Method for extracting and separating tectoridin from iridis tectori

Abstract

The invention relates to the technical field of effective extraction of plant components, in particular to a method for extracting and separating tectoridin from rhizoma iridis tectori, which comprises the following steps: 1) raw material pretreatment: cleaning the collected rhizoma iridis tectori medicinal material, removing silt and impurities, and drying at 40-60 DEG C until the weight is constant; according to the method, in the raw material pretreatment stage, the 80-mesh rhizoma iridis tectori powder is adopted, the solid-to-liquid ratio and the volume fraction of the ethanol aqueous solution are optimized, and the ultrasonic-assisted extraction technology is combined, so that the tectoridin can be more sufficiently released. In addition, in the stages of extracting solution concentration and macroporous resin separation, the enrichment efficiency and the recovery rate of the tectoridin are improved by accurately controlling the vacuum decompression condition, the concentration temperature and the elution flow rate.

Description

Technical Field

[0001] The invention relates to the technical field of effective extraction of plant components, in particular to a method for extracting and separating belamcanda glycosides from Sichuan belamcanda chinensis. Background Art

[0002] In the field of effective plant component extraction technology, extracting active ingredients with medicinal value from natural plants has always been a hot topic. As a traditional Chinese medicinal material, the rhizome of Sichuan Shematuria is rich in a variety of bioactive ingredients, among which Belamcanda glycosides are one of its main active ingredients, which has a variety of pharmacological effects, such as anti-inflammatory, antioxidant and anti-tumor. However, how to efficiently and stably extract and separate Belamcanda glycosides from Sichuan Shematuria is still a key issue in current research.

[0003] Due to technical limitations, traditional extraction methods often fail to fully release the active ingredients in plant cells, resulting in low extraction efficiency. At the same time, during the extraction process, due to improper control of conditions such as temperature and pH value, the active ingredients are prone to degradation or transformation, resulting in a large amount of loss. In addition, traditional extraction methods have many steps and complex operations, which not only increases production costs, but also limits its application in large-scale production.

[0004] In order to overcome these problems, researchers began to focus on the selection of extraction conditions, the optimization of the separation process, and the improvement of the purification effect. However, improvements in these aspects are not easy and require comprehensive consideration of multiple factors, such as the characteristics of the raw materials, the selection of solvents, the extraction temperature and time, etc. Therefore, it is particularly important to develop an efficient, stable, and simple method for extracting and separating belamcanda glycosides from Sichuan belamcanda. Summary of the invention

[0005] (I) Purpose of the invention

[0006] In view of this, the purpose of the present invention is to provide a method for extracting and separating belamcanda glycosides from Sichuan belamcanda oleifera, which solves the problems raised in the above background.

[0007] (II) Technical solution

[0008] A method for extracting and separating belamcanda glycosides from Sichuan belamcanda, the method comprising the following steps:

[0009] 1) Raw material pretreatment: The collected Sichuan Belamcanda chinensis medicinal materials are washed, the sand and impurities are removed, and then dried at 40-60° C. to a constant weight; then the dried Sichuan Belamcanda chinensis is crushed to a particle size of 60-100 meshes to obtain Sichuan Belamcanda chinensis powder;

[0010] 2) Solvent extraction: add the powder of Belamcanda chinensis to a 50% to 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 to 1:12 (g / mL), adjust the pH of the solution to 6 to 7, perform ultrasonic-assisted extraction at 50 to 70°C, and perform a single extraction for 30 to 60 minutes. Repeat the extraction 2 to 3 times and combine the extracts;

[0011] 3) Concentrating the extract: The obtained extract is passed through a vacuum decompression concentration device to evaporate the ethanol solvent at 40-50° C. to obtain a concentrated solution containing water;

[0012] 4) Macroporous resin separation: The concentrated solution is separated by passing through an AB-8 macroporous resin column, first eluted with distilled water until colorless, and then eluted with a 40% to 70% ethanol aqueous solution, and the ethanol eluate is collected to obtain the enriched fraction of belamcanda glycosides;

[0013] 5) Fine separation and purification: The enriched fractions are further purified by reverse phase high performance liquid chromatography (RP-HPLC), using a methanol-water gradient elution system as the mobile phase, collecting the main peak of the Belamcanda glycosides to obtain a purified Belamcanda glycosides solution;

[0014] 6) Drying and finished product preparation: The purified Belamcanda glycoside solution is freeze-dried or spray-dried to prepare a high-purity Belamcanda glycoside solid powder.

[0015] Preferably, the particle size of the Ilex serrata powder in step (1) is preferably 80 mesh to improve the extraction efficiency.

[0016] Preferably, the frequency of the ultrasonic-assisted extraction in step (2) is 20 to 40 kHz, and the ultrasonic power is 100 to 300 W to improve the extraction rate.

[0017] Preferably, the vacuum decompression condition in step (3) is -0.08 to -0.09 MPa, and the concentration temperature is preferably 45° C. to avoid thermal degradation of the active ingredient.

[0018] Preferably, the flow rate of the resin elution process in step (4) is controlled at 1 to 3 mL / min to ensure the separation effect and the recovery rate of belamcanda glycosides.

[0019] Preferably, the reverse phase high performance liquid chromatography purification conditions in step (5) are: the column temperature is controlled at 30° C., the flow rate is 1.0 mL / min, and the detection wavelength is 277 nm.

[0020] Preferably, the freeze-drying temperature in step (6) is -40°C to -50°C, and the vacuum degree is 0.1 to 0.2 mbar to ensure the stability and purity of the belamcanda glycosides.

[0021] It can be seen from the above technical solutions that the present application has the following beneficial effects:

[0022] 1. The invention uses 80-mesh Sichuan Belamcanda powder in the raw material pretreatment stage, optimizes the solid-liquid ratio and the volume fraction of ethanol-water solution, and combines ultrasound-assisted extraction technology to release Belamcanda glycosides more fully. In addition, in the stage of extract concentration and macroporous resin separation, the enrichment efficiency and recovery rate of Belamcanda glycosides are improved by precisely controlling the vacuum decompression conditions, concentration temperature and elution flow rate.

[0023] 2. The invention avoids the degradation or transformation of active ingredients such as Belamcanda glycosides during the extraction process by adjusting the pH value of the solution to the neutral range and selecting appropriate extraction temperature and ultrasonic conditions. At the same time, the temperature and vacuum degree are strictly controlled during the concentration and drying stages to ensure the stability and purity of Belamcanda glycosides. These mild extraction conditions not only improve the extraction efficiency of Belamcanda glycosides, but also ensure the integrity of its pharmacological activity.

[0024] 3. The invention has been carefully designed and optimized in every step from raw material pretreatment to finished product preparation, making the entire extraction process smoother and more efficient. In addition, the equipment and materials used in the method are relatively common, reducing production costs and investment risks. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the process of the present invention. DETAILED DESCRIPTION

[0026] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, and use. It should be understood that in all of these figures, the same or similar reference numerals indicate the same or similar parts and features. The various drawings only schematically represent the concepts and principles of the embodiments of the present disclosure, and do not necessarily show the specific dimensions and proportions of the various embodiments of the present disclosure. Specific parts in specific drawings may be exaggerated to illustrate the relevant details or structures of the embodiments of the present disclosure.

[0027] See also Figure 1 , an embodiment provided by the present invention:

[0028] A method for extracting and separating belamcanda glycosides from Sichuan belamcanda, the method comprising the following steps:

[0029] 1) Raw material pretreatment: The collected Sichuan Belamcanda chinensis medicinal materials are washed, the sand and impurities are removed, and then dried at 40-60° C. to a constant weight; then the dried Sichuan Belamcanda chinensis is crushed to a particle size of 60-100 meshes to obtain Sichuan Belamcanda chinensis powder;

[0030] 2) Solvent extraction: add the powder of Belamcanda chinensis to a 50% to 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 to 1:12 (g / mL), adjust the pH of the solution to 6 to 7, perform ultrasonic-assisted extraction at 50 to 70°C, and perform a single extraction for 30 to 60 minutes. Repeat the extraction 2 to 3 times and combine the extracts;

[0031] 3) Concentrating the extract: The obtained extract is passed through a vacuum decompression concentration device to evaporate the ethanol solvent at 40-50° C. to obtain a concentrated solution containing water;

[0032] 4) Macroporous resin separation: The concentrated solution is separated by passing through an AB-8 macroporous resin column, first eluted with distilled water until colorless, and then eluted with a 40% to 70% ethanol aqueous solution, and the ethanol eluate is collected to obtain the enriched fraction of belamcanda glycosides;

[0033] 5) Fine separation and purification: The enriched fractions are further purified by reverse phase high performance liquid chromatography (RP-HPLC), using a methanol-water gradient elution system as the mobile phase, collecting the main peak of the Belamcanda glycosides to obtain a purified Belamcanda glycosides solution;

[0034] 6) Drying and finished product preparation: The purified Belamcanda glycoside solution is freeze-dried or spray-dried to prepare a high-purity Belamcanda glycoside solid powder.

[0035] Furthermore, the particle size of the Belamcanda chinensis powder in step (1) is preferably 80 mesh to improve the extraction efficiency. Finer powder can increase the contact area with the solvent, making the active ingredients such as Belamcanda glycosides easier to be dissolved and extracted by the solvent.

[0036] Furthermore, the ultrasound-assisted extraction frequency in step (2) is 20 to 40 kHz, and the ultrasound power is 100 to 300 W to improve the extraction rate. The cavitation effect and mechanical effect generated by ultrasound can destroy the plant cell wall and promote the release of active ingredients in the cell.

[0037] Furthermore, the vacuum decompression conditions in step (3) are -0.08 to -0.09 MPa, and the concentration temperature is preferably 45°C to avoid thermal degradation of the active ingredients. This optimization not only ensures the stability of active ingredients such as belamcanda glycosides, but also improves the purity and quality of the concentrate, laying a good foundation for subsequent macroporous resin separation and purification.

[0038] Furthermore, the flow rate of the resin elution process in step (4) is controlled at 1 to 3 mL / min to ensure the separation effect and the recovery rate of scutellaria baicalensis glycosides. The appropriate flow rate can ensure sufficient contact and exchange between the resin and the extract, thereby effectively separating the target components such as scutellaria baicalensis glycosides.

[0039] Furthermore, the reverse-phase HPLC purification conditions in step (5) are: the column temperature is controlled at 30°C, the flow rate is 1.0 mL / min, and the detection wavelength is 277 nm. By precisely controlling the detection wavelength, the peak shape and content of scutellaria baicalensis can be accurately monitored, providing a reliable basis for subsequent quality control and product development.

[0040] Furthermore, the freeze-drying temperature in step (6) is -40°C to -50°C, and the vacuum degree is 0.1 to 0.2 mbar to ensure the stability and purity of the belamcanda glycosides. The freeze-drying technology can quickly sublime the water in the extract, thereby avoiding degradation or inactivation of the active ingredients due to long-term high-temperature drying.

[0041] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda, characterized in that: The method comprises the following steps: 1) Raw material pretreatment: The collected Sichuan Belamcanda chinensis medicinal materials are washed, the sand and impurities are removed, and then dried at 40-60° C. to a constant weight; then the dried Sichuan Belamcanda chinensis is crushed to a particle size of 60-100 meshes to obtain Sichuan Belamcanda chinensis powder; 2) Solvent extraction: add the powder of Belamcanda chinensis to a 50% to 70% ethanol aqueous solution at a solid-liquid ratio of 1:8 to 1:12 (g / mL), adjust the pH of the solution to 6 to 7, perform ultrasonic-assisted extraction at 50 to 70°C, and perform a single extraction for 30 to 60 minutes. Repeat the extraction 2 to 3 times and combine the extracts; 3) Concentrating the extract: The obtained extract is passed through a vacuum decompression concentration device to evaporate the ethanol solvent at 40-50° C. to obtain a concentrated solution containing water; 4) Macroporous resin separation: The concentrated solution is separated by passing through an AB-8 macroporous resin column, first eluted with distilled water until colorless, and then eluted with a 40% to 70% ethanol aqueous solution, and the ethanol eluate is collected to obtain the enriched fraction of belamcanda glycosides; 5) Fine separation and purification: The enriched fractions are further purified by reverse phase high performance liquid chromatography (RP-HPLC), using a methanol-water gradient elution system as the mobile phase, collecting the main peak of the Belamcanda glycosides to obtain a purified Belamcanda glycosides solution; 6) Drying and finished product preparation: The purified Belamcanda glycoside solution is freeze-dried or spray-dried to prepare a high-purity Belamcanda glycoside solid powder.

2. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda according to claim 1, characterized in that: The particle size of the Belamcanda chinensis powder in step (1) is preferably 80 meshes to improve the extraction efficiency.

3. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda according to claim 1, characterized in that: The ultrasonic-assisted extraction frequency in step (2) is 20 to 40 kHz, and the ultrasonic power is 100 to 300 W to improve the extraction rate.

4. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda according to claim 1, characterized in that: The vacuum decompression condition in step (3) is -0.08 to -0.09 MPa, and the concentration temperature is preferably 45° C. to avoid thermal degradation of the active ingredient.

5. The method for extracting and separating belamcanda glycosides from Sichuan belamcanda var. The flow rate of the resin elution process in step (4) is controlled at 1-3 mL / min to ensure the separation effect and the recovery rate of belamcanda glycosides.

6. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda according to claim 1, characterized in that: The reverse-phase high performance liquid chromatography purification conditions in step (5) are: the column temperature is controlled at 30° C., the flow rate is 1.0 mL / min, and the detection wavelength is 277 nm.

7. A method for extracting and separating belamcanda glycosides from Sichuan belamcanda according to claim 1, characterized in that: The freeze-drying temperature in step (6) is -40°C to -50°C, and the vacuum degree is 0.1 to 0.2 mbar to ensure the stability and purity of the belamcanda glycosides.

Images