Extraction method of agrimonia extract and extract thereof

Abstract

The application provides an extraction method of a vine tea extract and the extract. Primarily extracted is protocatechuic acid, and the extraction method mainly comprises a processing step, wherein the vine tea is steamed at 110-120 DEG C for 0.5-1.5 h, and then cut into segments for standby. The application also provides an application of the extract, which is used for preparing antioxidant and anti-inflammatory drugs and / or food and / or cosmetics. The application has the advantages that the extraction efficiency of protocatechuic acid is effectively enhanced through the synergistic effect of processing and extraction processes, the extraction rate is greatly increased from 0.1-0.6 mg / g in the prior art to 1-1.4 mg / g, and the increase is significant.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine technology, specifically a method for extracting Agrimonia pilosa extract and the extract thereof. Background Technology

[0002] Agrimony is the dried aerial part of Agrimony, a plant in the Rosaceae family. It is a traditional Chinese medicine. Its core phenolic acid active ingredient, protocatechuic acid (molecular formula C7H6O4), is an important material basis for Agrimony to exert its medicinal effects.

[0003] Protocatechuic acid possesses significant pharmacological activities such as antioxidant and anti-inflammatory properties, making it highly valuable in various fields. Agrimonia pilosa is abundant and inexpensive; the Henan Province drug standard stipulates that each 1g of Agrimonia pilosa granules contains 0.70mg-3.7mg of protocatechuic acid, highlighting the necessity of extraction. Furthermore, the utilization rate of its effective components in clinical applications is low; specialized extraction can achieve refined resource utilization and increase added value, aligning with industry development trends.

[0004] Currently, existing methods for extracting protocatechuic acid from Agrimonia pilosa primarily involve solvent infiltration to dissolve the target component followed by separation and purification. These methods mainly include the following categories: 1. Traditional solvent extraction method: Based on the principle of "like dissolves like", solvents such as water, methanol, and ethanol are commonly used. The product is obtained by crushing the raw material, soaking / heating and refluxing in the solvent, filtering and concentrating. The operation is simple but the efficiency is limited, and it is often used as a basic extraction method.

[0005] 2. Ultrasonic-assisted extraction: This method adds ultrasonic treatment to the traditional solvent extraction process. The ultrasonic effect breaks down the cell wall and accelerates the extraction. The commonly used power is 500W, the frequency is 40kHz, and the extraction time is 30-40 minutes. It is widely used in the preparation of formulation granules and the determination of content.

[0006] 3. Heating and reflux extraction method: Heating the solvent to reflux increases the solubility of protocatechuic acid and thus improves the extraction rate. Water or alcohol solvents are commonly used. Temperature and time need to be controlled to avoid degradation of the target components.

[0007] 4. Other auxiliary extraction methods: Enzyme-assisted and microwave-assisted extraction methods are rarely used. The former has not yet formed mature process parameters, and the latter has problems such as uneven extraction and easy degradation of target components. Neither has been applied on a large scale.

[0008] Although the above methods can extract protocatechuic acid, they have many drawbacks and cannot meet actual production needs, as follows: (1) Low extraction efficiency: Traditional methods do not sufficiently destroy cell walls, and ultrasonic and heating reflux methods also have problems with insufficient contact. Protocatechuic acid is easily adsorbed by impurities, which does not meet the needs of refined resource utilization.

[0009] (2) Low production efficiency: Traditional soaking takes several hours or more, and ultrasonic and heating reflux also takes more than 30 minutes. In addition, multiple extractions are required, resulting in a long production cycle that cannot meet the needs of large-scale production.

[0010] (3) High solvent consumption, environmental protection and cost pressure: The amount of solvent used is 10-20 times that of raw materials. Organic solvents are difficult to recover and easy to pollute. Water extraction has low extraction efficiency and high energy consumption for concentration, all of which increase costs and are not in line with green production.

[0011] (4) The target component is easily degraded: Protocatechuic acid is easily oxidized and degraded under high temperature and long time extraction, resulting in insufficient content and decreased activity, which may not meet the pharmacopoeia standards.

[0012] (5) Poor process stability: The extraction effect is affected by a variety of factors, and no standardized parameters have been formed. The extraction rate and purity of different batches of products vary greatly, which cannot meet the quality requirements of the pharmaceutical industry.

[0013] In summary, existing methods have many insurmountable shortcomings. Developing efficient, rapid, and green extraction methods to achieve refined utilization of Agrimonia pilosa resources, improve product quality, and reduce costs has significant practical and industrial value. Summary of the Invention

[0014] The purpose of this invention is to overcome the shortcomings of the prior art and provide a method for extracting protocatechuic acid from Agrimonia pilosa. The method includes a processing step, in which Agrimonia pilosa is steamed at 110℃-120℃ for 0.5-1.5h and then cut into sections for later use.

[0015] Furthermore, the method also includes an extraction step: the processed Agrimonia pilosa is first decocted with 12 times the amount of the medicinal slices in water and soaked at room temperature for 30 minutes, then heated to 80°C and soaked at 80°C for 1.0 hour, passed through a 60-mesh sieve, and the filtrate is collected; the second decocted with 10 times the amount of the medicinal slices in water and decocted for 0.5 hours, passed through a 60-mesh sieve, and the filtrate is collected; the third decocted with 8 times the amount of the medicinal slices in water and decocted for 0.5 hours, passed through a 60-mesh sieve, and the filtrate is collected; the filtrates from the third decocted are combined.

[0016] Furthermore, the method also includes a concentration step, wherein the concentration process controls the steam pressure to not exceed 0.12 MPa, the vacuum degree to -0.03 to -0.09 MPa, the concentration temperature to 50 to 85°C, and the concentration is carried out under reduced pressure to obtain a clear paste with a temperature of 60 to 70°C and a relative density of 1.01 to 1.10.

[0017] Furthermore, the method also includes a drying step, wherein the drying is performed using a spray dryer, with the inlet air temperature controlled at 120–180°C, the liquid inlet frequency at 5.0–30.0 Hz, and the outlet air temperature at 80–110°C.

[0018] Furthermore, the method also includes a granulation step: granulation is performed using a dry pressing method, with a 12-mesh sieve for granulation and 10-mesh and 40-mesh sieves for granulation. The feeding speed is 20–230 r / min, the pressing roller speed is 3–40 r / min, and the granulation speed is 20–230 r / min. The mass ratio of the dried extract powder obtained after drying during the granulation process to dextrin is 1:0–0.5.

[0019] Furthermore, after processing the Agrimonia pilosa, cut it into small sections of 5-10mm for later use.

[0020] The Agrimonia pilosa extract obtained by this invention contains 1-1.4 mg / g of protocatechuic acid, which is different from the protocatechuic acid in the prior art. Therefore, the Agrimonia pilosa extract obtained by this invention is also within the scope of protection of this invention.

[0021] After achieving synergistic effects through the above-mentioned technical solutions, the beneficial effects demonstrated by this invention are particularly significant: through the synergistic effect of the processing and extraction processes, the extraction efficiency of protocatechuic acid is effectively enhanced, with the extraction rate increasing dramatically from 0.1-0.6 mg / g in existing technologies to 1-1.4 mg / g, a substantial improvement. This method uses only water as the extraction solvent, eliminating the need for complex processes and equipment such as ultrasonic extraction and reflux extraction, while completely avoiding the use of any organic reagents. This not only reduces material costs but also significantly reduces chemical pollution, meeting green environmental protection requirements and demonstrating good environmental friendliness. The extracted product is dried and granulated, improving its physical stability, facilitating long-term storage and transportation, and effectively slowing down the degradation rate of active ingredients, thereby better maintaining product quality. Furthermore, this process is simple to operate and highly stable. In practical applications, over a hundred repeated experiments have consistently maintained the extraction rate within the range of 1-1.4 mg / g, demonstrating good reproducibility and strong promotional value and industrialization potential. Detailed Implementation

[0022] The following embodiments provide a complete and clearer description of this technical solution. Unless otherwise specified, all technical means employed are existing technologies.

[0023] Example 1: The present invention provides a method for extracting protocatechuic acid from Agrimonia pilosa, including a processing step in which Agrimonia pilosa is steamed at 110℃ for 0.5h and then cut into sections for later use.

[0024] Furthermore, the extraction process includes the following steps: for the first decoction of processed Agrimonia pilosa, add 12 times the amount of water to the decoction pieces and soak at room temperature for 30 minutes, then continue to heat to 80℃ and soak at 80℃ for 1.0 hour, pass through a 60-mesh sieve, and collect the filtrate; for the second decoction, add 10 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; for the third decoction, add 8 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; combine the filtrates from the third decoction.

[0025] Furthermore, it also includes a concentration step, in which the steam pressure is controlled to not exceed 0.12 MPa, the vacuum degree to -0.03 MPa, the concentration temperature to 50°C, and the concentration is carried out under reduced pressure to a clear paste with a temperature of 60°C and a relative density of 1.01.

[0026] Furthermore, it also includes a drying step, which uses a spray dryer, with the inlet air temperature controlled at 120°C, the liquid inlet frequency at 5.0 Hz, and the outlet air temperature at 80°C.

[0027] Furthermore, the process includes a granulation step: granulation is performed using a dry pressing method, with a 12-mesh sieve for granulation and 10-mesh and 40-mesh sieves for granulation. The conveying speed is 20 r / min, the pressing roller speed is 3 r / min, and the granulation speed is 20 r / min. The mass ratio of the dried extract powder to dextrin obtained after granulation is 1:0.1.

[0028] Furthermore, after processing the Agrimonia pilosa, cut it into 5mm pieces for later use.

[0029] Example 2: The present invention provides a method for extracting protocatechuic acid from Agrimonia pilosa, including a processing step, wherein Agrimonia pilosa is steamed at 120°C for 1.5 hours and then cut into sections for later use.

[0030] Furthermore, the extraction process includes the following steps: for the first decoction of processed Agrimonia pilosa, add 12 times the amount of water to the decoction pieces and soak at room temperature for 30 minutes, then continue to heat to 80℃ and soak at 80℃ for 1.0 hour, pass through a 60-mesh sieve, and collect the filtrate; for the second decoction, add 10 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; for the third decoction, add 8 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; combine the filtrates from the third decoction.

[0031] Furthermore, it also includes a concentration step, in which the steam pressure is controlled to not exceed 0.12 MPa, the vacuum degree to -0.09 MPa, the concentration temperature to 85°C, and the concentration is carried out under reduced pressure to a clear paste with a temperature of 70°C and a relative density of 1.10.

[0032] Furthermore, it also includes a drying step, which uses a spray dryer, controlling the inlet air temperature at 180°C, the liquid inlet frequency at 30Hz, and the outlet air temperature at 110°C.

[0033] Furthermore, the process includes a granulation step: granulation is performed using a dry pressing method, with a 12-mesh sieve for granulation and 10-mesh and 40-mesh sieves for granulation. The conveying speed is 230 r / min, the pressing roller speed is 40 r / min, and the granulation speed is 230 r / min. The mass ratio of the dried extract powder to dextrin obtained after granulation is 1:0.5.

[0034] Furthermore, after processing the Agrimonia pilosa, cut it into 10mm pieces for later use.

[0035] Example 3: The present invention provides a method for extracting protocatechuic acid from Agrimonia pilosa, including a processing step, wherein Agrimonia pilosa is steamed at 115°C for 1 hour and then cut into sections for later use.

[0036] Furthermore, the extraction process includes the following steps: for the first decoction of processed Agrimonia pilosa, add 12 times the amount of water to the decoction pieces and soak at room temperature for 30 minutes, then continue to heat to 80℃ and soak at 80℃ for 1.0 hour, pass through a 60-mesh sieve, and collect the filtrate; for the second decoction, add 10 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; for the third decoction, add 8 times the amount of water to the decoction pieces and decoct for 0.5 hours, pass through a 60-mesh sieve, and collect the filtrate; combine the filtrates from the third decoction.

[0037] Furthermore, it also includes a concentration step, in which the steam pressure is controlled to not exceed 0.12 MPa, the vacuum degree to -0.06 MPa, the concentration temperature to 75°C, and the concentration is carried out under reduced pressure to a clear paste with a relative density of 1.05 at a temperature of 65°C.

[0038] Furthermore, it also includes a drying step, which uses a spray dryer, controlling the inlet air temperature at 160°C, the liquid inlet frequency at 20Hz, and the outlet air temperature at 100°C.

[0039] Furthermore, the process includes a granulation step: granulation is performed using a dry pressing method, with a 12-mesh sieve for granulation, and 10-mesh and 40-mesh sieves for finishing. The feeding speed is 150 r / min, the pressing roller speed is 20 r / min, and the granulating speed is 200 r / min. The mass ratio of the dried extract powder to dextrin obtained after granulation is 1:0.3.

[0040] Furthermore, after processing the Agrimonia pilosa, cut it into 8mm pieces for later use.

[0041] The following are examples of experiments conducted during the development process to illustrate the synergistic effect of various conditional parameters in the preparation and extraction of this invention.

[0042] It should be noted that the above experiments were conducted through numerous trials before the technical solution of this invention was finally obtained. To save space, only some experimental examples are listed. Experiments 12-14 were conducted to verify the reliability of the extraction method of this invention. In fact, they were repeated hundreds of times in parallel. To save space, they will not be described in detail.

[0043] The main medicinal component of Agrimonia pilosa extract obtained by this invention, protocatechuic acid, has been increased from 0.1-0.6 mg / g in the prior art to 1-1.4 mg / g.

[0044] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-described technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for extracting Agrimonia pilosa extract, characterized in that, The extract is protocatechuic acid. The method includes a processing step, in which Agrimonia pilosa is steamed at 110℃-120℃ for 0.5-1.5 hours and then cut into sections for later use.

2. The method according to claim 1, characterized in that, The method also includes an extraction step: the processed Agrimonia pilosa is first decoction with 12 times the amount of water as the medicinal slices, then soaked at room temperature for 30 minutes, and then heated to 80°C and soaked at 80°C for 1.0 hour. The decoction is then passed through a 60-mesh sieve and the filtrate is collected. The second decoction is decocted with 10 times the amount of water as the medicinal slices for 0.5 hours, and the filtrate is collected. The third decoction is decocted with 8 times the amount of water as the medicinal slices for 0.5 hours, and the filtrate is collected. The filtrates from the third decoction are then combined.

3. The method according to claim 1 or 2, characterized in that, The method further includes a concentration step, wherein the steam pressure is controlled to not exceed 0.12 MPa, the vacuum degree is -0.03 to -0.09 MPa, the concentration temperature is 50 to 85°C, and the concentration is carried out under reduced pressure to obtain a clear paste with a temperature of 60 to 70°C and a relative density of 1.01 to 1.

10.

4. The method according to any one of claims 3, characterized in that, The method further includes a drying step, wherein a spray dryer is used for drying, and the inlet air temperature is controlled at 120-180°C, the liquid inlet frequency is 5.0-30.0Hz, and the outlet air temperature is 80-110°C.

5. The method according to claim 4, characterized in that, The method also includes a granulation step: the granulation is carried out by dry pressing granulation, the granulation screen has a mesh size of 12 mesh, the granulation screen has a mesh size of 10 mesh and 40 mesh, the conveying speed is 20-230 r / min, the pressing roller speed is 3-40 r / min, and the granulation speed is 20-230 r / min.

6. The method according to claim 5, characterized in that, The mass ratio of the dried extract obtained after granulation to dextrin is 1:0 to 0.

5.

7. The method according to claim 1, characterized in that, After processing, the Agrimonia pilosa is cut into small sections of 5-10mm and set aside.

8. An extract of Agrimonia pilosa, characterized in that, The protocatechuic acid content in Agrimonia pilosa is 1-1.4 mg / g, obtained by extraction according to any one of claims 1-2, 4-7.

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