Control method and system for ultrasonic-assisted extraction of high-purity flavonoid compounds
By dynamically adjusting the ultrasonic power and extraction time according to material characteristics and extraction process in ultrasonic assisted extraction technology, the problems of low energy utilization efficiency and degradation of active ingredients in the prior art are solved, and efficient extraction of high-purity flavonoids is achieved.
Patent Information
- Application Number
- CN202411845396.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-16
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2044-12-16
AI Technical Summary
The existing ultrasonic assisted extraction technology cannot be adjusted in real time according to the dynamic changes of the extraction process, resulting in low energy utilization efficiency and easy degradation of the active ingredients, affecting the purity and yield of the extract.
By optimizing the formulation conditions according to material characteristics, using segmented control strategies for ultrasonic processing, and tracking the extraction process in real time through chromatography detection, adjusting the ultrasonic power and extraction time based on the changing trend of the efficiency curve.
It significantly improves the energy utilization efficiency, prevents excessive degradation of active ingredients, and improves the control accuracy of the extraction process and the purity of the extract.
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Figure CN119303339B_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of compound extraction, and in particular to a control method and system for ultrasonic-assisted extraction of high-purity flavonoid compounds. Background Art
[0002] As an important type of plant secondary metabolites, flavonoids are used in medicine, health products, functional foods, etc. Traditional extraction methods often have problems such as low extraction efficiency and high solvent consumption.
[0003] Ultrasonic assisted extraction technology enhances mass transfer through cavitation effect and is often used in the field of natural product extraction. This technology uses the micro-jets and shear force generated by ultrasound in the liquid to destroy the cell wall structure and accelerate the precipitation of active ingredients from the plant matrix, thereby improving the extraction efficiency.
[0004] However, existing ultrasound-assisted extraction technology generally uses fixed power and preset time for extraction, and cannot be adjusted in real time according to dynamic changes in the extraction process, resulting in low energy utilization efficiency and easily causing degradation of effective ingredients, affecting the purity and yield of the extract. This situation needs to be further improved. Summary of the invention
[0005] In order to solve the problem of low purity of extracts during extraction using the existing ultrasound-assisted extraction technology, the present application provides a control method and system for ultrasound-assisted extraction of high-purity flavonoid compounds, which adopts the following technical solutions:
[0006] In a first aspect, the present application provides a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds, comprising the following steps:
[0007] Determine the mass ratio of the raw material to the solvent and the component ratio of the solvent according to the material properties, and mix the raw material with the prepared solvent;
[0008] Controlling the ultrasonic power and extraction time to ultrasonically treat the mixture to obtain a flavonoid compound extract;
[0009] Detecting the content of flavonoid compounds in the extract by a chromatograph to determine extraction reaction data;
[0010] Draw a dynamic change curve of extraction efficiency according to the extraction reaction data;
[0011] The ultrasonic power and extraction time are adjusted based on the dynamic change curve.
[0012] By adopting the above technical scheme, the current ultrasonic system generally adopts fixed power and preset time for extraction. In actual application, under the same power level, the extraction rate of flavonoid compounds often shows a trend of first fast and then slow. If high-power operation is maintained continuously, it will not only cause energy waste, but also may cause the extracted effective ingredients to degrade. The present application first optimizes the preparation conditions according to the material characteristics, and then adopts a segmented control strategy for ultrasonic treatment. At the same time, the extraction process is tracked in real time through chromatographic detection, and the process parameters are adjusted in time based on the changing trend of the efficiency curve, avoiding the blindness of the traditional fixed parameter control method, and significantly improving the energy utilization efficiency through intelligent dynamic adjustment, effectively preventing the excessive degradation of effective ingredients, and improving the control accuracy of the extraction process.
[0013] Optionally, the mixture is ultrasonically treated by controlling the ultrasonic power and extraction time, specifically comprising the following steps:
[0014] The temperature of the mixture is detected before extraction to obtain initial temperature data;
[0015] Setting the starting power of the ultrasonic power according to the initial temperature data to obtain a power parameter;
[0016] Performing ultrasonic treatment according to the power parameters to obtain an extract;
[0017] Real-time detection of the temperature of the extract to obtain temperature change data;
[0018] The ultrasonic power is dynamically adjusted according to the temperature change data.
[0019] By adopting the above technical scheme, the complex influence of temperature on the extraction process is often ignored in traditional ultrasonic extraction. When the temperature is too high, the degradation of effective ingredients will be accelerated, while when the temperature is too low, the extraction efficiency will be reduced. The present application first detects the initial temperature of the mixture to establish a benchmark parameter, and then sets a reasonable starting power according to the temperature range. During the continuous extraction process, temperature data is collected in real time and the power output is dynamically adjusted accordingly. The temperature change is used as the key parameter for power regulation. Through the coordinated optimization of temperature and power, the extraction efficiency is guaranteed and the adverse effects that may be caused by drastic temperature fluctuations are avoided.
[0020] Optionally, setting the starting power of the ultrasonic power according to the initial temperature data specifically includes the following steps:
[0021] Detect the initial temperature value and divide it into low temperature zone, medium temperature zone and high temperature zone to obtain temperature zones;
[0022] According to the temperature partition, selecting a corresponding rated power percentage as a starting power;
[0023] Determining the power fluctuation allowable range based on a preset ratio of the starting power;
[0024] Maintaining continuous output mode operation within the permissible range of power fluctuation;
[0025] Record the extraction efficiency during continuous operation and determine the optimal power operation range.
[0026] By adopting the above-mentioned technical scheme, the present application first divides the working conditions into low temperature zone, medium temperature zone and high temperature zone according to the detected initial temperature, and then matches the preset rated power as the starting power respectively, and maintains continuous output mode operation within the allowable fluctuation range, and determines the optimal power operation range by real-time monitoring of the extraction efficiency, which effectively avoids local overheating and significantly improves the extraction efficiency and energy utilization.
[0027] Optionally, drawing a dynamic change curve of extraction efficiency according to the extraction reaction data specifically includes the following steps:
[0028] Calculate the amount of flavonoids extracted per unit time to obtain the extraction rate;
[0029] Recording the change of the extraction rate over time to obtain rate data;
[0030] Arranging the rate data in time series to obtain a dynamic change curve;
[0031] Marking the rate mutation point in the dynamic change curve to obtain the mutation time node;
[0032] The extraction phases are divided according to the mutation time nodes.
[0033] By adopting the above technical scheme, the present application first calculates the rate of change of the extraction amount of flavonoid compounds in each time period, plots these rate data into a dynamic change curve in time series, identifies the rate mutation point by analyzing the curve characteristics, and divides the entire extraction process into a rapid extraction period, a deceleration extraction period and a balanced extraction period. Through the dynamic monitoring of the extraction rate and the segmented control strategy, the regulation of process parameters is achieved, and the energy waste caused by blindly extending the extraction time is avoided, which significantly improves the efficiency and economy of the extraction process.
[0034] Optionally, marking the rate mutation point in the dynamic change curve to obtain the mutation time node specifically includes the following steps:
[0035] Collect the extraction rate values at three consecutive time points to obtain a rate sequence;
[0036] Calculating the variation range of the rate sequence to obtain variation data;
[0037] Mark the time points where the change amplitude is greater than a preset threshold as mutation points to obtain a mutation point set;
[0038] The point with the largest change amplitude is selected from the mutation point set and determined as the mutation time node.
[0039] By adopting the above technical solution, the present application first collects and extracts rate values at three consecutive time points to form a rate sequence, calculates the rate change amplitude between adjacent time points, and includes the time points whose change amplitude exceeds a preset threshold into a mutation point set. Finally, the point with the largest change amplitude is selected from the mutation point set as the mutation time node. Through multi-point rate sequence analysis and threshold screening, the accuracy of mutation point identification is improved, and timely adjustment of process parameters is achieved.
[0040] Optionally, adjusting the ultrasonic power and extraction time based on the dynamic change curve specifically includes the following steps:
[0041] Detect the slope of the extraction efficiency decline interval to obtain the decay rate;
[0042] Setting a power adjustment step according to the attenuation speed to obtain a power change;
[0043] Adjusting the ultrasonic power according to the power variation to obtain a change in extraction efficiency;
[0044] When the extraction efficiency changes less than the set ratio, the current time point is recorded;
[0045] The time point is determined as the extraction termination time.
[0046] By adopting the above technical scheme, when the extraction efficiency enters the decline period, blindly increasing the ultrasonic power or extending the time often fails to effectively increase the extraction volume, but instead increases energy consumption and equipment burden; the present application first calculates the slope value of the efficiency decline interval to characterize the attenuation rate, and determines the corresponding power adjustment step according to the size of the attenuation rate. When the increase in the extraction efficiency after power adjustment is lower than the preset ratio, the time point is determined as the optimal termination time. Through efficiency decay analysis and dynamic power adjustment, the extraction end point is accurately determined, avoiding energy waste caused by excessive extraction.
[0047] In a second aspect, the present application provides a control system for ultrasonic-assisted extraction of high-purity flavonoid compounds, comprising:
[0048] A preparation module is used to determine the mass ratio of the raw material to the solvent and the composition ratio of the solvent according to the material properties, and mix the raw material with the prepared solvent;
[0049] An ultrasonic module is used to control the ultrasonic power and extraction time to perform ultrasonic treatment on the mixture to obtain a flavonoid compound extract;
[0050] A detection module, used to detect the content of flavonoid compounds in the extract by a chromatograph to determine extraction reaction data;
[0051] An analysis module, used for drawing a dynamic change curve of extraction efficiency according to the extraction reaction data;
[0052] A control module is used to adjust the ultrasonic power and extraction time based on the dynamic change curve.
[0053] Optionally, the ultrasound module includes:
[0054] A temperature detection unit, used to detect the temperature of the mixture before extraction to obtain initial temperature data;
[0055] A power setting unit, used to set the starting power of the ultrasonic power according to the initial temperature data to obtain a power parameter;
[0056] An ultrasonic processing unit, used for performing continuous ultrasonic processing according to the power parameters to obtain an extract;
[0057] A temperature monitoring unit, used to detect the temperature of the extract in real time and obtain temperature change data;
[0058] A power regulating unit is used to dynamically adjust the ultrasonic power according to the temperature change data.
[0059] Optionally, the power setting unit includes:
[0060] A partition subunit is used to detect the initial temperature value and divide it into a low temperature zone, a medium temperature zone and a high temperature zone to obtain a temperature partition;
[0061] A selection subunit, for selecting a corresponding percentage of rated power as a starting power according to the temperature partition;
[0062] A fluctuation subunit, used to determine the power fluctuation allowable range according to a preset ratio of the starting power;
[0063] An output subunit, used to maintain continuous output mode operation within the allowable range of power fluctuation;
[0064] The efficiency subunit is used to record the extraction efficiency during continuous operation and determine the optimal power operation range.
[0065] Optionally, the analysis module includes:
[0066] A calculation unit, used to calculate the extraction amount of flavonoids per unit time to obtain the extraction rate;
[0067] A recording unit, used to record the change of the extraction rate over time to obtain rate data;
[0068] A drawing unit, used for arranging the rate data in time series to obtain a dynamic change curve;
[0069] A marking unit, used to mark the rate mutation point in the dynamic change curve to obtain the mutation time node;
[0070] A division unit is used to divide the extraction phase according to the mutation time node.
[0071] In summary, the present application includes at least one of the following beneficial technical effects:
[0072] The present application first optimizes the preparation conditions according to the material characteristics, then adopts a segmented control strategy for ultrasonic treatment, and simultaneously tracks the extraction process in real time through chromatographic detection, and adjusts the process parameters in a timely manner based on the changing trend of the efficiency curve, thereby avoiding the blindness of the traditional fixed parameter control method, significantly improving the energy utilization efficiency through intelligent dynamic adjustment, effectively preventing the excessive degradation of the effective ingredients, and improving the control accuracy of the extraction process;
[0073] In traditional ultrasonic extraction, the complex effect of temperature on the extraction process is often ignored. When the temperature is too high, the degradation of the effective ingredients will be accelerated, while when the temperature is too low, the extraction efficiency will be reduced. The present application first detects the initial temperature of the mixture to establish the benchmark parameters, and then sets a reasonable starting power according to the temperature range. During the continuous extraction process, the temperature data is collected in real time and the power output is dynamically adjusted accordingly. The temperature change is used as the key parameter for power regulation. Through the coordinated optimization of temperature and power, the extraction efficiency is guaranteed and the adverse effects that may be caused by drastic temperature fluctuations are avoided.
[0074] The present application first divides the operating conditions into low temperature zone, medium temperature zone and high temperature zone according to the detected initial temperature, and then matches the preset rated power as the starting power respectively, and maintains continuous output mode operation within the allowable fluctuation range, and determines the optimal power operation range by real-time monitoring of the extraction efficiency, which effectively avoids local overheating and significantly improves the extraction efficiency and energy utilization. BRIEF DESCRIPTION OF THE DRAWINGS
[0075] Figure 1 It is a schematic flow chart of a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds according to an embodiment of the present application;
[0076] Figure 2 It is a flow chart of step S200 in a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds in an embodiment of the present application;
[0077] Figure 3 It is a flow chart of step S220 in a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds in an embodiment of the present application;
[0078] Figure 4It is a flow chart of step S400 in a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds in an embodiment of the present application;
[0079] Figure 5 It is a flow chart of step S440 in a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds in an embodiment of the present application;
[0080] Figure 6 It is a flow chart of step S500 in a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds in an embodiment of the present application;
[0081] Figure 7 This is a module schematic diagram of a control system for ultrasonic-assisted extraction of high-purity flavonoid compounds according to an embodiment of the present application;
[0082] Figure 8 It is a diagram of the internal structure of an electronic device according to an embodiment of the present application. DETAILED DESCRIPTION
[0083] The terms used in the following embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to be used as limitations to the present application. As used in the specification and appended claims of the present application, the singular expressions "one", "a kind of", "said", "above", "the" and "this" are intended to also include plural expressions, unless there is a clear indication to the contrary in the context. It should also be understood that the term "and / or" used in the present application refers to any or all possible combinations comprising one or more listed items.
[0084] In the following, the terms "first" and "second" are used for descriptive purposes only and are not to be understood as suggesting or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features, and in the description of the embodiments of the present application, unless otherwise specified, "plurality" means two or more.
[0085] The embodiments of the present application are further described in detail below in conjunction with the drawings in the specification.
[0086] In the first aspect, the present application provides a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds, referring to Figure 1 , including the following steps:
[0087] S100, determining the mass ratio of the raw material to the solvent and the component ratio of the solvent according to the material properties, and mixing the raw material with the prepared solvent.
[0088] Among them, the raw materials can be selected from kudzu root, licorice, mulberry leaf, hawthorn and other medicinal and edible plants with high total flavonoid content. The raw materials need to be cleaned and dried before use, and ground to a preset particle size such as 20-40 mesh. The solvent is an ethanol-water mixed solvent. After the raw materials and the solvent are evenly mixed, they are left to stand to allow the materials to be fully soaked.
[0089] S200, controlling the ultrasonic power and extraction time to perform ultrasonic treatment on the mixture to obtain a flavonoid compound extract.
[0090] In this embodiment, ultrasonic treatment uses ultrasound with a frequency of 20-40kHz and a power range of 200-800W. The extraction temperature is controlled in the range of 20-60°C. The extraction effect is maintained by adjusting the power and temperature. The extraction time can be adjusted according to actual conditions.
[0091] Specifically, the infiltrated mixture was transferred to an ultrasonic extraction device, the ultrasonic frequency was set to 28 kHz, the initial power was 500 W, the extraction temperature was controlled at about 45°C, and intermittent ultrasonic treatment was performed. After each treatment for 30 minutes, a 5-minute pause was performed, and the extraction process was monitored in real time by an online monitoring system.
[0092] S300, detecting the content of flavonoid compounds in the extract by means of a chromatograph to determine extraction reaction data.
[0093] In this embodiment, the content of flavonoids in the extract was detected by high performance liquid chromatography, a C18 reverse phase column was selected as the chromatographic column, a methanol-water system was used as the mobile phase, the detection wavelength was set at 350 nm, and quantitative analysis was performed by the external standard method.
[0094] Specifically, 2 mL of sample was taken from the extraction system every 10 minutes, filtered through a 0.45 μm filter membrane, and then analyzed by HPLC, and the peak area value was recorded and converted into the flavonoid content in the extract. Rutin was used as a reference substance, and a standard solution with a concentration of 0.1 mg / mL was prepared, and a standard curve was established for quantitative analysis.
[0095] S400, drawing a dynamic change curve of extraction efficiency according to the extraction reaction data.
[0096] In this embodiment, the extraction efficiency is characterized by the amount of flavonoid compounds extracted per unit time. The extraction rate is obtained by calculating the change in extraction amount between consecutive sampling points. The data of the change in extraction rate over time is plotted into a curve graph for analyzing the dynamic characteristics of the extraction process.
[0097] Specifically, the flavonoid content data measured at each sampling time point are arranged in chronological order, the difference in extraction amount between two adjacent time points is calculated, and the extraction rate of the period is obtained by dividing it by the time interval. With time as the horizontal axis and the extraction rate as the vertical axis, a dynamic change curve of the extraction efficiency is drawn.
[0098] S500, adjusting the ultrasonic power and extraction time based on the dynamic change curve.
[0099] In this embodiment, by analyzing the characteristics of the dynamic change curve of the extraction efficiency, the key turning point of the extraction process is determined, and the ultrasonic power is adjusted in time according to the change trend of the curve. When the improvement of the extraction efficiency is not obvious, the extraction end point can be determined, thereby optimizing the extraction process parameters.
[0100] Specifically, when a clear downward trend in the extraction efficiency curve is observed, the ultrasonic power is increased by 50W. If the increase in extraction efficiency is less than 5% after three consecutive adjustments, it is determined that the optimal extraction endpoint has been reached. For example, when the extraction efficiency begins to decrease at an initial power of 500W, it is gradually increased to 550W, 600W, and 650W. If the efficiency improvement is not obvious, the extraction process is stopped.
[0101] The complex effect of temperature on the extraction process is often ignored in traditional ultrasonic extraction. When the temperature is too high, the degradation of the active ingredients will be accelerated, while when the temperature is too low, the extraction efficiency will be reduced. In one embodiment, referring to Figure 2 In step S200, the ultrasonic power and extraction time are controlled to perform ultrasonic treatment on the mixture, which specifically includes the following steps:
[0102] S210, detecting the temperature of the mixture before extraction to obtain initial temperature data.
[0103] In this embodiment, a temperature sensor is used to monitor the temperature of the mixture in real time, and the temperature detection accuracy is ±0.1° C. The temperature sensor probe is immersed in the center of the mixture, and the initial temperature value is recorded after the temperature reading stabilizes.
[0104] Specifically, after the prepared mixture is allowed to stand for 30 minutes, the temperature sensor probe is inserted into the center of the mixture, 3 cm from the bottom of the container, and the reading is allowed to stabilize for 2 minutes, and this temperature is recorded as the initial temperature data.
[0105] S220. Setting the starting power of the ultrasonic power according to the initial temperature data to obtain a power parameter.
[0106] In this embodiment, the temperature range is divided into multiple intervals according to different initial temperatures, and each interval corresponds to a different initial power value, so as to ensure a steady rise in temperature during the extraction process and avoid adverse effects of drastic temperature fluctuations on the extraction effect.
[0107] Specifically, when the initial temperature is in the range of 20-30°C, 60% of the rated power is selected as the starting power; when the temperature is in the range of 30-40°C, 50% of the rated power is selected as the starting power. For example, for an ultrasonic device with a maximum power of 1000W, if the initial temperature is 25°C, the starting power is set to 600W.
[0108] S230, performing ultrasonic treatment according to power parameters to obtain an extract.
[0109] In this embodiment, the continuous ultrasonic treatment adopts a constant power mode, and the stability of the output power is maintained by a power control system. The frequency of the ultrasonic wave is kept at a fixed value, generally selected at about 28kHz.
[0110] Specifically, after setting the power to 600W, the ultrasonic system was turned on for processing. During the processing, the actual output power was monitored in real time through the power feedback control system to ensure that the power fluctuation range was within ±5%. The extract was sampled and analyzed every 30 minutes to monitor the extraction effect.
[0111] S240, detecting the temperature of the extract in real time to obtain temperature change data.
[0112] In this embodiment, a distributed temperature detection system is used, and multiple temperature sensors are set at different positions of the extraction container to monitor the temperature distribution of the extract in real time. The temperature data is collected once per second, and the temperature information is transmitted to the control system through the data acquisition module to record the temperature change trend over time.
[0113] Specifically, a temperature sensor is installed at the bottom, middle and top of the extraction container, and the collection positions are 1 cm, 5 cm and 9 cm from the bottom of the container respectively. The system records the temperature data of the three positions every 1 second, calculates the average temperature value, and draws a temperature-time curve for analyzing the temperature change characteristics.
[0114] S250, dynamically adjusting the ultrasonic power according to the temperature change data.
[0115] In this embodiment, a dynamic adjustment strategy of temperature and power is established by analyzing the temperature change rate and temperature distribution uniformity. When the temperature rise rate is too fast, the power is appropriately reduced; when the temperature distribution is uneven, the convection of the mixture is promoted by adjusting the power to achieve a uniform temperature field.
[0116] In one embodiment, referring to Figure 3 In step S220, the starting power of the ultrasonic power is set according to the initial temperature data, which specifically includes the following steps:
[0117] S221. Detect the initial temperature value and divide it into a low temperature zone, a medium temperature zone and a high temperature zone to obtain temperature zones.
[0118] The temperature range is divided based on the thermal stability characteristics of flavonoids and the temperature dependence of extraction efficiency. The low temperature zone is set at 15-30°C, the medium temperature zone is 30-45°C, and the high temperature zone is 45-60°C. The temperature of the mixture is measured at multiple points, and the average value is taken as the initial temperature value, and the temperature range is determined accordingly.
[0119] S222. According to the temperature zone, select a corresponding rated power percentage as the starting power.
[0120] Different temperature ranges correspond to different power percentages. The low temperature zone uses higher power to quickly increase the system temperature, and the high temperature zone uses lower power to avoid excessive temperature rise. The gradient setting can achieve a smooth temperature transition.
[0121] Specifically, when the initial temperature is detected to be 26.8°C, which belongs to the low temperature zone, 75% of the rated power is selected as the starting power. If the rated power of the ultrasonic device is 1000W, the starting power is set to 750W, which will be used as the reference power for subsequent pulse control.
[0122] S223: Determine the power fluctuation allowable range based on a preset ratio of the starting power.
[0123] In this embodiment, the power fluctuation range needs to be set in consideration of the stability and control accuracy of the equipment, and the fluctuation range is generally set within ±10% of the starting power. The output power is monitored in real time through the power detection module. When the power exceeds the allowable range, the control system automatically makes corrections to ensure the stability of the extraction process.
[0124] Specifically, for a starting power of 750 W, the power fluctuation allowable range is set to ±75 W, i.e. 675-825 W. The control system collects the actual output power every 0.1 seconds. When it detects that the power value exceeds this range, it immediately starts the power compensation mechanism to adjust the power back to the allowable range.
[0125] S224. Maintain continuous output mode operation within the allowable range of power fluctuation.
[0126] In this embodiment, maintaining a stable output of ultrasound in the continuous output mode can maintain a stable cavitation effect and improve the extraction efficiency. The power control system adjusts the output power in real time through a closed-loop feedback method to keep it within the set fluctuation range.
[0127] Specifically, the control system uses a PID control algorithm to achieve precise power regulation in a continuous operation range of 675-825W. For example, when the ambient temperature fluctuates and causes a ±5% power deviation, the control system can adjust the power to the target value within 2 seconds to ensure the stability of the extraction process.
[0128] S225. Record the extraction efficiency during continuous operation and determine the optimal power operation range.
[0129] In this embodiment, the extraction efficiency data at different power levels is recorded by an online monitoring system to establish a corresponding relationship curve between power and extraction efficiency. The system collects samples for analysis at fixed intervals and obtains the optimal power operating range through data processing.
[0130] In one embodiment, referring to Figure 4 In step S400, a dynamic change curve of extraction efficiency is drawn according to the extraction reaction data, which specifically includes the following steps:
[0131] S410, calculating the extraction amount of flavonoids per unit time to obtain the extraction rate.
[0132] In this embodiment, the extraction rate is calculated by using a continuous sampling analysis method and is determined by measuring the increment of flavonoid compounds in the extract per unit time.
[0133] Specifically, 2 mL of sample was taken from the extraction system every 10 minutes, and the flavonoid content was determined by ultraviolet spectrophotometry. The average extraction rate of the time period was obtained by calculating the difference of the flavonoid content in two adjacent sampling times and dividing it by the time interval.
[0134] S420, record the change of extraction rate over time to obtain rate data.
[0135] In this embodiment, the rate data is recorded using an automated data acquisition system, which stores the extracted rate data at each time point in real time and organizes them into a data sequence.
[0136] Specifically, a computer control system is used to establish a database, and information such as the time and extraction rate of each sampling point is stored in a preset format.
[0137] S430, arranging the rate data in time series to obtain a dynamic change curve.
[0138] In this embodiment, the dynamic change curve is drawn using professional data analysis software, and the collected rate data points are connected in chronological order to form a continuous change trend line.
[0139] Specifically, the rate data is imported and a curve graph is generated using data processing software, with the abscissa being the extraction time and the ordinate being the extraction rate. For example, during the extraction process of 0-120 minutes, the curve shows a characteristic of first rising rapidly and then falling slowly, with the highest extraction rate occurring at around 35 minutes.
[0140] S440, marking the rate mutation point in the dynamic change curve to obtain the mutation time node.
[0141] Among them, the determination of the rate mutation point is based on the significant change in the slope of the curve. The numerical analysis method is used to calculate the rate of change of each point on the curve. When the rate of change exceeds the preset threshold, it is marked as a mutation point.
[0142] Specifically, when the slope change between two adjacent data points exceeds the set slope change threshold, the point is marked as a mutation point. For example, during the extraction process, it was found that there were obvious slope mutations at 25 minutes and 85 minutes, and these two time points were determined as mutation time nodes.
[0143] S450, dividing the extraction phases according to the mutation time nodes.
[0144] In this embodiment, the division of the extraction phases is based on the distribution characteristics of the mutation time nodes, and the entire extraction process is divided into different phases such as a rapid extraction phase, a stable extraction phase, and a decay phase.
[0145] In one embodiment, referring to Figure 5 In step S440, the rate mutation point in the dynamic change curve is marked to obtain the mutation time node, which specifically includes the following steps:
[0146] S441, collecting extraction rate values at three consecutive time points to obtain a rate sequence.
[0147] In this embodiment, the rate series is collected using a sliding window method, and the extraction rate data of three consecutive time points are taken for analysis each time, which effectively eliminates the influence of single-point fluctuations and improves the accuracy and reliability of mutation point judgment.
[0148] Specifically, according to the sampling interval of 10 minutes, three adjacent time point data are selected each time to form a sequence group.
[0149] S442. Calculate the change amplitude of the rate sequence to obtain change data.
[0150] S443: Mark the time points where the change amplitude is greater than a preset threshold as mutation points to obtain a mutation point set.
[0151] The preset threshold is determined based on historical data analysis and process experience, and a critical value that can effectively distinguish normal fluctuations from significant changes is selected. The system automatically marks and stores all time points that exceed the threshold to form a set of candidate mutation points.
[0152] S444. Select the point with the largest change amplitude from the mutation point set and determine it as the mutation time node.
[0153] Among them, the final mutation time node is determined by the extreme value screening method, and the point with the most significant change amplitude is selected from the set of candidate mutation points as the key time node.
[0154] Specifically, the points in the mutation point set are sorted, and the point with the largest change amplitude is selected as the mutation time node. For example, among the three mutation points mentioned above, the change amplitude at t=85 minutes is 0.38 mg / min, which is the largest, so this time point is determined as the mutation time node.
[0155] In one embodiment, referring to Figure 6 In step S500, the ultrasonic power and extraction time are adjusted based on the dynamic change curve, which specifically includes the following steps:
[0156] S510, detecting the slope of the extraction efficiency decreasing interval to obtain the attenuation rate.
[0157] Among them, the detection of the attenuation rate adopts a real-time data analysis method, which is determined by calculating the rate of change of the extraction efficiency curve in the descending range, reflecting the speed at which the extraction process gradually slows down.
[0158] S520: Set the power adjustment step size according to the attenuation speed to obtain the power change.
[0159] In this embodiment, the power adjustment step size is set based on the numerical value of the attenuation speed, and a proportional adjustment strategy is adopted. When the attenuation speed is large, the power adjustment step size is increased to compensate for the efficiency drop; when the attenuation speed is small, a smaller adjustment step size is used to avoid over-compensation.
[0160] S530, adjusting the ultrasonic power according to the power change to obtain a change in extraction efficiency.
[0161] In this embodiment, the ultrasonic power is adjusted in a gradual increase manner, and is adjusted each time according to the set power change amount, while monitoring the response of the extraction efficiency to avoid the impact of sudden power changes on the extraction system.
[0162] S540: When the extraction efficiency changes less than the set ratio, record the current time point.
[0163] In this embodiment, the judgment of the change in extraction efficiency is based on the comparison of the efficiency after two consecutive power adjustments. The system pre-sets a minimum threshold for efficiency improvement. When the actual improvement effect is lower than this threshold, it means that continuing to increase the power can no longer significantly improve the extraction effect.
[0164] S550: Determine the time point as the extraction termination time.
[0165] It should be understood that the size of the serial numbers of the steps in the above embodiments does not mean the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
[0166] In the second aspect, the present application provides a control system for ultrasonic-assisted extraction of high-purity flavonoid compounds. The control system for ultrasonic-assisted extraction of high-purity flavonoid compounds of the present application is described below in combination with the above-mentioned control method for ultrasonic-assisted extraction of high-purity flavonoid compounds.
[0167] Reference Figure 7 , a control system for ultrasonic-assisted extraction of high-purity flavonoid compounds, comprising:
[0168] A preparation module is used to determine the mass ratio of the raw material to the solvent and the composition ratio of the solvent according to the material properties, and mix the raw material with the prepared solvent;
[0169] An ultrasonic module is used to control the ultrasonic power and extraction time to perform ultrasonic treatment on the mixture to obtain a flavonoid compound extract;
[0170] A detection module, used to detect the content of flavonoid compounds in the extract by means of a chromatograph and determine extraction reaction data;
[0171] An analysis module is used to draw a dynamic change curve of extraction efficiency based on extraction reaction data;
[0172] The control module is used to adjust the ultrasonic power and extraction time based on the dynamic change curve.
[0173] In one embodiment, the ultrasound module comprises:
[0174] A temperature detection unit, used to detect the temperature of the mixture before extraction to obtain initial temperature data;
[0175] A power setting unit, used to set the starting power of the ultrasonic power according to the initial temperature data to obtain the power parameter;
[0176] An ultrasonic processing unit, used for performing continuous ultrasonic processing according to power parameters to obtain an extract;
[0177] The temperature monitoring unit is used to detect the temperature of the extract in real time and obtain temperature change data;
[0178] The power regulating unit is used to dynamically adjust the ultrasonic power according to the temperature change data.
[0179] In one embodiment, the power setting unit includes:
[0180] A partition subunit is used to detect the initial temperature value and divide it into a low temperature zone, a medium temperature zone and a high temperature zone to obtain a temperature partition;
[0181] A selection subunit is used to select a corresponding percentage of rated power as a starting power according to the temperature partition;
[0182] A fluctuation subunit, used to determine the power fluctuation allowable range with a preset ratio of the starting power;
[0183] The output subunit is used to maintain the continuous output mode operation within the allowable range of power fluctuation;
[0184] The efficiency subunit is used to record the extraction efficiency during continuous operation and determine the optimal power operation range.
[0185] In one embodiment, the analysis module includes:
[0186] A calculation unit, used to calculate the extraction amount of flavonoids per unit time to obtain the extraction rate;
[0187] A recording unit, used to record the change of the extraction rate over time to obtain rate data;
[0188] A drawing unit is used to arrange the rate data in time series to obtain a dynamic change curve;
[0189] A marking unit is used to mark the rate mutation point in the dynamic change curve to obtain the mutation time node;
[0190] The division unit is used to divide the extraction phase according to the mutation time nodes.
[0191] In one embodiment, the marking unit comprises:
[0192] A collection subunit, used for collecting extraction rate values at three consecutive time points to obtain a rate sequence;
[0193] A calculation subunit is used to calculate the change amplitude of the rate sequence and obtain the change data;
[0194] A judgment subunit is used to mark the time point when the change amplitude is greater than a preset threshold as a mutation point to obtain a mutation point set;
[0195] The subunit is selected to select the point with the largest change amplitude from the mutation point set and determine it as the mutation time node.
[0196] In one embodiment, the control module includes:
[0197] A slope detection unit, used to detect the slope of the extraction efficiency decline interval to obtain the decay rate;
[0198] A step length setting unit, used to set a power adjustment step length according to the attenuation speed to obtain a power change amount;
[0199] A power regulating unit, used to regulate the ultrasonic power according to the power variation to obtain the extraction efficiency variation;
[0200] A time recording unit, used to record the current time point when the extraction efficiency changes less than a set ratio;
[0201] The termination determination unit is used to determine a time point as the extraction termination time.
[0202] In one embodiment, the present application provides an electronic device, which may be a server, and its internal structure diagram may be as follows: Figure 8 As shown. The electronic device includes a processor, a memory and a network interface connected through a system bus. Among them, the processor of the electronic device is used to provide computing and control capabilities. The memory of the electronic device includes a non-volatile storage medium and an internal memory. The non-volatile storage medium stores an operating system, a computer program and a database. The internal memory provides an environment for the operation of the operating system and the computer program in the non-volatile storage medium. The database of the electronic device is used to store data. The network interface of the electronic device is used to communicate with an external terminal through a network connection. When the computer program is executed by the processor, a control method for ultrasonic-assisted extraction of high-purity flavonoid compounds is implemented.
[0203] Those skilled in the art will understand that Figure 8 The structure shown in the figure is merely a block diagram of a partial structure related to the scheme of the present application, and does not constitute a limitation on the electronic device to which the scheme of the present application is applied. The specific electronic device may include more or fewer components than shown in the figure, or combine certain components, or have a different arrangement of components.
[0204] In one embodiment, an electronic device is further provided, including a memory and a processor, wherein a computer program is stored in the memory, and the processor implements the steps in the above method embodiments when executing the computer program.
[0205] Those of ordinary skill in the art can understand that all or part of the processes in the above-mentioned embodiment methods can be completed by instructing the relevant hardware through a computer program, and the above-mentioned computer program can be stored in a non-volatile computer-readable storage medium. When the computer program is executed, it can include the processes of the embodiments of the above-mentioned methods. Among them, any reference to memory, storage, database or other media used in the embodiments provided in this application can include at least one of non-volatile and volatile memory. Non-volatile memory can include read-only memory (ROM), tape, floppy disk, flash memory or optical memory, etc. Volatile memory can include random access memory (RAM) or external cache memory. As an illustration and not limitation, RAM can be in various forms, such as static random access memory (SRAM) or dynamic random access memory (DRAM).
[0206] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.
Claims
1. A control method for ultrasonic-assisted extraction of high-purity flavonoid compounds, characterized in that: The steps include: Determine the mass ratio of the raw material to the solvent and the component ratio of the solvent according to the material properties, and mix the raw material with the prepared solvent; Controlling the ultrasonic power and extraction time to ultrasonically treat the mixture to obtain a flavonoid compound extract; Detecting the content of flavonoid compounds in the extract by a chromatograph to determine extraction reaction data; Draw a dynamic change curve of extraction efficiency according to the extraction reaction data; Adjusting the ultrasonic power and extraction time based on the dynamic change curve; The ultrasonic treatment of the mixture is performed by controlling the ultrasonic power and the extraction time, which specifically includes the following steps: The temperature of the mixture is detected before extraction to obtain initial temperature data; Setting the starting power of the ultrasonic power according to the initial temperature data to obtain a power parameter; Performing ultrasonic treatment according to the power parameters to obtain an extract; Real-time detection of the temperature of the extract to obtain temperature change data; Dynamically adjust the ultrasonic power according to the temperature change data; The step of setting the starting power of the ultrasonic power according to the initial temperature data specifically includes the following steps: The initial temperature value is detected and divided into a low temperature zone, a medium temperature zone and a high temperature zone to obtain a temperature zone. The temperature zone is divided based on the thermal stability characteristics of flavonoids and the temperature dependence of extraction efficiency. The low temperature zone is set at 15-30°C, the medium temperature zone is set at 30-45°C, and the high temperature zone is set at 45-60°C. According to the temperature partition, a corresponding rated power percentage is selected as the starting power, and different temperature intervals correspond to different power percentages; Determining the power fluctuation allowable range based on a preset ratio of the starting power; Maintaining continuous output mode operation within the permissible range of power fluctuation; Record the extraction efficiency during continuous operation and determine the optimal power operation range.
2. The control method for ultrasonic-assisted extraction of high-purity flavonoid compounds according to claim 1, characterized in that: Drawing a dynamic change curve of extraction efficiency according to the extraction reaction data specifically includes the following steps: Calculate the amount of flavonoids extracted per unit time to obtain the extraction rate; Recording the change of the extraction rate over time to obtain rate data; Arranging the rate data in time series to obtain a dynamic change curve; Marking the rate mutation point in the dynamic change curve to obtain the mutation time node; The extraction phases are divided according to the mutation time nodes.
3. The control method for ultrasonic-assisted extraction of high-purity flavonoid compounds according to claim 2, characterized in that: Marking the rate mutation point in the dynamic change curve to obtain the mutation time node specifically includes the following steps: Collect the extraction rate values at three consecutive time points to obtain a rate sequence; Calculating the variation range of the rate sequence to obtain variation data; Mark the time points where the change amplitude is greater than a preset threshold as mutation points to obtain a mutation point set; The point with the largest change amplitude is selected from the mutation point set and determined as the mutation time node.
4. The control method for ultrasonic-assisted extraction of high-purity flavonoid compounds according to claim 1, characterized in that: Adjusting the ultrasonic power and extraction time based on the dynamic change curve specifically includes the following steps: Detect the slope of the extraction efficiency decline interval to obtain the decay rate; Setting a power adjustment step according to the attenuation speed to obtain a power change; Adjusting the ultrasonic power according to the power variation to obtain a change in extraction efficiency; When the extraction efficiency changes less than the set ratio, the current time point is recorded; The time point is determined as the extraction termination time.
5. A control system for ultrasonic-assisted extraction of high-purity flavonoid compounds, characterized in that: include: A preparation module is used to determine the mass ratio of the raw material to the solvent and the composition ratio of the solvent according to the material properties, and mix the raw material with the prepared solvent; An ultrasonic module is used to control the ultrasonic power and extraction time to perform ultrasonic treatment on the mixture to obtain a flavonoid compound extract; A detection module, used to detect the content of flavonoid compounds in the extract by a chromatograph to determine extraction reaction data; An analysis module, used for drawing a dynamic change curve of extraction efficiency according to the extraction reaction data; A control module, used for adjusting the ultrasonic power and extraction time based on the dynamic change curve; The ultrasound module comprises: A temperature detection unit, used to detect the temperature of the mixture before extraction to obtain initial temperature data; A power setting unit, used to set the starting power of the ultrasonic power according to the initial temperature data to obtain a power parameter; An ultrasonic processing unit, used for performing continuous ultrasonic processing according to the power parameters to obtain an extract; A temperature monitoring unit, used to detect the temperature of the extract in real time and obtain temperature change data; A power regulating unit, used for dynamically regulating the ultrasonic power according to the temperature change data; The power setting unit comprises: The partition subunit is used to detect the initial temperature value and divide it into a low temperature zone, a medium temperature zone and a high temperature zone to obtain a temperature partition. The temperature interval division is based on the thermal stability characteristics of flavonoids and the temperature dependence of extraction efficiency. The low temperature zone is set at 15-30°C, the medium temperature zone is 30-45°C, and the high temperature zone is 45-60°C. According to the temperature partition, a corresponding rated power percentage is selected as the starting power, and different temperature intervals correspond to different power percentages; A fluctuation subunit, used to determine the power fluctuation allowable range according to a preset ratio of the starting power; An output subunit, used to maintain continuous output mode operation within the allowable range of power fluctuation; The efficiency subunit is used to record the extraction efficiency during continuous operation and determine the optimal power operation range.
6. The control system for ultrasonic-assisted extraction of high-purity flavonoid compounds according to claim 5, characterized in that: The analysis module comprises: A calculation unit, used to calculate the extraction amount of flavonoids per unit time to obtain the extraction rate; A recording unit, used to record the change of the extraction rate over time to obtain rate data; A drawing unit, used for arranging the rate data in time series to obtain a dynamic change curve; A marking unit, used to mark the rate mutation point in the dynamic change curve to obtain the mutation time node; A division unit is used to divide the extraction phase according to the mutation time node.
Citation Information
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