A method for extracting effective components from radix paeoniae alba

Abstract

The application discloses a method for extracting effective components of radix paeoniae alba, which comprises the following steps: (1) preparing a radix paeoniae alba suspension, and feeding the radix paeoniae alba suspension into a treatment cavity; (2) a needle-plate electrode structure is arranged in the treatment cavity, the needle-plate electrode structure is connected with a high-frequency pulse power supply, and high-voltage pulse treatment is applied to the radix paeoniae alba suspension in the treatment cavity; and (3) the extracted solution after treatment is concentrated under reduced pressure to obtain active extracts. The extraction process can quickly inhibit enzyme activity, prevent paeoniflorin from being hydrolyzed by coexisting enzymes, realize efficient extraction of paeoniflorin at low temperature, and ensure the structural integrity of macromolecular active components such as radix paeoniae alba polysaccharide; and the scheme can improve the extraction efficiency and shorten the production cycle.

Description

Technical Field

[0001] This application belongs to the field of traditional Chinese medicine extraction, and specifically relates to a method for extracting the effective components of white peony root. Background Technology

[0002] The main active ingredients of white peony root are monoterpenoid glycosides such as paeoniflorin, which also suffer from easy enzymatic degradation and thermal instability. In addition, white peony root is rich in peony polysaccharides, which are also an important active ingredient. Traditional processes struggle to efficiently extract paeoniflorin while preserving the natural structure of the polysaccharides. To overcome the limitations of water-boiling methods in extracting active components of traditional Chinese medicine, existing technologies have provided an extraction technique using pulsed discharge plasma. However, the extraction efficiency of pulsed discharge plasma technology, especially for heat-sensitive active components, needs further improvement. Summary of the Invention

[0003] Purpose of the invention: In order to solve the problems existing in the prior art, this application provides a method for extracting the effective components of white peony. The solution of this application can quickly inhibit enzyme activity and prevent paeoniflorin from being hydrolyzed by coexisting enzymes; it can achieve efficient extraction of paeoniflorin at low temperature and ensure the structural integrity of macromolecular active components such as peony polysaccharides. The solution of this application can also improve extraction efficiency and shorten the production cycle.

[0004] Technical solution: This application provides a method for extracting the effective components of white peony root, including the following steps: (1) Prepare a white peony suspension and send the white peony suspension into the processing chamber; (2) A needle plate electrode structure is provided in the processing chamber. The needle plate electrode structure is connected to the high-frequency pulse power supply to apply high-voltage pulse treatment to the white peony suspension in the processing chamber. (3) The processed extract is concentrated under reduced pressure to obtain the active extract.

[0005] The technical solution of this application can quickly inactivate the hydrolytic enzymes in white peony, preventing the effective components such as paeoniflorin from being enzymatically degraded; and can quickly complete the extraction at a low temperature of 25℃~30℃, avoiding the destruction of heat-sensitive glycoside components.

[0006] The extraction process described in this application can improve the selectivity of the target components and reduce the dissolution of impurities.

[0007] In some embodiments, the ratio of the white peony root mixture to the liquid is 1:(15~20) g / mL. In other embodiments, the solvent for the white peony root suspension of this application is pure water.

[0008] In some embodiments, the needle plate electrode structure includes an electrode plate and an electrode needle, wherein the distance between the electrode plate and the electrode needle is 3mm to 5mm.

[0009] In some embodiments, the electrode needle includes an electrode needle body, and the outer side of the electrode needle body has a first coating, the thickness of which is 1~3μm.

[0010] In some embodiments, the electrode needle is made of titanium, and the first coating is made of platinum.

[0011] In some embodiments, a flow channel is provided on the inner side of the electrode needle body.

[0012] In some embodiments, the top end of the electrode needle body has a sloping structure.

[0013] In some embodiments, the flow rate of the white peony suspension is 200 mL / min to 300 mL / min.

[0014] In some embodiments, a 4kV~5kV high voltage pulse is applied to the needle plate electrode.

[0015] In some embodiments, the pulse processing time is 8 to 12 seconds.

[0016] In some embodiments, the pulse processing temperature is 25°C to 30°C.

[0017] In some embodiments, a 100MPa to 150MPa instantaneous shock wave is applied during the treatment of the white peony mixture.

[0018] In some embodiments, the pulse width of the pulse applied during the treatment of the white peony mixture is 10-20 mm.

[0019] In some embodiments, the pulse frequency is 6kHz to 8kHz.

[0020] Beneficial effects: This application discloses a method for extracting effective components of Paeonia lactiflora, including the following steps: (1) preparing a Paeonia lactiflora suspension and sending the Paeonia lactiflora suspension into a processing chamber; (2) the processing chamber is provided with a needle plate electrode structure, the needle plate electrode structure is connected to the high-frequency pulse power supply, and high-voltage pulse treatment is applied to the Paeonia lactiflora suspension in the processing chamber; (3) the treated extract is concentrated under reduced pressure to obtain an active extract. Compared with the prior art, the technical solution of this application can achieve the following effects: (1) Enzyme activity control and component protection: The instantaneous high-energy field of pulsed plasma can effectively destroy the spatial structure of enzyme proteins, realize rapid enzyme inactivation, and provide a stable extraction environment for paeoniflorin. Low temperature conditions ensure that paeoniflorin and peony polysaccharide do not undergo thermal denaturation; (2) High efficiency release: Under the parameters of 4~5kV and 10-20μs, through the synergistic effect of electroporation and shock wave, paeoniflorin can be efficiently released from the cell sap and polysaccharide from the cell wall and intracellular space, achieving an extremely high extraction rate within 8~12 seconds; (3) The extraction process of this application shortens the extraction process of several hours to the second level, greatly improving production efficiency, reducing overall cost, and ensuring the stability and high quality of the extract's active ingredients. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a chromatogram of the extraction of effective components from white peony root according to an embodiment of this application; Figure 2 This is a schematic diagram of the liquid phase discharge plasma device in the embodiments of this application; Figure 3 This is a schematic diagram of the electrode needle structure in an embodiment of this application; Figure 4 for Figure 3 A schematic diagram of the structure of part A in the diagram; Reference numerals: 10-Reaction device, 100-Equipment body, 101-Electrode wire, 102-Fixing plate, 103-Electrical control connector, 104-Current probe, 105-Voltage probe, 106-Electrode plate, 110-Electrode needle, 111-Electrode needle body, 112-First coating, 113-Flow channel, 200-First cavity, 20-Airflow device, 21-Flow meter, 300-Second cavity, 30-Detection device, 31-Processor, 40-Pulse voltage generator, 50-Oscilloscope. Detailed Implementation

[0023] It should be noted that the following detailed descriptions are exemplary and intended to provide further explanation of this application. Unless otherwise specified, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0024] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application. In addition, in the description of this application, the term "comprising" means "including but not limited to". The terms first, second, third, etc. are used only as illustrative purposes and do not impose numerical requirements or establish an order. Various embodiments of this application may exist in the form of a range; it should be understood that the description in the form of a range is only for convenience and conciseness and should not be construed as a hard limitation on the scope of this application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single values ​​within that range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which applies regardless of the range. Additionally, whenever a numerical range is specified in this document, it means that any referenced number (fraction or integer) within the range is included.

[0025] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art described herein. While only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this application. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail. Unless otherwise stated, “%” means percentage based on mass.

[0026] Example 1: To improve the extraction efficiency of active substances from white peony root, this application provides a structure of liquid-phase discharge plasma. The structure of the liquid-phase discharge plasma of this application is as follows: Figure 2As shown, the liquid phase discharge plasma device in this embodiment includes a reaction device 10, which includes a device body 100. In some embodiments, the device body 100 has a cylindrical structure and is made of a non-conductive material, such as acrylic. In some specific embodiments, the height of the device body 100 is 20cm and the diameter is 30cm. The volume of the device body 100 can be adjusted as needed. Figure 2 and Figure 3 As shown, the device body 100 is provided with a plurality of electrode needles 110. In some embodiments, the plurality of electrode needles 110 are evenly distributed in a circular shape inside the device body 100 and are fixed by a fixing plate 102.

[0027] In some embodiments, there is a gap between the bottom ends of a plurality of electrode needles 110 and the bottom of the device body 100, for gas to be sent from the airflow device 20 to the bottom of the device body 100. The fixing plate 102 and the device body 100 form a first cavity 200. The first cavity 200 is connected to the air outlet of the airflow device 20. The gas sent from the airflow device 20 is distributed in the first cavity 200. The gas is sent from the gap at the bottom of the electrode needles 110 into the flow channel 113 of the electrode needles 110.

[0028] In some embodiments, the bottom of the electrode needle 110 is connected to a pulse voltage generator 40 via an electrode wire 101. The pulse voltage generator 40 provides AC high-voltage pulse power, providing bipolar pulses. The electrode needle 110, connected via the electrode wire 101, serves as the high-voltage electrode of the reaction device 10. An electrode plate 106, a low-voltage electrode, is disposed above the electrode needle 110 and is welded to the inner wall of the device body 100. In some embodiments, the distance between the top of the electrode needle 110 and the electrode plate 106 is 3mm to 15mm. This distance is used to control the field strength and is adjusted according to the type of medicinal material and the active substance to be extracted. In some embodiments, the electrode plate in this application is a 0.25mm thick stainless steel annular electrode plate.

[0029] In some embodiments, the top of the electrode plate 106 is connected to an oscilloscope 50, and the voltage probe 105 and current probe 104 are used to detect the waveforms of the voltage and current between the two electrodes and display and store them on the oscilloscope 50.

[0030] In some embodiments, the electrode plate 106, the fixing plate 102, and the side wall of the device body 100 form a second cavity 300, which is connected to the detection device 30. In some specific embodiments, the detection device 30 is a high-performance liquid chromatograph. The processed drug solution is tracked and detected by high-performance liquid chromatography and analyzed by processor 31. The processor 31 can be a computer device dedicated to the detection device 30.

[0031] In some embodiments, the electrode needles 110 in this application are distributed in multiple circumferential layers, such as using 7 to 10 electrode needles 110. In some specific embodiments, the electrode needle 110 includes an electrode needle body 111, the top of which has a sloping structure. Using a flat needle-like structure without a sloping structure reduces the extraction efficiency of active substances in traditional Chinese medicine by 5 to 10%. It can be seen that the sloping structure design of this application improves the plasma generation efficiency. This structure uses a needle-plate electrode structure. Gas enters the electrode needle body 111 from the flow channel and exits from the top of the electrode needle body 111. The air and the liquid medicine achieve more complete contact. The gas and the pulse current generated by the electrode needle body 111 work together to generate more plasma to destroy the cell tissue of the medicinal material and promote the dissolution of the active ingredients. This tip discharge mode combined with gas infusion will form more plasma channels. The plasma channels contain highly ionized fluids in a high-pressure and high-temperature state. Once the plasma channels are formed, they will diffuse outward. The mechanical inertia of the surrounding water will resist this expansion, resulting in the generation of extremely high pressure. The magnitude of pressure change is determined by the ratio of the heating rate to the difference between the speed of sound and the expansion rate. The heating rate is the time derivative of the dissipated power. The energy stored in the plasma channel is gradually dissipated in the form of thermal radiation and mechanical work; this dissipation process is relatively slow compared to the plasma formation process.

[0032] Before the discharge wave, the high pressure generated in the plasma is conducted to the water interface, forming a strong compression wave (shock wave). Only under extremely high pressures does the compression wave propagate faster than the propagation speed of the diffusing bubble, reaching several times the speed of sound (at a pressure of 6 kbar, the speed of sound is only 1.56 times higher than at normal pressure). The pressure variation range of the shock wave is between 5 and 20 kbar. When the shock wave reaches the free surface, under pressureless conditions, the compression wave at the interface immediately transforms into a tension wave (or rarefaction wave) and is reflected back into the liquid medium, simultaneously propelling water into the air. When the rarefaction wave returns from the water, cavitation occurs. The shock wave, rarefaction wave, and bubble expansion maintain a highly turbulent mixing state in the fluid until all pressures reach equilibrium.

[0033] In some embodiments, a first coating 112 is provided on the outer side of the electrode needle body 111, and a flow channel 113 is provided on the inner side of the electrode needle body 111. In some specific embodiments, the electrode needle body 111 is made of titanium metal, the diameter d1 of the electrode needle body 111 is 1 mm to 1.5 mm, the first coating 112 is made of platinum metal, the thickness of the first coating 112 is 1 μm to 3 μm, and the diameter d2 of the flow channel 113 is 0.2 mm to 0.4 mm. The titanium-plated platinum electrode of this application is mainly characterized by the following aspects: (1) excellent corrosion resistance, the platinum coating (1-3 μm) makes the corrosion rate of the electrode in a strong oxidizing environment (·OH concentration 50~80 μmol / L) <0.001 mm / year, can withstand extreme environments with pH 1~14, and is suitable for various Chinese medicine extraction systems; (2) stable electrochemical performance, suppressing the occurrence of side reactions, adapting to high-frequency pulse conditions, and reducing energy consumption.

[0034] Example 2: This application provides a method for continuous room-temperature extraction of active ingredients from Paeonia lactiflora based on liquid-phase discharge plasma, specifically including the following steps: First, dried Paeonia lactiflora tubers (origin: Bozhou City, Anhui Province) are pulverized through a 40-mesh sieve to obtain coarse powder, which is then mixed with deionized water at a material-to-liquid ratio of 1:15 g / mL to form a uniform suspension; A needle-plate electrode structure (3-5 mm spacing, titanium-plated platinum material) and a high-frequency pulse power supply (6-8 kHz) are used, and the mixture is transported to the electrode area by a peristaltic pump at a flow rate of 200-300 mL / min, and a 4kV-5kV high-voltage pulse is applied for 10±1s, during which the temperature is automatically maintained at 25-30℃; This process generates a 100MPa-150MPa instantaneous shock wave and a turbulent velocity gradient of >500s⁻¹; The extract is coarsely filtered through a 100-mesh sieve and concentrated under reduced pressure at 60℃ to 1 / 5 of the original volume. The specific parameters of samples 1-19, comparative example 1, and comparative example 2 are detailed in Table 1.

[0035] Parameter control: In this application, parameters are controlled in the following ways: the high-frequency pulse power supply is adjusted by changing the input voltage; the peristaltic pump is used to control the flow rate of the input raw materials; the high-frequency pulse power supply is used to control the high-voltage pulse, and the pulse frequency and pulse width can be adjusted; the instantaneous shock wave is controlled by controlling the voltage magnitude, pulse frequency, and pulse width parameters.

[0036] Detection method: The chromatographic column was a Zorbax Eclipse Plus C1000 chromatographic column. 18The column was 250 mm × 4.6 mm, 5 μm; the mobile phase was acetonitrile-0.1% phosphoric acid aqueous solution, with gradient elution: 0–25 min, 5%–18% acetonitrile; 25–30 min, 18% acetonitrile; 30–40 min, 18%–34% acetonitrile; 40–43 min, 34%–38% acetonitrile; 43–46 min, 38%–100% acetonitrile; the acquisition time was 46 min, the flow rate was 1.0 mL / min, the detection wavelength was 244 nm, the column temperature was 25 ℃, and the injection volume was 10 μL.

[0037] Table 1. Extraction process and active component extraction results with different parameters in this application.

[0038] Note: The data analyzed are expressed as mean values, and the number of parallel samples is 3 (n=3).

[0039] The results from samples 1-3 show that, in this application, controlling the distance between the needle electrode and the ring electrode plate affects the distribution and intensity of the electric field, thereby influencing the extraction efficiency of the active components. This application controls the distance between the electrode needle and the electrode plate to 3-5 mm. The instantaneous high-energy field of the pulsed plasma generated under high electric field intensity can effectively disrupt the spatial structure of the enzyme protein, achieving rapid enzyme inactivation and providing a stable extraction environment for paeoniflorin. When the distance between the electrode needle and the electrode plate is controlled at 4 mm, the extraction efficiency of monoterpenoid glycosides, such as paeoniflorin, is the highest.

[0040] As can be seen from the data of samples 4 to 19 of this application, by controlling the voltage, pulse width, and pulse frequency, and thus controlling the instantaneous shock wave at 100-150 MPa, the extraction efficiency of monoterpenoid glycosides such as paeoniflorin can be improved.

[0041] As can be seen from the data of Sample 2 and Comparative Example 1, this application further optimizes the discharge characteristics by changing the structure of the electrode needle: the electron work function of the platinum coating surface (5.3eV) is significantly lower than that of pure titanium (4.3eV), the discharge initiation voltage is reduced by 15-20%, the plasma luminescence efficiency is increased by 30%, and the titanium-platinum electrode has a unique surface effect, providing more active sites, increasing the bubble nucleation density by 5 times (>1000 bubbles / cm²·s), and enhancing the turbulence intensity by 30% (Reynolds number Re>5000), thereby improving the extraction efficiency of monoterpenoid glycosides such as paeoniflorin.

[0042] Increasing the energy of a single pulse may enhance mass transfer during the extraction process, allowing substances to be released or distributed into the extractant more quickly. Data from Sample 2 and Comparative Example 2 show that the applicant's integrated design of the gas introduced through the original pores with the flow channel of the electrode needle allows the introduced gas to be used to increase plasma generation, significantly improving the extraction efficiency of active ingredients from traditional Chinese medicine.

[0043] In the above embodiments, the descriptions of each embodiment have different focuses. For parts not described in detail in a certain embodiment, please refer to the relevant descriptions in other embodiments.

[0044] The above provides a detailed description of a method for extracting effective components from Paeonia lactiflora according to the embodiments of this application. Specific examples have been used to illustrate the principles and implementation methods of this application. The description of the above embodiments is only for the purpose of helping to understand the method and core ideas of this application. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the ideas of this application. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A method for extracting the effective components of white peony root, characterized in that, Includes the following steps: (1) Prepare a white peony suspension and send the white peony suspension into the processing chamber; (2) A needle plate electrode structure is provided in the processing chamber. The needle plate electrode structure is connected to the high-frequency pulse power supply to apply high-voltage pulse treatment to the white peony suspension in the processing chamber. (3) The processed extract is concentrated under reduced pressure to obtain the active extract.

2. The method for extracting the effective components of white peony root according to claim 1, characterized in that, The needle plate electrode structure includes an electrode plate and an electrode needle, and the distance between the electrode plate and the electrode needle is 3mm to 5mm.

3. The method for extracting the effective components of white peony root according to claim 1, characterized in that, The electrode needle includes an electrode needle body, and the outer side of the electrode needle body has a first coating, the thickness of which is 1~3μm.

4. The method for extracting the effective components of white peony root according to claim 3, characterized in that, The electrode needle is made of titanium, and the first coating is made of platinum.

5. The method for extracting the effective components of white peony root according to claim 3, characterized in that, A flow channel is provided on the inner side of the electrode needle body.

6. The method for extracting the effective components of white peony root according to claim 3, characterized in that, The top of the electrode needle body has a sloping structure.

7. The method for extracting the effective components of white peony root according to claim 1, characterized in that, A 4kV~5kV high voltage pulse is applied to the needle plate electrode.

8. The method for extracting the effective components of white peony root according to claim 1, characterized in that, The pulse processing time is 8 to 12 seconds.

9. The method for extracting the effective components of white peony root according to claim 1, characterized in that, The pulse width applied during the treatment of the white peony suspension is 10-20 mm.

10. The method for extracting the effective components of white peony root according to claim 1, characterized in that, The pulse frequency is 6kHz~8kHz.

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