Method for controlling activity retention of shampoo plant raw material in low temperature short time extraction
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANGXI YUMEI COSMETICS CO LTD
- Filing Date
- 2026-03-02
- Publication Date
- 2026-06-05
Smart Images
Figure CN122141279A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of plant extract technology for shampoo, and in particular to a method for controlling the activity of plant extracts extracted at low temperature and in a short time for shampoo. Background Technology
[0002] In the field of plant-based ingredient extraction for shampoo, existing technologies generally employ fixed parameter control methods, such as fixed temperature and fixed time, which leads to the loss of active ingredients during the extraction process due to the inability to adjust the parameters.
[0003] Traditional high-temperature extraction at 60-80°C can cause heat-sensitive active ingredients such as flavonoids to degrade by more than 30%; while a fixed extraction time of 30-60 minutes often results in fluctuations in retention rate due to insufficient or excessive extraction of active ingredients. Although existing technologies have introduced low-temperature environments, they have not solved the problem of parameter linkage and cannot adjust the extraction endpoint according to the real-time active concentration, leading to unstable active ingredient retention rates.
[0004] This invention establishes a mathematical model for active ingredient retention rate, quantifying the interrelationships of parameters such as temperature, time, stirring speed, and solvent ratio, thus achieving closed-loop control of monitoring, calculation, and adjustment. Based on raw material-specific coefficients b, c, d, and E, this model ensures the extraction process terminates at the target active ingredient retention rate, avoiding prolonged ineffective extraction and achieving an overall improvement in active ingredient retention rate. This solves the problem of active ingredient loss due to independent parameter control in low-temperature, short-time extraction, providing a scientifically effective technical path for the extraction of plant-based raw materials for shampoo. Summary of the Invention
[0005] The purpose of this invention is to provide a method for controlling the activity of plant-based raw materials extracted at low temperature and in a short time for shampoo.
[0006] The problem this invention aims to solve is that existing shampoo plant raw material extraction processes rely on fixed parameters, which leads to the degradation of active ingredients during high-temperature or excessively long extraction processes, resulting in low activity retention rates; the lack of an activity monitoring and adjustment mechanism makes it impossible to control the extraction endpoint, causing activity loss or insufficient extraction.
[0007] A method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature, short-time extraction, the technical solution of which is as follows: S1: Raw Material Pretreatment and Activity Benchmark Setting: The plant raw materials are pulverized to obtain materials with uniform particle size. They are then pre-soaked in an ethanol-water mixed solvent to remove impurities and stabilize active ingredients. After filtration, a pre-treated solution is obtained. The initial concentration of the target active ingredient in the pre-treated solution is determined using standard analytical methods. This serves as the baseline value for calculating the activity retention rate; S2: Initialization of the Low-Temperature Extraction System and Presetting of Model Parameters: Transfer the pretreated liquid to the low-temperature reactor and set the initial extraction parameters, including extraction temperature, stirring speed, and solvent-to-material ratio. Based on the type of plant material, establish a mathematical model for activity retention rate through small-scale experiments, determine the specific temperature sensitivity coefficient b, time response coefficient c, stirring efficiency coefficient d, and solvent ratio response coefficient E for that material, and set the target activity retention rate based on the small-scale experimental data. ; S3: Parameter-linked control execution: Start the extraction process, monitor the concentration of the target active ingredient in the extract, and calculate the current activity retention rate. The required extraction time was calculated based on a mathematical model of activity retention rate. The extraction time parameters are adjusted in conjunction with the calculation results to achieve precise closed-loop control of the activity retention rate. During the extraction process, the extraction temperature, stirring speed, and solvent ratio remain unchanged from their initial settings, and only the extraction time is adjusted. S4: Post-extraction treatment: After extraction is terminated, the extract is filtered at low temperature using a filter membrane with a pore size that matches the stability of the active ingredient. The filtration temperature is maintained at a low temperature. The filtered extract is then refrigerated to ensure the stability of the active ingredient in subsequent processing.
[0008] Furthermore, in step S1, the initial concentration of the target active ingredient in the pretreatment solution is determined using standard analytical methods. As a benchmark for calculating the activity retention rate, it includes: The standard analytical method is a conventional method for detecting active ingredients. By establishing the correspondence between the concentration of active ingredients and the detection signal, the initial concentration of the target active ingredient in the pretreatment solution is determined. During the pre-soaking process in an ethanol-water mixed solvent, the active ingredients are stabilized through a pretreatment step to ensure... The measured values can accurately reflect the initial state of the active ingredients in the raw materials, providing a benchmark for subsequent calculation of the activity retention rate.
[0009] Furthermore, in step S2, a mathematical model for the activity retention rate is established through small-scale experiments, and a target activity retention rate is set based on the small-scale experimental data. ,include: Collect the activity concentration data of the target active ingredient under different extraction parameters, including temperature, time, stirring speed, and solvent ratio combinations, and form multiple sets of corresponding relationships; A mathematical model for the activity retention rate was established using nonlinear regression analysis. Where R is the activity retention rate, T is the extraction temperature, t is the extraction time, N is the stirring speed, and S / V is the solvent / material ratio; Nonlinear regression analysis was used to fit the raw material-specific coefficients b, c, d, and E, enabling the model to accurately characterize the quantitative relationship between raw material properties and activity retention rate. The target activity retention rate Based on the characteristics of the active ingredients in the raw materials and the process requirements, the target values for parameter linkage control are determined through routine experimental data.
[0010] Furthermore, in step S3, the current activity retention rate is calculated. ,include: During the extraction process, the activity concentration of the extract is monitored at fixed time intervals. The activity concentration monitoring adopts near-infrared spectroscopy technology and selects wavelengths based on the characteristic absorption peaks of the target active ingredient. The monitoring frequency is set based on the change pattern of the active ingredient during the extraction process, and the key time points of the change in active concentration are determined through experiments; The active concentration is calculated by converting it with a calibration curve established by a standard analytical method. This is achieved by correlating the pre-established near-infrared spectral signal with the calibration curve of the standard analytical method, and using the calibration curve to convert the spectral detection signal into an active concentration value. The activity retention rate ,in This represents the real-time active concentration. This represents the initial active concentration.
[0011] Furthermore, in step S3, the required extraction time is calculated based on a mathematical model of activity retention rate. ,include: This is achieved through the inverse solution of the mathematical model for activity retention rate, using conventional algebraic operations to determine the target activity retention rate. By associating with the current parameter, we obtain an explicit expression for time t. Based on the current extraction parameters, including temperature, stirring speed, solvent ratio, and preset target activity retention rate. The optimal extraction time point was derived.
[0012] Furthermore, in step S3, the extraction time parameter is adjusted in conjunction with the calculation results, including: when < Then calculate based on the current extraction parameters. The extraction time is dynamically adjusted to ;like ≥ If the extraction time reaches the preset upper limit, the extraction will be terminated immediately; if the extraction time reaches the preset upper limit and < If this occurs, the extraction process will be forcibly terminated.
[0013] The beneficial effects of this invention are: by establishing a mathematical model for the retention rate of active ingredients and controlling the parameters in a coordinated manner, the active ingredients in the low-temperature short-time extraction process of plant raw materials for shampoo are preserved, thereby improving the overall retention rate of active ingredients.
[0014] By quantifying the quantitative effects of temperature, time, stirring speed, and solvent ratio on the activity retention rate, this study solves the problem of activity loss caused by degradation or insufficient extraction of active ingredients in traditional fixed-parameter extraction. It enables the extraction process to adjust the extraction time according to the real-time activity concentration, ensuring that the activity retention rate terminates at the target value, avoiding ineffective extraction extension or activity loss. This provides a scientific basis and feasible technical path for the efficient extraction and stable retention of active ingredients. Attached Figure Description
[0015] Figure 1 This is a flowchart of a method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction. Detailed Implementation
[0016] The present invention will be further described clearly and completely below, but the scope of protection of the present invention is not limited thereto.
[0017] Furthermore, the term "and / or" in this article is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. Additionally, the character " / " in this article, unless otherwise specified, generally indicates that the preceding and following related objects have an "or" relationship.
[0018] Example 1 A method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature, short-time extraction, the technical solution of which is as follows: S1: Raw Material Pretreatment and Activity Benchmark Setting: The plant raw materials are pulverized to obtain materials with uniform particle size. They are then pre-soaked in an ethanol-water mixed solvent to remove impurities and stabilize active ingredients. After filtration, a pre-treated solution is obtained. The initial concentration of the target active ingredient in the pre-treated solution is determined using standard analytical methods. This serves as the baseline value for calculating the activity retention rate; S2: Initialization of the Low-Temperature Extraction System and Presetting of Model Parameters: Transfer the pretreated liquid to the low-temperature reactor and set the initial extraction parameters, including extraction temperature, stirring speed, and solvent-to-material ratio; based on the type of plant raw material, establish a mathematical model for activity retention rate through small-scale experiments, determine the specific coefficients b, c, d, and E for that raw material, and set the target activity retention rate based on the small-scale experimental data. ; S3: Parameter-linked control execution: Start the extraction process, monitor the concentration of the target active ingredient in the extract, and calculate the current activity retention rate. The required extraction time was calculated based on a mathematical model of activity retention rate. The extraction time parameters are adjusted in conjunction with the calculation results to achieve precise closed-loop control of the activity retention rate. During the extraction process, the extraction temperature, stirring speed, and solvent ratio remain unchanged from their initial settings, and only the extraction time is adjusted. S4: Post-extraction treatment: After extraction is terminated, the extract is filtered at low temperature using a filter membrane with a pore size that matches the stability of the active ingredient. The filtration temperature is maintained at a low temperature. The filtered extract is then refrigerated to ensure the stability of the active ingredient in subsequent processing.
[0019] refer to Figure 1 The diagram shown is a flowchart of a method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction.
[0020] Furthermore, in step S1, the plant raw materials are pulverized, pre-soaked in an ethanol-water mixed solvent, and filtered to obtain a pre-treated solution, comprising: A universal pulverizer is used to pulverize plant raw materials to 100-200 mesh (particle size range 75-150μm) to ensure uniform material surface area and avoid uneven extraction due to particle size differences. Particle size that is too small (<100 mesh) is prone to mechanical damage to active ingredients, while particle size that is too large (>200 mesh) will reduce extraction efficiency. The 100-200 mesh range has been experimentally verified as the optimal range for active ingredient retention.
[0021] The volume fraction of ethanol should be 70-80%. Small-scale experiments have shown that below 70% the solubility of active ingredients is insufficient, while above 80% it can easily lead to the inactivation of heat-sensitive components. The solvent to material ratio should be 10:1 (mL / g) to ensure sufficient wetting while avoiding excessive dilution of active ingredients by the solvent. The soaking time should be 30-60 minutes to ensure that impurities are fully removed and active ingredients are stabilized. If the time is too short, impurities will not be completely removed, and if it is too long, activity will be lost. The soaking temperature should be 4-10℃, as low temperature inhibits enzyme activity and prevents degradation of active ingredients.
[0022] The filter membrane has a pore size of 0.22μm, which matches the molecular weight of the active ingredient, effectively removing particulate impurities. The filtration is carried out at a low temperature of 4℃ and a filtration pressure of ≤0.2 MPa. Low-temperature filtration avoids the deactivation of heat-sensitive components.
[0023] Furthermore, in step S1, the initial concentration of the target active ingredient in the pretreatment solution is determined using standard analytical methods. As a benchmark for calculating the activity retention rate, it includes: The standard analytical method is a conventional method for detecting active ingredients, employing high-performance liquid chromatography (HPLC). The chromatographic column is a C18 reversed-phase column, 250×4.6mm, 5μm, a standard column type, which provides optimal separation of plant active ingredients. The mobile phase is acetonitrile-0.1% phosphoric acid aqueous solution, where acetonitrile improves solubility and phosphoric acid adjusts pH to inhibit degradation. The detection wavelength is determined based on the characteristic absorption peaks of the target active ingredients: 254 nm for flavonoids and 320 nm for polyphenols.
[0024] By establishing the correlation between active ingredient concentration and detection signal, a series of concentration solutions were prepared using high-purity target active ingredient standards. These solutions were then injected into HPLC, and the peak area corresponding to each concentration (i.e., the detection signal) was recorded, establishing a linear equation between concentration and peak area. The HPLC detection signal of the pretreated solution was converted into an active concentration value to ensure... Consistent with the initial state of the raw materials.
[0025] During the pre-soaking process in an ethanol-water mixed solvent, the active ingredients are stabilized through a pretreatment step to ensure... The measured values can accurately reflect the initial state of the active ingredients in the raw materials, providing a benchmark for subsequent calculation of the activity retention rate.
[0026] Furthermore, the initial extraction parameters set in S2 include extraction temperature, stirring speed, and solvent-to-material ratio, including: The extraction temperature is 5-8℃. Below 10℃, enzyme activity can be inhibited, while above 5℃, solvent fluidity is ensured. Small-scale experiments show that when the temperature is above 10℃, the activity loss is >15%. The stirring speed is 300-600 rpm. Below 300 rpm, the extraction is uneven, and above 600 rpm, the shear force causes damage to the active ingredients. Small-scale experiments show that 500 rpm is optimal. The solvent to material ratio is 8:1 to 12:1 mL / g. Below 8:1, the active ingredients are not fully dissolved, and above 12:1, the dilution effect is significant. Small-scale experiments show that the activity retention rate is highest at 10:1.
[0027] Furthermore, in step S2, a mathematical model for the activity retention rate is established through small-scale experiments, and a target activity retention rate is set based on the small-scale experimental data. ,include: Collect the activity concentration data of the target active ingredient under different extraction parameters, including temperature, time, stirring speed, and solvent ratio combinations, and form multiple sets of corresponding relationships; Based on a low-temperature environment setting of 5-8℃, covering the sensitive range of activity retention rate, the extraction temperature T was tested in the range of 5℃, 6℃, 7℃, and 8℃; based on the time gradient determined by pre-experiments, covering the rapid change range of activity retention rate, the extraction time t was tested in the range of 10, 20, 30, 40, and 50 min; covering the optimal range of activity retention rate, the stirring speed N was tested in the range of 300, 400, 500, and 600 rpm; based on the optimal ratio of 10:1, the solvent ratio S / V was tested in the range of 8:1, 9:1, 10:1, and 11:1. Each parameter combination was repeated 3 times to eliminate random errors; the activity concentration was determined using the HPLC method in S1; a total of 4×5×4×4=320 sets of data were generated, covering the entire parameter space.
[0028] A mathematical model for the activity retention rate was established using nonlinear regression analysis. Where R is the activity retention rate, T is the extraction temperature, t is the extraction time, N is the stirring speed, and S / V is the solvent / material ratio; 320 sets of experimental data were fitted using the nonlinear least squares method, and the fitting accuracy requirement was a correlation coefficient of not less than 0.95; This indicates that increased temperature accelerates active degradation, showing a negative correlation. The results indicate that prolonged extraction time promotes active ingredient extraction, showing a positive correlation, but this correlation gradually approaches saturation. and This indicates that moderate stirring / solvent ratio improves activity retention, showing a positive correlation.
[0029] Nonlinear regression analysis was used to fit the raw material-specific coefficients b, c, d, and E, enabling the model to accurately characterize the quantitative relationship between raw material characteristics and activity retention rate. b is the temperature sensitivity coefficient, characterizing the rate of activity loss caused by temperature increase; c is the time response coefficient, characterizing the promoting effect of extended extraction time on activity retention; d is the stirring efficiency coefficient, characterizing the contribution of stirring speed to activity protection; and E is the solvent ratio response coefficient, characterizing the promoting effect of solvent ratio on activity dissolution.
[0030] The target activity retention rate Based on the characteristics of the active ingredients in the raw materials and process requirements, the activity-stability curve of the raw materials is determined through routine experimental data. A safety threshold is then selected based on product process requirements and used as the target value for parameter-linked control. For heat-sensitive raw materials, No less than 90%, =90% product stability is optimal; for stable raw materials. No less than 85%, The overall cost-effectiveness is highest when the ratio is 85%.
[0031] Furthermore, in step S3, the current activity retention rate is calculated. ,include: During the extraction process, the activity concentration of the extract is monitored at fixed time intervals. The activity concentration monitoring adopts near-infrared spectroscopy technology, and wavelength selection is performed on the characteristic absorption peaks of the target active ingredient. The wavelength selection is strictly based on the characteristic wavelengths detected by HPLC.
[0032] The monitoring frequency is set based on the change pattern of active ingredients during the extraction process. The key time points of active concentration change are determined through experiments to avoid monitoring redundancy or omission due to fixed frequency. During the rapid change period: in the early stage of extraction t<20min, the monitoring frequency is 5 min / time; during the stable period t≥20min, the monitoring frequency is 15 min / time.
[0033] The active concentration is converted by a calibration curve established with the standard analytical method. This is achieved by correlating the pre-established near-infrared spectral signal with the calibration curve of the standard analytical method. The calibration curve is used to convert the spectral detection signal into an active concentration value. The active concentration of 320 pretreatment solutions is determined by HPLC, and the near-infrared spectra of the corresponding samples are collected simultaneously. The spectral signal intensity of the above-mentioned characteristic absorption peaks is selected and a linear fit is performed. The real-time active concentration is calculated by a linear fit formula without directly using the raw near-infrared signal.
[0034] The activity retention rate ,in This represents the real-time active concentration. This represents the initial active concentration.
[0035] Furthermore, in step S3, the required extraction time is calculated based on a mathematical model of activity retention rate. ,include: This is achieved through the inverse solution of the mathematical model for activity retention rate, using conventional algebraic operations to determine the target activity retention rate. By associating with the current parameter, an explicit expression for time t is obtained; The mathematical model for activity retention rate is as follows: ,make ,but , , , Substitute get ; Based on the current extraction parameters, including temperature, stirring speed, solvent ratio, and preset target activity retention rate. Obtain the raw material-specific coefficients b, c, d, E and The optimal extraction time point was derived.
[0036] Furthermore, in step S3, the extraction time parameter is adjusted in conjunction with the calculation results, including: when < Then calculate based on the current extraction parameters. The extraction time is dynamically adjusted to ;like ≥ If the extraction time reaches the preset upper limit, the extraction will be terminated immediately; if the extraction time reaches the preset upper limit and < If the extraction time is forced to terminate, the extraction will be terminated. For heat-sensitive raw materials, the preset upper limit for extraction time is 45 min. For stable raw materials, the preset upper limit for extraction time is 50 min.
[0037] Furthermore, in step S4, a filter membrane with a pore size matching the stability of the active ingredient is used to perform low-temperature filtration of the extract. The filtration temperature is maintained at a low temperature, and the filtered extract is then refrigerated and stored under low-temperature conditions, including: The filter membrane has a pore size of 0.22 μm. The pore size of 0.22 μm can effectively trap impurity particles while allowing active ingredients to pass through. A pore size <0.2 μm results in an active ingredient retention rate >15%, while a pore size >0.45 μm results in an impurity removal rate <80%.
[0038] The filtration temperature is 5-8°C, which inhibits the enzymatic degradation of active ingredients at low temperatures. When the temperature is >10°C, the activity loss is ≥8%, which is compatible with the low-temperature environment of the system. The filtration pressure is ≤0.2 MPa to avoid structural damage to active ingredients caused by high-pressure shearing. The filter medium is a 0.22 μm pore size filter membrane, which is resistant to low temperatures and chemically inert to avoid catalytic degradation by metal ions.
[0039] The low-temperature storage temperature is 0-4°C. Below 0°C, the solvent freezes and destroys the active ingredients, while above 4°C, it accelerates microbial growth. The storage time before subsequent processing should be ≤24 hours. If it exceeds 24 hours, the activity loss rate will increase.
[0040] Example 2 Rosemary leaves were pulverized to 150 mesh using a universal pulverizer to ensure uniform surface area. Pre-soaking was performed using an ethanol-water mixed solvent with 75% volume fraction ethanol, a solvent-to-material ratio of 10:1 mL / g, a soaking time of 45 min, a soaking temperature of 7℃, a filter membrane pore size of 0.22 μm, a filtration temperature of 4℃, and a filtration pressure of 0.15 MPa.
[0041] The initial concentration of rosmarinic acid was determined by HPLC using a C18 column (250 × 4.6 mm, 5 μm), with acetonitrile-0.1% phosphoric acid aqueous solution as the mobile phase and a detection wavelength of 320 nm. Standards were prepared at concentrations ranging from 0.1 to 10 mg / mL. The peak area of the calibration curve was calculated to be 1.25 × 10⁻⁶. +0.01 (correlation coefficient = 0.996); peak area measured in the treated solution = 125.3, calculated as follows: =100.2 mg / mL.
[0042] Initial extraction parameters were set as follows: extraction temperature 6℃, stirring speed 500 rpm, solvent to material ratio 10:1 mL / g. Nonlinear regression analysis was used to fit the mathematical model parameters for the activity retention rate: temperature sensitivity coefficient b = 0.028, time response coefficient c = 0.015, temperature sensitivity coefficient d = 0.0005, and temperature sensitivity coefficient E = 0.003. The target activity retention rate was... =85%, with the highest overall cost-effectiveness when the stable raw material content is 85%.
[0043] Activity concentration monitoring: The monitoring frequency was 5 min / time during the initial stage of extraction when t < 20 min, and 15 min / time during the stable period when t ≥ 20 min; the characteristic wavelength was 1525 cm⁻¹, corresponding to the near-infrared characteristic peak of 320 nm in HPLC detection; the calibration curve was 0.82 × spectral signal intensity + 0.03, and the correlation coefficient was 0.983.
[0044] Calculation of activity retention rate at t=25 min: near-infrared spectral signal intensity 120.5, real-time activity concentration. The concentration is 0.82 × 120.5 + 0.03 = 98.83 mg / mL, and the activity retention rate is... The value is 98.83 / 100.2*100%=98.63%.
[0045] The required extraction time was calculated based on a mathematical model of activity retention rate. Given the current parameters T=6℃, N=500rpm, and S / V=10:1, the calculation yields... It is 98.3 min, since t=25 min is currently less than The remaining time was set to 98.3-25=73.3 min. The extraction continued for 73.3 minutes and then stopped. At this point, the activity retention rate was 85%.
[0046] The filter membrane is a 0.22μm PVDF membrane, the filtration temperature is 6℃, and the filtration pressure is 0.18 MPa; the refrigerated storage temperature is 2℃, the storage time is no more than 24 hours, and the storage container is a deep-cold light-proof glass bottle with a sealed cap.
[0047] Example 3 Aloe vera gel was pulverized to 120 mesh using a multi-purpose grinder, avoiding over-grinding. Pre-soaking in an ethanol-water mixture was performed using 75% ethanol for 35 minutes at 5°C. The filter membrane had a pore size of 0.22 μm and was filtered at 4°C. Active ingredients were determined using HPLC. =78.5mg / mL, detection wavelength 254 nm, and the correlation coefficient of the calibration curve is 0.994.
[0048] Initial extraction parameters were set as follows: extraction temperature 5℃, stirring speed 400 rpm, solvent to material ratio 10:1 mL / g. Nonlinear regression analysis was used to fit the mathematical model parameters for the activity retention rate: temperature sensitivity coefficient b = 0.028, time response coefficient c = 0.009, temperature sensitivity coefficient d = 0.0003, and temperature sensitivity coefficient E = 0.0025. The target activity retention rate was... =90%, and the product stability is optimal when the content of heat-sensitive raw materials is 85%.
[0049] The active concentration of heat-sensitive raw materials changes more rapidly; for example, the active concentration change rate of aloe vera is >60% within 0-15 min, therefore a higher monitoring frequency is required. For the initial extraction phase (t < 15 min), the monitoring frequency is 3 min / time; for the stable extraction phase (t ≥ 15 min), the frequency is 10 min / time. Sampling is performed every 3 min, and the characteristic wavelength for near-infrared spectroscopy is 1680 cm⁻¹. -1 The correlation coefficient of the calibration curve corresponding to HPLC 254 nm is 0.985.
[0050] When t=0min =0% → Continue extraction; at t=5min =75.3% < 90%, calculate =12.8min → Remaining time set to 7.8min; at t=12.8min, = 90.5% > 90%, stop extraction immediately; total extraction time is 12.8 min.
[0051] The filter membrane is a 0.22μm PVDF membrane, and the filtration temperature is 5℃; the refrigeration storage temperature is 0℃, the storage time is no more than 12 hours, and the storage container is a cryogenic light-proof glass bottle wrapped with aluminum foil.
[0052] The above formulas are all dimensionless calculations. Dimensionless calculations can be performed using various methods such as standardization, which will not be elaborated here. The formulas are derived from software simulations based on a large amount of collected data, and the preset parameters in the formulas can be set by those skilled in the art according to the actual situation.
[0053] In conclusion, the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
[0054] This invention discloses a method for controlling the activity retention of plant-based raw materials in shampoo extraction at low temperatures and for a short time. By establishing a mathematical model for activity retention rate, it achieves coordinated control of temperature, time, stirring speed, and solvent ratio. The method includes: raw material pretreatment and activity benchmark setting: pulverization, ethanol-water pre-soaking, and initial concentration measurement; low-temperature extraction system initialization and model parameter preset: setting initial parameters, determining raw material-specific coefficients b, c, d, and E through small-scale experiments, and setting the target activity retention rate; parameter-coordinated control execution: real-time monitoring of activity concentration, calculation of the current activity retention rate, calculation of the required extraction time, and adjustment of the extraction time; and post-treatment of the extract: low-temperature filtration and cold storage. Through this monitoring-calculation-adjustment closed-loop control, the activity retention rate is improved, the extraction process is precisely terminated, and activity loss or ineffective prolongation is avoided, providing a reliable technical path for the extraction of active raw materials for shampoo.
Claims
1. A method for controlling the activity retention of plant-based raw materials extracted at low temperature and for a short time in shampoo production, characterized in that, include: S1: Raw Material Pretreatment and Activity Benchmark Setting: Plant raw materials are pulverized to obtain materials with uniform particle size, pre-soaked in an ethanol-water mixed solvent, and filtered to obtain a pretreatment solution. The initial concentration of the target active ingredient in the pretreatment solution is determined using standard analytical methods. This serves as the baseline value for calculating the activity retention rate; S2: Initialization of the Low-Temperature Extraction System and Presetting of Model Parameters: Transfer the pretreated liquid to the low-temperature reactor and set the initial extraction parameters, including extraction temperature, stirring speed, and solvent-to-material ratio; establish a mathematical model for activity retention rate based on the type of plant raw material through small-scale experiments, and set the target activity retention rate based on the experimental data. ; S3: Parameter-linked control execution: Start the extraction process, monitor the concentration of the target active ingredient in the extract, and calculate the current activity retention rate. The required extraction time was calculated based on a mathematical model of activity retention rate. The extraction time parameters are adjusted in conjunction with the calculation results; during the extraction process, the extraction temperature, stirring speed and solvent ratio remain unchanged from their initial settings. S4: Post-extraction treatment: After extraction is terminated, the extract is filtered at low temperature using a filter membrane with a pore size that matches the stability of the active ingredient. The filtered extract is then refrigerated and stored at low temperature.
2. The method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction as described in claim 1, characterized in that, In step S1, the initial concentration of the target active ingredient in the pretreatment solution is determined using standard analytical methods. As a benchmark for calculating the activity retention rate, it includes: The correlation between the concentration of the active ingredient and the detection signal was established using standard analytical methods, and the initial concentration of the target active ingredient in the pretreatment solution was determined. ; The active ingredients are stabilized through a pretreatment process during the pre-soaking process in an ethanol-water mixed solvent.
3. The method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction as described in claim 1, characterized in that, In step S2, a mathematical model for activity retention rate is established through small-scale experiments, and a target activity retention rate is set based on the experimental data. ,include: Collect the activity concentration data of the target active ingredient under different extraction parameters, including temperature, time, stirring speed, and solvent ratio combinations, and form multiple sets of corresponding relationships; A mathematical model for the activity retention rate was established using nonlinear regression analysis. Where R is the activity retention rate, T is the extraction temperature, t is the extraction time, N is the stirring speed, and S / V is the solvent / material ratio; Nonlinear regression analysis was used to fit and obtain the raw material-specific temperature sensitivity coefficient b, time response coefficient c, stirring efficiency coefficient d, and solvent ratio response coefficient E; the target activity retention rate Based on the characteristics of the active ingredients in the raw materials and the process requirements, the target values for parameter linkage control are determined through experimental data.
4. The method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction as described in claim 1, characterized in that, The current activity retention rate is calculated in step S3. ,include: During the extraction process, near-infrared spectroscopy is used to monitor the active concentration of the extract at fixed time intervals, and wavelength selection is performed based on the characteristic absorption peaks of the target active ingredient. The monitoring frequency is set based on the change pattern of the active ingredient during the extraction process, and the key time points of the change in active concentration are determined through experiments; The active concentration is calculated by converting the pre-established near-infrared spectral signal with a calibration curve of the standard analysis method, and the spectral detection signal is converted into an active concentration value using the calibration curve; The activity retention rate ,in This represents the real-time active concentration. This represents the initial active concentration.
5. The method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction as described in claim 1, characterized in that, The required extraction time in S3 is calculated based on a mathematical model of activity retention rate. ,include: By inversely solving the mathematical model of activity retention rate, based on the current extraction parameters and the target activity retention rate... calculate The optimal extraction time point is derived, and the current extraction parameters include temperature, stirring speed, and solvent ratio.
6. The method for controlling the activity retention of plant-based raw materials in shampoo through low-temperature short-time extraction as described in claim 1, characterized in that, The S3 step involves adjusting the extraction time parameter based on the calculation results, including: When the current activity retention rate is lower than the target activity retention rate, the required extraction time is calculated based on the current extraction parameters, and the extraction time is dynamically adjusted to that extraction time; when the current activity retention rate is not lower than the target activity retention rate, the extraction is terminated; when the extraction time reaches the preset upper limit and the current activity retention rate is still lower than the target activity retention rate, the extraction is forcibly terminated.