 kWh / kg), which may be caused by grid voltage fluctuations.
[0072] A method for preparing tangerine peel soda water comprises the following steps: (a) Tangerine peel pretreatment and low-temperature extraction; Select 3-5 year old Xinhui dried tangerine peel with intact skin and plump oil chambers. After high-pressure water mist cleaning (0.3-0.5 MPa) to remove surface impurities, the peel is immediately placed in a liquid nitrogen quick freezer (-196°C) for 5-8 minutes to brittle the peel. The peel is then pulverized in an ultra-low temperature pulverizer under liquid nitrogen protection, maintaining the pulverization chamber temperature below -50°C for 15-20 minutes, yielding a 500-600 mesh ultrafine powder (specific surface area ≥8 m² / g). The powder and deionized water were put into the distillation kettle at a material-liquid ratio of 1:15, and a gradient heating strategy was adopted: preheating at 50°C for 10 minutes in the initial stage (to activate enzyme passivation), then raised to 90°C at 2°C / min and maintained for 2 hours. The distilled condensate was cooled in two stages (first stage 4°C, second stage -10°C), and then filtered through a 0.22μm ceramic membrane cross-flow filtration (transmembrane pressure difference 0.1-0.3MPa) to retain macromolecular colloidal substances, and finally a clear extract with an essential oil content of 0.8-1.5% was obtained.
[0073] (b) gas-liquid synergistic stabilization treatment; In a double-layer reactor, the extract was mixed with hydroxypropyl-β-cyclodextrin (HP-β-CD, degree of substitution 0.6-0.9) at a molar ratio of 1:3. Stirring was continued for 120 minutes using a double-ribbon stirrer (600-1000 rpm) and jacketed circulating water to control the temperature (35-45°C ± 1°C). Molecular dynamics simulation software (GROMACS) was used to optimize the encapsulation parameters and determine the optimal conformation of the encapsulated complex. Premixed gas (N₂ purity ≥99.99%; CO₂ food grade) was then introduced into the reactor top using a two-stage charging process: CO₂ was first introduced at a flow rate of 0.5 L / min to a pressure of 0.08 MPa, followed by N₂ at a flow rate of 1.2 L / min to a total pressure of 0.15 MPa. The gas ratio (6:4-8:2) was precisely controlled by a mass flow meter (Brooks SLA5850). The headspace oxygen content was monitored in real time by a laser gas analyzer (LGA-4500), and the automatic gas replenishment program was triggered when the oxygen content was >0.6%.
[0074] (c) Preparation of time-controlled release microspheres; Acid controlled-release shell: Using a fluidized bed spray coating system (Glatt GPCG2), citric acid powder (D50 = 40 μm, span ≤ 1.2) was placed in a fluidized bed with an inlet air temperature of 45°C ± 2°C and a bed pressure differential of 80-120 Pa. HPMCP was dissolved in 95% ethanol (10% w / v) and 0.1% polyethylene glycol 400 was added as a plasticizer. The product was sprayed through a two-fluid nozzle (1.2 mm aperture) at an atomization pressure of 0.2 MPa and a spray rate of 3 mL / min, forming a gradient cross-linked shell layer with a thickness of 30-50 μm (surface cross-linking degree 85% → core cross-linking degree 60%).
[0075] Sweet controlled-release core layer: Erythritol crystals (particle size 20-60 μm) were mixed with chitosan (degree of deacetylation ≥85%, 2.0% w / v)-sodium alginate (0.8% w / v) colloid in a 1:2 mass ratio and injected into a CaCl₂ solution (0.1 mol / L) for ionic crosslinking. Dynamic oscillation (frequency 5 Hz, amplitude 2 mm) was used for 30 minutes to form a three-dimensional network structure. The crosslink density was controlled using a rheometer (TA Instruments) at G' = 500-800 Pa.
[0076] (d) Mixing and chaotic dispersion; The embedding solution, microspheres (sour:sweet = 1:1.2 w / w), sodium bicarbonate (0.08% w / v), and mineral salts (sodium bicarbonate:magnesium hydrogen phosphate:potassium chloride = 6:2.5:1) were placed in a vacuum mixing tank (vacuum level -0.08 MPa). An ultrasonic dispersion system (Hielscher UP400St) was activated. The base frequency was set to 20 kHz, with superimposed random frequency perturbations (0.1-2.0 kHz, Poisson distribution λ = 1.0), a power density of 50 W / L, and a treatment time of 6 minutes. Particle size distribution was monitored using an online particle size analyzer (Malvern Insitec). Dispersion was terminated when D90 ≤ 80 μm and span value ≤ 1.0.
[0077] (e) Integration of aseptic filling and dynamic monitoring; An aseptic cold filling line (Krones filling system) was used, with the filling temperature controlled at 6°C ± 1°C. The CO2 volume was maintained at 1.8 vol ± 0.1 vol using an in-line density meter (Anton Paar DMA 4500). The bottle cap was injection-molded from PP (mold temperature 80°C) and embedded with an NFC chip (model NTAG216, 888 bytes of storage capacity). The chip was pre-programmed to record the production batch, timestamp, and environmental thresholds. The bottle was screen-printed with a pH-responsive ink: methyl red 0.1% w / v (dissolved in ethanol) and bromocresol green 0.05% w / v (dissolved in 0.1 mol / L NaOH). The ink was cured at 60°C ± 5°C, forming a 10-15 μm thick indicator layer.
[0078] (f) Closed-loop control of process parameters; Build a multivariable control model: Embedment rate feedback: The limonene embedding rate was detected every 15 minutes by online HPLC (Agilent 1260 Infinity II). When the detection value was lower than the set value (≥82%), the HP-β-CD addition program was triggered (addition speed 0.02-0.05 g / s).
[0079] Gas ratio adjustment: Based on the headspace oxygen content data, the N2 / CO2 mixing ratio is dynamically adjusted by a PID controller (proportional coefficient Kp=0.8, integral time Ti=120s), with an adjustment range of ±5%.
[0080] Energy consumption optimization: Ultrasonic power is dynamically adjusted based on real-time impedance analysis (LCR meter, Keysight E4980A) to maintain electroacoustic conversion efficiency ≥ 65%.
[0081] Shelf life prediction: Sensor data is uploaded to the cloud server every 30 minutes, and the remaining shelf life is predicted using an LSTM neural network model (hidden layer with 128 nodes), with an error compensation rate of ≤5%.
[0082] 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 tangerine peel soda water, characterized in that It includes the following components by volume percentage: Tangerine peel extract 0.8-1.5% v / v; Natural sweetener 5-7°Bx; Acidulant 0.3-0.8% w / v; Carbonated water balance; Hydroxypropyl-β-cyclodextrin 0.02-0.05% w / v; The headspace in the bottle is filled with a nitrogen / carbon dioxide mixture with a volume ratio of 6:4-8:2; Time-controlled release microspheres comprising an acid-controlled release shell layer and a sweet-controlled release core layer 0.3-0.8% w / w; Mineral salts 0.06-0.15% w / v; The bottle body is printed with pH-responsive ink, and the bottle cap is integrated with an NFC temperature and humidity sensor.
2. A tangerine peel soda water according to claim 1, characterized in that The headspace mixed gas pressure is 0.10-0.20 MPa, and the residual oxygen content is ≤0.6% v / v.
3. A tangerine peel soda water according to claim 1, characterized in that In the time-controlled release microspheres, the thickness of the acid-controlled release shell layer is 30-50 μm, and the particle size of the sweet-controlled release core layer is 20-60 μm.
4. A tangerine peel soda water according to claim 1, characterized in that The mineral salt is a mixture of sodium bicarbonate, magnesium hydrogen phosphate and potassium chloride in a mass ratio of 5:2:1 to 7:3:
1.
5. A tangerine peel soda water according to claim 1, characterized in that The pH responsive ink contains 0.05-0.15% w / v of methyl red and 0.02-0.08% w / v of bromocresol green.
6. A method for preparing tangerine peel soda water, according to any one of claims 1 to 5, characterized in that: The following steps are involved: (a) Tangerine peel pretreatment and low-temperature extraction; (b) gas-liquid synergistic stabilization treatment; (c) Preparation of time-controlled release microspheres; (d) Mixing and chaotic dispersion; (e) Integration of aseptic filling and dynamic monitoring; (f) Closed-loop control of process parameters.
7. The method for preparing tangerine peel soda water according to claim 6, wherein: In the step (b): The molar ratio of hydroxypropyl-β-cyclodextrin to tangerine peel essential oil is 1:2-1:4, the stirring temperature is 35-45° C., and the stirring time is 90-150 min.
8. The method for preparing tangerine peel soda water according to claim 6, wherein: In the step (b): Gas replacement adopts two-stage filling, first injecting CO2 to a pressure of 0.05-0.10MPa, and then injecting N2 to a total pressure of 0.12-0.18MPa.
9. The method for preparing tangerine peel soda water according to claim 6, wherein: In the step (c): The acid controlled-release shell layer was coated using a fluidized bed with an inlet air temperature of 40-50°C, a HPMCP ethanol solution concentration of 8-12% w / v, and a spraying rate of 2-4 mL / min.
10. The method for preparing tangerine peel soda water according to claim 6, wherein: In the step (d): The ultrasonic dispersion parameters are: basic frequency 18-22 kHz, random perturbation amplitude 0.05-2.5 kHz, power 300-500 W, and time 4-8 min.
