Method for extracting natural active ingredients through ultrasonic coupling gradient temperature regulation and application
Through ultrasonic coupled gradient temperature regulation and dynamic solvent polarity regulation, combined with the online separation system, the problems of low extraction efficiency and poor selectivity of traditional natural active ingredients are solved, and efficient, green and energy-saving extraction and purification effects are achieved.
Patent Information
- Application Number
- CN202510640405.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-19
- Publication Date
- 2025-07-18
AI Technical Summary
Traditional natural active ingredient extraction methods are inefficient and poorly selective, and the use of toxic solvents leads to high residual risk, making it difficult to achieve efficient, green extraction and purification.
Ultrasonic coupled gradient temperature regulation technology is adopted, combined with dynamic solvent polarity regulation and online separation system, different polar components are extracted in stages, and integrated extraction-purification is achieved through multi-stage membrane separation and temperature-sensitive molecular blotting resin.
It improves extraction selectivity by 50%, reduces solvent usage by 50%, reduces energy consumption by 30%, and shortens the processing time to 1/3 of the traditional methods, supporting industrial continuous production.
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of extraction and separation of natural products, and particularly relates to an efficient extraction method of natural active ingredients based on ultrasonic coupling gradient temperature regulation, which is applicable to the green extraction of thermosensitive and highly polar active ingredients in raw materials such as traditional Chinese medicines, tea, fruits and vegetables, and can be extended to the food, pharmaceutical and cosmetic industries. Background Art
[0002] The extraction efficiency of natural active ingredients (such as flavonoids, terpenoids, alkaloids, polysaccharides, etc.) is limited by the limitations of traditional methods: 1. Single-temperature extraction: Conventional ultrasonic or heating reflux methods use constant-temperature operation, resulting in low dissolution rates or degradation of some components due to unsuitable temperatures (for example, high temperatures destroy vitamin C, and low temperatures cannot release fat-soluble components); 2. Coexistence of impurities: Multiple components are mixed in the crude extract, making subsequent purification difficult; 3. Solvent dependence: Toxic solvents such as methanol and chloroform need to be used, and the risk of residue is high. Summary of the Invention
[0003] Object of the Invention The present invention proposes an ultrasonic coupling gradient temperature dynamic regulation technology, which through the intelligent matching of temperature and ultrasonic parameters, targets and extracts different polar active ingredients in stages, and integrates an online separation system to achieve extraction-purification integration, breaking through the technical bottlenecks of low efficiency and poor selectivity of traditional methods. Technical Solution
[0004] 1. Gradient temperature regulation module: The first stage (low-temperature cell wall breaking): At 20 - 35 °C, low-frequency ultrasonic waves (20 - 40 kHz) are used to break the cell wall and release water-soluble components (such as polysaccharides, amino acids); The second stage (medium-temperature release): The temperature is raised to 40 - 55 °C, and high-frequency ultrasonic waves (50 - 80 kHz) are switched to enhance the dissolution of medium-polarity components (such as flavonoids, polyphenols); The third stage (high-temperature extraction): The temperature is raised to 60 - 75 °C, and pulsed ultrasound (duty cycle 1:1) is combined to extract fat-soluble components (such as terpenoids, volatile oils); 2. Optimization of the solvent system: An adjustable polarity solvent system: a ternary system of water / ethanol / deep eutectic solvent (DES), where DES is composed of betaine and lactic acid (molar ratio 1:2), and the solvent ratio is dynamically adjusted according to the polarity of the target component; Solvent recycling: Ethanol is recovered by thin-film evaporation, and the recovery rate of DES ≥ 95%; 3. Online separation system: The extract is imported into a series-connected multi-stage membrane separation device (ultrafiltration membrane + nanofiltration membrane) in real time, and the active ingredients are intercepted by molecular weight grading; Combined with temperature-sensitive molecularly imprinted resin (such as thermosensitive MIPs), selective adsorption of target components is achieved. Innovation points
[0005] 1. Temperature-ultrasonic frequency synergistic mechanism: Through the precise matching of temperature gradient and ultrasonic frequency, the release of components in different regions of cells is activated in stages, and the extraction rate is increased by 40%-60%; 2. Dynamic solvent polarity regulation: Automatically adjust the solvent polarity according to temperature changes, avoid multi-batch operations, and reduce energy consumption by 30%; 3. Integrated extraction-separation: Integrate online membrane separation and thermosensitive adsorption technologies, and the purity of the crude extract can reach more than 80%. Specific implementation methods
[0006] Example: Extraction of flavonoid components from Ginkgo biloba leaves 1. Crush Ginkgo biloba leaves to 60 mesh, and add a water / ethanol / DES (5:3:2) mixed solvent according to a solid-liquid ratio of 1:20; 2. Gradient temperature control: Treat at 30°C and 30 kHz for 20 minutes (cell wall breaking stage); Treat at 50°C and 60 kHz for 30 minutes (flavonoid release); Treat at 70°C and pulsed 80 kHz for 15 minutes (removal of lipophilic impurities); 3. The extract is separated by a 100 kDa ultrafiltration membrane to obtain a flavonoid purity of 82.3% and a total extraction rate of 91.5% (the traditional constant temperature method is 68%). Beneficial effects
[0007] 1. Targeted extraction: Design temperature-ultrasonic parameters for different polar components, and the extraction selectivity is increased by 50%; 2. Energy conservation and environmental protection: The solvent consumption is reduced by 50%, and DES can be recycled; 3. Industrial adaptation: Support continuous production, and the processing time is shortened to 1 / 3 of the traditional method.
Claims
1. A method for extracting natural active ingredients by ultrasonic coupling gradient temperature regulation, characterized in that It includes the following steps: Gradient temperature staged regulation, ultrasonic frequency dynamic matching, adjustable polarity solvent system and on-line multi-stage separation.
2. The method according to claim 1, wherein The gradient temperature is divided into three stages: 20 - 35 °C (low-frequency ultrasonic cell wall breaking), 40 - 55 °C (medium-frequency release of medium-polarity components), 60 - 75 °C (high-frequency pulse extraction of lipophilic components).
3. The method according to claim 1, wherein A ternary system of water / ethanol / deep eutectic solvent (DES) is adopted, and DES is synthesized from a hydrogen bond donor and an acceptor in a molar ratio of 1:1 - 1:
3.
4. The method according to claim 1, wherein An on-line separation system integrating ultrafiltration - nanofiltration membranes and temperature-sensitive molecularly imprinted resins.