Efficient notoginsenoside extraction and separation process based on supercritical CO2 extraction

Abstract

The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to a high-efficiency notoginsenoside extraction and separation process based on supercritical CO2 extraction, which comprises the following steps: raw material pretreatment: selecting a high-quality pseudo-ginseng raw material, and drying the pseudo-ginseng raw material until the water content is lower than 5%; by optimizing pretreatment, extraction parameters, pre-soaking and the synergistic effect of supercritical CO2 and ethanol, the extraction rate of notoginsenoside is greatly improved, the extraction rate is far better than that of the traditional method, the product quality is excellent, the whole process is low-temperature closed, the saponin activity is prevented from being damaged by high temperature, the content of effective components is high, the purity is excellent, CO2 is recycled, and the method is suitable for industrial production. The method has the advantages of reduction of organic solvent consumption, reduction of pollution and recovery cost, substantial reduction of energy consumption compared with the traditional technology, simple operation, easy parameter control, high equipment automation degree, continuous industrial production, obvious efficiency improvement, simplified process, integration of extraction and separation, no need of subsequent complex treatment, shortened production period, and prominent comprehensive benefits.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine extraction, and in particular to a high-efficiency extraction and separation process of notoginseng saponins based on supercritical CO2 extraction. Background Art

[0002] Panax notoginseng leaves, derived from the Araliaceae plant Panax notoginseng, have the properties of dispersing blood stasis, arresting bleeding, reducing swelling, and alleviating pain. They are commonly used to treat hematemesis, epistaxis, hematochezia, bleeding from trauma, swelling and pain from falls, and carbuncles. The Compendium of Materia Medica states that the stems and leaves of Panax notoginseng "treat fractures and falls, stopping bleeding immediately when applied, and dissipating bruises overnight, with other benefits similar to the root." Modern chemical analysis has shown that the main components of Panax notoginseng leaves are ginsenosides Rb1, Rb3, and Re, gypenosides, and notoginsenosides Fa, Fc, and Fe. Modern pharmacological studies have shown that total saponins from Panax notoginseng leaves have lipid-lowering, calming, and sedative effects, enhancing immune function, and prolonging lifespan in experimental animals. They also exhibit significant analgesic effects against pain induced by both thermal and chemical stimuli. This analgesic effect is achieved by raising the pain threshold and inhibiting central and peripheral nociceptive factors, with a rapid onset and long-lasting effect. They also have a vasoconstrictive effect on cerebral blood vessels and inhibit platelet aggregation.

[0003] In general, notoginseng and notoginseng total saponins are primarily obtained through the extraction of Panax notoginseng medicinal materials. Currently, the utilization of Panax notoginseng resources primarily focuses on the extraction and separation of notoginseng total saponins and their monomers from Panax notoginseng. In the prior art, the method for extracting notoginseng total saponins is mainly based on alcohol extraction of Panax notoginseng, and the extract often contains notoginseng. If this is not utilized, notoginseng would be wasted. Furthermore, extraction and separation processes often tend to increase the yield of notoginseng total saponins and take certain measures to reduce impurity content, which can easily lead to the loss of other active ingredients in Panax notoginseng, such as notoginseng. Summary of the Invention

[0004] In view of the deficiencies in the prior art, the present invention provides a highly efficient extraction and separation process for notoginseng saponins based on supercritical CO2 extraction, which solves the problem that, in general, notoginseng saponins and notoginseng total saponins are mainly obtained by extracting notoginseng medicinal materials. At present, the utilization of notoginseng resources mainly focuses on the extraction and separation of notoginseng total saponins and their monomers in notoginseng. In the prior art, the method for extracting notoginseng total saponins is mainly based on alcohol extraction of notoginseng, and the extract often also contains notoginseng saponins. If it is not utilized, it will result in a waste of notoginseng saponins. At the same time, the extraction and separation process methods often tend to increase the yield of notoginseng total saponins and take certain measures to reduce the impurity content, which will easily cause the loss of other active ingredients in notoginseng, such as notoginseng saponins.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] As a preferred technical solution of the present invention, raw material pretreatment: select high-quality Panax notoginseng raw material, dry it to a moisture content of less than 5%, and then use a crushing device to crush the Panax notoginseng into 50-100 mesh.

[0007] As a preferred technical solution of the present invention, the extraction agent is selected and prepared by selecting 60%-70% ethanol as an entrainer, which synergistically acts with supercritical CO2 to enhance the solubility of notoginseng saponins. The crushed notoginseng and ethanol are placed in an extraction kettle and an ethanol storage tank, respectively, at a mass ratio of 1:5 to 1:7, for later use.

[0008] As a preferred technical solution of the present invention, pre-soaking treatment: soak 50-100 mesh Panax notoginseng and 60%-70% ethanol according to the above ratio at room temperature for 10-15 hours.

[0009] As a preferred technical solution of the present invention, supercritical CO2 extraction: transfer the pre-soaked Panax notoginseng to an extraction kettle, turn on the heating device, raise the temperature of the extraction kettle to 55-65°C, and simultaneously heat the temperature of the separation kettle to 45-55°C. Open the carbon dioxide storage tank, and pump CO2 into the extraction kettle via a CO2 plunger pump to pressurize the extraction kettle. When the pressure of the extraction kettle reaches 25-32MPa, adjust the carbon dioxide flow rate to 12-24L / h, maintain the temperature and pressure conditions, and carry out the extraction operation for 2.5-3 hours.

[0010] As a preferred technical solution of the present invention, saponin separation: The supercritical CO2 fluid containing notoginsenosides exiting the extraction kettle enters a separation kettle. In the separation kettle, the CO2 is separated from the notoginsenosides by reducing the pressure or increasing the temperature. The CO2 becomes gaseous and can be recirculated through a pipeline back to the carbon dioxide storage tank for recycling. The separated notoginsenosides are collected from the extraction outlet at the bottom of the separation kettle.

[0011] Compared with the prior art, the present invention provides a highly efficient extraction and separation process for notoginseng saponins based on supercritical CO2 extraction, which has the following beneficial effects:

[0012] 1. This efficient extraction and separation process of Panax notoginseng saponins based on supercritical CO2 extraction, by optimizing pretreatment, extraction parameters and pre-soaking, and the synergistic effect of supercritical CO2 and ethanol, greatly improves the extraction rate of Panax notoginseng saponins, far exceeding traditional methods. The whole process is kept at low temperature and sealed to avoid high temperature destruction of saponin activity, and the content of active ingredients is high and the purity is excellent.

[0013] 2. This efficient extraction and separation process of Panax notoginseng saponins based on supercritical CO2 extraction reduces organic solvent consumption, pollution and recovery costs through the recycling of CO2, and significantly reduces energy consumption compared to traditional processes. It is easy to operate, parameters are easy to control, the equipment has a high degree of automation, and can be used for continuous industrial production. The efficiency is significantly improved, the process is simplified, and extraction and separation are integrated, eliminating the need for subsequent complex treatment and shortening the production cycle. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a flow chart of the process of the present invention. DETAILED DESCRIPTION

[0015] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0016] Example

[0017] See also Figure 1 This embodiment includes the following technical features: Raw material pretreatment: Select high-quality Panax notoginseng raw material and dry it to a moisture content of less than 5%. Then, use a crushing device to crush the Panax notoginseng to 50-100 mesh, increasing the contact area with the extractant and improving extraction efficiency. This pretreatment method effectively breaks down the cell structure of Panax notoginseng, allowing the subsequent extractant to more easily penetrate the cells, fully contact with the notoginseng saponins, and dissolve them.

[0018] In this embodiment, the extraction agent is selected and prepared as follows: ethanol with a content of 60%-70% is selected as an entrainer, which works synergistically with supercritical CO2 to enhance the solubility of Panax notoginseng saponins. The crushed Panax notoginseng and ethanol are placed in an extraction kettle and an ethanol storage tank respectively at a mass ratio of 1:5 to 1:7 for standby use. Ethanol, as an entrainer, can change the polarity of supercritical CO2, thereby improving the solubility of polar substances such as Panax notoginseng saponins, and can significantly improve the extraction effect compared to using supercritical CO2 alone;

[0019] In this embodiment, the pre-soaking treatment involves soaking 50-100 mesh Panax notoginseng in 60%-70% ethanol at room temperature for 10-15 hours. The pre-soaking process helps the ethanol fully penetrate the interior of the Panax notoginseng cells, disrupting the cell structure and further creating favorable conditions for subsequent supercritical CO2 extraction. After pre-soaking, the Panax notoginseng cells swell and the cell wall permeability increases, allowing supercritical CO2 to more smoothly enter the cells during extraction, dissolving and extracting the Panax notoginseng saponins.

[0020] Supercritical CO2 Extraction: Transfer the pre-soaked Panax notoginseng to the extraction kettle. Turn on the heating device and raise the temperature of the extraction kettle to 55-65°C. Simultaneously, heat the separation kettle to 45-55°C. Within this temperature range, the solubility and mass transfer properties of supercritical CO2 are ideal, effectively improving the extraction rate of notoginseng saponins while preventing damage to the active ingredients of the saponins caused by excessive temperatures. Open the CO2 storage tank and pump CO2 into the extraction kettle using a CO2 plunger pump to pressurize the extraction kettle. When the pressure in the extraction kettle reaches 25-32 MPa, adjust the CO2 flow rate to 12-24 L / h. Maintaining these temperature and pressure conditions, continue the extraction process for 2.5-3 hours. The appropriate pressure and flow rate ensure sufficient contact and mass transfer between the supercritical CO2 and the Panax notoginseng raw material, ensuring the maximum extraction of notoginseng saponins. To further improve the extraction rate, multiple extractions can be used. For example, the crushed Panax notoginseng and ethanol are placed in an ethanol storage tank and an extraction kettle at a mass ratio of 1:7, and the extraction kettle is heated to 60°C and the separation kettle is heated to 50°C through a heating device; the carbon dioxide storage tank is opened and the extraction kettle is pressurized. When the pressure of the extraction kettle reaches 30MPa, the carbon dioxide flow rate is adjusted to 18L / h, and the temperature and pressure are maintained. Three extractions are performed, each extraction time is 1 hour. Multiple extractions can make the Panax notoginseng saponins in the raw materials be more fully extracted, further improving the extraction rate.

[0021] Saponin separation: The supercritical CO2 fluid containing notoginseng saponins coming out of the extraction kettle enters the separation kettle. In the separation kettle, CO2 is separated from notoginseng saponins by reducing the pressure or increasing the temperature. CO2 becomes gaseous and can be refluxed to the carbon dioxide storage tank through a pipeline for recycling; the separated notoginseng saponins are collected from the extraction outlet at the bottom of the separation kettle. In this process, the separation kettle can be arranged in parallel with a primary separation kettle and a secondary separation kettle to further improve the separation effect. The bottom ends of the primary separation kettle and the secondary separation kettle are both provided with extraction outlets, and the top ends are respectively provided with reflux pipes connected to the CO2 storage tank and the ethanol storage tank to achieve the recovery and reuse of CO2 and ethanol. This separation method can effectively separate the extract from the extractant and recover the extractant at the same time, reducing production costs and meeting environmental protection requirements.

[0022] Example 1:

[0023] Raw material pretreatment: 1000g of high-quality Panax notoginseng raw material was selected, dried to a moisture content of 4%, and then crushed to 80 mesh using a grinder;

[0024] Selection and preparation of extraction agent: Place the crushed Panax notoginseng into the extraction kettle, take another 60% ethanol solution, and place 1667g of ethanol into the ethanol storage tank according to the mass ratio of Panax notoginseng to ethanol of 1:6.

[0025] Pre-soaking treatment: Mix the Panax notoginseng in the extraction kettle with the ethanol in the ethanol storage tank and soak at room temperature for 12 hours;

[0026] Supercritical CO2 extraction: Transfer the pre-soaked Panax notoginseng to the extraction kettle. Turn on the heating device and raise the temperature of the extraction kettle to 60°C. Heat the separation kettle to 50°C. Open the CO2 storage tank and pump CO2 into the extraction kettle using a CO2 plunger pump. When the pressure in the extraction kettle reaches 30MPa, adjust the CO2 flow rate to 18L / h. Maintain the temperature and pressure and continue the extraction operation for 3 hours.

[0027] Saponin Separation: Supercritical CO2 fluid containing notoginsenosides enters the separation kettle, where the pressure is reduced to separate the CO2 from the notoginsenosides. The CO2 is then returned to the CO2 storage tank via a pipeline, and the separated notoginsenosides are collected from the extraction outlet at the bottom of the separation kettle.

[0028] Example 2:

[0029] Raw material pretreatment: 1500g of high-quality Panax notoginseng raw material was selected, dried to a moisture content of 3%, and crushed to 100 mesh;

[0030] Extraction agent selection and preparation: According to the mass ratio of Panax notoginseng to ethanol of 1:7, 2143g of 70% ethanol solution was placed in the ethanol storage tank, and the crushed Panax notoginseng was placed in the extraction kettle;

[0031] Pre-soaking treatment: soak Panax notoginseng in ethanol at room temperature for 15 hours;

[0032] Supercritical CO2 extraction: The extraction kettle temperature was raised to 65°C, and the separation kettle temperature was raised to 55°C. The pressure was increased to 32 MPa, and the CO2 flow rate was adjusted to 24 L / h. The extraction was continued for 2.5 hours.

[0033] Saponin Separation: Supercritical CO2 fluid containing notoginsenosides enters the separation kettle, where the pressure is reduced to separate the CO2 from the notoginsenosides. The CO2 is then returned to the CO2 storage tank via a pipeline, and the separated notoginsenosides are collected from the extraction outlet at the bottom of the separation kettle.

[0034] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A highly efficient extraction and separation process for notoginseng saponins based on supercritical CO2 extraction, characterized by: The process includes raw material pretreatment: selecting high-quality Panax notoginseng raw materials, drying them to a moisture content of less than 5%, and then crushing them into 50-100 mesh using a crushing device. Extraction agent selection and preparation: Use 60%-70% ethanol as an entrainer, which synergizes with supercritical CO2 to enhance the solubility of notoginseng saponins. Place crushed notoginseng and ethanol in an extraction kettle and an ethanol storage tank, respectively, at a mass ratio of 1:5 to 1:7, for later use. Pre-soaking treatment: soak 50-100 mesh Panax notoginseng with 60%-70% ethanol according to the above ratio at room temperature for 10-15 hours. Supercritical CO2 extraction: Transfer the pre-soaked Panax notoginseng to the extraction kettle. Turn on the heating device and raise the temperature of the extraction kettle to 55-65°C. Simultaneously, heat the separation kettle to 45-55°C. Open the CO2 storage tank and pump CO2 into the extraction kettle via a CO2 plunger pump to pressurize the extraction kettle. When the pressure in the extraction kettle reaches 25-32MPa, adjust the CO2 flow rate to 12-24L / h. Maintain the temperature and pressure conditions and continue the extraction operation for 2.5-3 hours. Saponin separation: The supercritical CO2 fluid containing Panax notoginseng saponins coming out of the extraction kettle enters the separation kettle. In the separation kettle, the CO2 is separated from the notoginsenosides by reducing the pressure or increasing the temperature. The CO2 becomes gaseous and can be recycled back to the carbon dioxide storage tank through a pipeline. The separated notoginsenosides are collected from the extraction outlet at the bottom of the separation kettle.

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