Method for extracting active ingredients of dandelion

Abstract

The invention relates to a method for extracting active ingredients of dandelion, in particular to a method for extracting active ingredients of dandelion. The invention aims to solve the problems of low extraction rate and low comprehensive utilization rate of the active ingredients of the dandelion in the prior art. And a novel low-cost eutectic solvent is adopted, so that pollution and energy consumption are remarkably reduced. An ultrasonic-assisted extraction technology is adopted, so that the extraction rate of active ingredients is effectively improved. And a macroporous adsorption resin separation and enrichment technology is adopted, so that the enrichment degree and the enrichment rate of the active ingredients are remarkably improved, physical low-temperature extraction of the active ingredients is realized, and the biological activity of the extract is effectively guaranteed. The ultrasonic extraction process is a physical change process, no chemical reaction occurs in the whole extraction process, harmful substances are not generated, and meanwhile, the physiological activity of the dandelion extract is not influenced. In the extraction process, the sample does not need to be subjected to high-temperature heating treatment, so that the energy loss is reduced.

Description

Technical Field

[0001] The invention relates to a method for extracting active components from dandelion. Background Art

[0002] Dandelion is a typical plant with both medicinal and edible properties. It is a safe plant source of natural compounds and is rich in nutrients such as protein, fat, and dietary fiber. The active ingredients of dandelion mainly include phenolic acid, flavonoids, polysaccharides, sterols, terpenes, pigments, alkaloids, etc. The pharmacological effects mainly include antibacterial, antioxidant, anti-gastric damage, anti-diabetes, anti-tumor, anti-virus, etc. It can be used to treat a variety of acute inflammations, colds, fevers, urinary tract infections and other diseases. With the development of the economy and the improvement of people's living standards, the number of people in sub-health status is increasing. People have new requirements for health. The big health industry is in a stage of rapid development. Dandelion and its active ingredients have extremely high nutritional and medical value. It is a good dietary element and medical resource. It is suitable for development into various pharmaceutical products, health foods, and beauty and skin care products to promote the development of the big health industry. In summary, dandelion has a high development value.

[0003] There are many methods for extracting active ingredients from dandelions. They are:

[0004] (1) Reflux extraction method: An organic solvent is used as the extraction solvent. By mixing different solvents, the polarity and boiling point of a single solvent can be changed to obtain a solvent suitable for extracting different active ingredients. The commonly used reflux extraction device consists of a flask and a condenser. The dandelion is crushed and placed in a flask, mixed with the extraction solvent and heated to promote the dissolution of the active ingredient. The solvent evaporates after being heated, condenses at the condenser and refluxes into the flask, reducing the loss of the solvent. Compared with other methods, the extract obtained by reflux is more complete and fully extracted, has a wider range of applications, and the extraction process is simpler and easier to implement. The loss of solvent is less. After being collected by evaporation and condensation, the next cycle can be carried out. However, the amount of extracted medicinal materials is small and is not suitable for large-scale production. The Soxhlet extraction method is an improvement on the reflux method. It mainly uses a solvent reflux device and a siphon principle to extract the active ingredients from the raw medicinal materials. It is mostly completed using a Soxhlet extractor. Factors affecting the extraction efficiency of active ingredients in this extraction process include solvent type, solvent amount to raw medicinal material ratio, extraction temperature, etc. The advantage of this method is that it saves solvent. After completing a solvent extraction, the solution is heated, the volatilized solvent is condensed through the condenser, and re-enters the extraction environment to start a new extraction process. The extraction is highly complete. Solvent extraction can be performed multiple times. Disadvantages: high energy consumption, high equipment requirements, and it cannot be put into large-scale industrial production at present.

[0005] (2) Microwave extraction method: The principle is to use the effect of microwave heating to realize the entire process of extraction and separation. Microwave technology can significantly increase the extraction efficiency of effective ingredients and avoid various problems caused by long-term heating. At the same time, due to the characteristics of microwaves on compounds, such as breaking weak chemical bonds and chemical bond reorganization leading to compound structure transformation, the most important thing is that microwave extraction of dandelion active ingredients has a high extraction rate, low energy consumption, short time, and is more environmentally friendly. However, the equipment for this method is relatively expensive and cannot be put into large-scale industrial production. Microwave-assisted extraction is also a thermal extraction method, so it is not suitable for extracting heat-sensitive active ingredients.

[0006] (3) Ultra-high pressure extraction method: High pressure or ultra-high pressure technology (pressure above 100 MPa) mainly increases the hydrostatic pressure of the liquid-feed mixture, maintains the pressure for a period of time, and then quickly releases the pressure to carry out the subsequent extraction steps. This method can significantly reduce the extraction time, reduce the loss of solvent, and improve the extraction efficiency of effective ingredients. It can replace most processes that rely on heat treatment methods. It is relatively simple to operate and has high safety performance. However, the equipment used in this method is relatively expensive, the asset investment is large, low temperature is required during use, and there are problems such as difficulty in decomposing residual pesticides.

[0007] (4) Supercritical fluid extraction: This is a relatively new extraction technology. When the extraction temperature and pressure exceed the critical point of the substance, a relatively single phase, namely supercritical fluid, will be formed. The density of supercritical fluid is similar to that of liquid, but due to its low viscosity and strong diffusivity, the solubility of supercritical fluid is stronger than other liquids, and it can achieve efficient and rapid mass transfer extraction. When using this method, the diffusion coefficient of solute in supercritical fluid is similar to that of gas, which has the advantages of fast conduction and short extraction time. At the same time, the extraction selectivity of this method is strong, and it is easier to concentrate because it is in a gas state after extraction. However, the extraction process is relatively long, the cost is expensive, and the return rate is low. Therefore, the above methods are not suitable for large-scale factory extraction of dandelion active ingredients. Compared with international manufacturers, my country's extraction production level is far behind the world's advanced extraction level. In addition to the low extraction yield, the ability to separate the effective ingredients of the product is also poor. To this end, this project uses a new type of low eutectic solvent to extract through ultrasonic assisted extraction. Summary of the invention

[0008] In order to solve the problems of low extraction rate and comprehensive utilization rate of the existing dandelion active ingredients, the invention provides a method for extracting the dandelion active ingredients.

[0009] The method for extracting active ingredients from dandelion of the present invention is carried out according to the following steps:

[0010] 1. Preparation of low eutectic solvent: Choline chloride and solvent are mixed in a reactor with a molar ratio of 1:2, heated to 80°C, and stirred for 2 hours to form a transparent and uniform solvent;

[0011] 2. Preparation of extraction solvent: adding deionized water to the low eutectic solvent prepared in step 1 to prepare an extraction solvent with a water content of 0-50%;

[0012] 3. Extraction: Wash, dry and crush the dandelion to obtain dandelion powder, place the dandelion powder and the extraction solvent prepared in step 2 in a reaction container at a material-liquid ratio of 10-40:1 mg / mL; place the material in an ultrasonic-assisted extractor for ultrasonic extraction to obtain an extract, and filter the extract to obtain a dandelion crude extract;

[0013] 4. Separation and purification:

[0014] The dandelion crude extract obtained in step three is adsorbed by macroporous adsorption resin. After adsorption, impurities are eluted with 2-8 BV deionized water, and then eluted with 10-90% ethanol solution by volume, and the eluate is collected, concentrated and dried.

[0015] The present invention adopts a new low-cost low eutectic solvent, which significantly reduces pollution and energy consumption. Low eutectic solvents, also known as low eutectic ionic liquids, are considered to be a new type of green ionic liquid or ionic liquid analogs that can effectively replace traditional organic solvents. Due to its unique physical and chemical properties, low eutectic solvents have been widely used in the extraction and separation of traditional Chinese medicine plant materials. Researchers use low eutectic solvents to extract and separate natural active ingredients. Therefore, low-cost, low-pollution and high-extraction-rate low eutectic solvents are bound to bring extremely high returns.

[0016] The present invention adopts ultrasound-assisted extraction technology to effectively improve the extraction rate of active ingredients. Ultrasonic-assisted extraction technology is an extraction method that uses the vibration and energy brought by ultrasound to increase the movement speed of medium molecules and the penetration of the medium to extract biological effective ingredients. Through ultrasonic treatment, the solvent can be fully contacted with the medicinal material, which reduces the reaction time, improves the extraction rate of effective ingredients, and is conducive to the full utilization of resources. The extraction rate of dandelion active ingredients is more than 1 times higher than that of the single ethanol extraction method, eliminating the use of toxic chemical extraction reagents and ensuring the application safety of active ingredients. Ultrasonic-assisted extraction is applied to the extraction of effective content of Chinese medicinal materials and various animals and plants due to its unique advantages such as low extraction temperature, high extraction rate, short extraction time and wide adaptability, and the obtained extraction liquid contains fewer impurities, making the effective ingredients easier to separate and purify experiments.

[0017] The present invention adopts macroporous adsorption resin separation and enrichment technology to significantly improve the enrichment degree and rate of active ingredients. Macroporous adsorption resin is an organic polymer adsorbent that selectively adsorbs on the surface. It has the advantages of large specific surface area, fast exchange rate, large adsorption capacity, fast adsorption rate, stable physical and chemical properties, strong anti-pollution ability, low energy consumption, and wide range of use. In the process of modernization of traditional Chinese medicine, macroporous adsorption resin can be used on a large scale for the enrichment of effective compound components due to its low price, high stability and low energy consumption.

[0018] The present invention realizes physical low-temperature extraction of active ingredients and effectively ensures the biological activity of the extract. The ultrasonic extraction process is a physical change process. No chemical reaction occurs during the entire extraction process, no harmful substances are generated, and the physiological activity of the dandelion extract is not affected. In addition, the sample does not need to be subjected to high-temperature heating treatment during the extraction process, which reduces energy loss and avoids the adverse effects of long-term high-temperature heating on the active ingredients of the extract in conventional decoction and reflux extraction methods. DETAILED DESCRIPTION

[0019] The technical solution of the present invention is not limited to the specific implementation modes listed below, but also includes any reasonable combination of the specific implementation modes.

[0020] Specific implementation method 1: The method for extracting active ingredients from dandelions in this implementation method is carried out according to the following steps:

[0021] 1. Preparation of low eutectic solvent: Choline chloride and solvent are mixed in a reactor with a drying tube at a molar ratio of 1:2, heated to 80°C, and stirred for 2 hours to form a transparent and uniform solvent;

[0022] 2. Preparation of extraction solvent: adding deionized water to the low eutectic solvent prepared in step 1 to prepare an extraction solvent with a water content of 0-50%;

[0023] 3. Extraction: Wash, dry and crush the dandelion to obtain dandelion powder, place the dandelion powder and the extraction solvent prepared in step 2 in a reaction container at a material-liquid ratio of 10-40:1 mg / mL; place the material in an ultrasonic-assisted extractor for ultrasonic extraction to obtain an extract, and filter the extract to obtain a dandelion crude extract;

[0024] 4. Separation and purification:

[0025] The dandelion crude extract obtained in step three is adsorbed by macroporous adsorption resin. After adsorption, impurities are eluted with 2-8 BV deionized water, and then eluted with 10-90% ethanol solution by volume, and the eluate is collected, concentrated and dried.

[0026] This embodiment has the following beneficial effects:

[0027] This embodiment uses a new low-cost low eutectic solvent to significantly reduce pollution and energy consumption. Low eutectic solvents, also known as low eutectic ionic liquids, are considered to be a new type of green ionic liquid or ionic liquid analog that can effectively replace traditional organic solvents. Due to its unique physical and chemical properties, low eutectic solvents have been widely used in the extraction and separation of traditional Chinese medicine plant materials. Researchers use low eutectic solvents to extract and separate natural active ingredients. Therefore, low-cost, low-pollution and high-extraction low eutectic solvents are bound to bring extremely high returns.

[0028] This embodiment adopts ultrasound-assisted extraction technology to effectively improve the extraction rate of active ingredients. Ultrasonic-assisted extraction technology is an extraction method that uses the vibration and energy brought by ultrasound to increase the movement speed of medium molecules and the penetration of the medium to extract biological active ingredients. Through ultrasonic treatment, the solvent can be fully contacted with the medicinal material, which reduces the reaction time, improves the extraction rate of effective ingredients, and is conducive to the full utilization of resources. The extraction rate of dandelion active ingredients is more than 1 times higher than that of the single ethanol extraction method, eliminating the use of toxic chemical extraction reagents and ensuring the application safety of active ingredients. Ultrasonic-assisted extraction is used for the extraction of effective content of Chinese medicinal materials and various animals and plants due to its unique advantages such as low extraction temperature, high extraction rate, short extraction time and wide adaptability, and the obtained extraction liquid contains fewer impurities, making the effective ingredients easier to separate and purify experiments.

[0029] This embodiment adopts macroporous adsorption resin separation and enrichment technology to significantly improve the enrichment degree and rate of active ingredients. Macroporous adsorption resin is an organic polymer adsorbent that selectively adsorbs on the surface. It has the advantages of large specific surface area, fast exchange rate, large adsorption capacity, fast adsorption rate, stable physical and chemical properties, strong anti-pollution ability, low energy consumption, and wide range of use. In the process of modernization of traditional Chinese medicine, macroporous adsorption resin can be used on a large scale for the enrichment of effective compound components due to its low price, high stability and low energy consumption.

[0030] This embodiment realizes the physical low-temperature extraction of active ingredients, effectively ensuring the biological activity of the extract. The ultrasonic extraction process is a physical change process. No chemical reaction occurs during the entire extraction process, no harmful substances are produced, and the physiological activity of the dandelion extract is not affected. In addition, the sample does not need to be heated at high temperature during the extraction process, which reduces energy loss and avoids the adverse effects of long-term high-temperature heating on the active ingredients of the extract in conventional decoction and reflux extraction methods.

[0031] Specific implementation method 2: This implementation method is different from specific implementation method 1 in that: the adsorption process is a resin column diameter-to-height ratio of 1:3, a sample loading volume of 40-50 BV, and an adsorption flow rate of 1-1.5 BV / h.

[0032] Specific implementation method three: This implementation method is different from specific implementation methods one or two in that: the macroporous adsorption resin is AB-8, LX-218, XDA-6, D-101, LX-T28 or LX-26.

[0033] Specific embodiment 4: This embodiment is different from any one of specific embodiments 1 to 3 in that: the solvent is one of ethylene glycol, glycerol, triethanolamine, levulinic acid, malonic acid and trifluoroacetic acid.

[0034] Specific implementation method five: This implementation method is different from any one of specific implementation methods one to four in that: the ultrasonic process is an ultrasonic-assisted extraction for 90 minutes at 40° C. and an ultrasonic power of 450 W.

[0035] Example 1

[0036] The method for extracting active ingredients from dandelion in this embodiment is carried out according to the following steps:

[0037] 1. Preparation of low eutectic solvent: Choline chloride and solvent are mixed in a reactor with a drying tube at a molar ratio of 1:2, heated to 80°C, and stirred for 2 hours to form a transparent and uniform solvent;

[0038] 2. Preparation of extraction solvent: adding deionized water to the low eutectic solvent prepared in step 1 to prepare an extraction solvent with a water content of 0-50%;

[0039] 3. Extraction: Wash, dry and crush the dandelion to obtain dandelion powder, place the dandelion powder and the extraction solvent prepared in step 2 in a reaction container at a material-liquid ratio of 30:1 mg / mL; place the material in an ultrasonic-assisted extractor for ultrasonic extraction to obtain an extract, and filter the extract to obtain a crude dandelion extract;

[0040] 4. Separation and purification:

[0041] The dandelion crude extract obtained in step three is adsorbed by macroporous adsorption resin. After the adsorption is completed, impurities are eluted with 6BV deionized water, and then eluted with 80% ethanol solution by volume, and the eluate is collected, concentrated and dried.

[0042] The adsorption process is as follows: the resin column diameter-to-height ratio is 1:3, the sample loading volume is 50 BV, and the adsorption flow rate is 1.5 BV / h;

[0043] The macroporous adsorption resin is AB-8;

[0044] The solvent is ethylene glycol;

[0045] The ultrasonic process is to carry out ultrasonic-assisted extraction for 90 minutes at 40°C and an ultrasonic power of 450W;

[0046] This embodiment uses a new low-cost low eutectic solvent to significantly reduce pollution and energy consumption. Low eutectic solvents, also known as low eutectic ionic liquids, are considered to be a new type of green ionic liquid or ionic liquid analogs that can effectively replace traditional organic solvents. Due to its unique physical and chemical properties, low eutectic solvents have been widely used in the extraction and separation of traditional Chinese medicine plant materials. Researchers use low eutectic solvents to extract and separate natural active ingredients. Therefore, low-cost, low-pollution and high-extraction low eutectic solvents are bound to bring extremely high returns.

[0047] This embodiment uses ultrasound-assisted extraction technology to effectively improve the extraction rate of active ingredients. Ultrasonic-assisted extraction technology is an extraction method that uses the vibration and energy brought by ultrasound to increase the movement speed of medium molecules and the penetration of the medium to extract biological active ingredients. Through ultrasonic treatment, the solvent can be fully contacted with the medicinal material, which reduces the reaction time, improves the extraction rate of effective ingredients, and is conducive to the full utilization of resources. The extraction rate of dandelion active ingredients is more than 1 times higher than that of the single ethanol extraction method, eliminating the use of toxic chemical extraction reagents and ensuring the application safety of active ingredients. Ultrasonic-assisted extraction is used for the extraction of effective content of Chinese medicinal materials and various animals and plants due to its unique advantages such as low extraction temperature, high extraction rate, short extraction time and wide adaptability, and the obtained extraction liquid contains fewer impurities, making the effective ingredients easier to separate and purify experiments.

[0048] This embodiment adopts macroporous adsorption resin separation and enrichment technology to significantly improve the enrichment degree and rate of active ingredients. Macroporous adsorption resin is an organic polymer adsorbent that selectively adsorbs on the surface. It has the advantages of large specific surface area, fast exchange rate, large adsorption capacity, fast adsorption rate, stable physical and chemical properties, strong anti-pollution ability, low energy consumption, and wide range of use. In the process of modernization of traditional Chinese medicine, macroporous adsorption resin can be used on a large scale for the enrichment of effective compound components due to its low price, high stability and low energy consumption.

[0049] This embodiment realizes the physical low-temperature extraction of active ingredients, effectively ensuring the biological activity of the extract. The ultrasonic extraction process is a physical change process. No chemical reaction occurs during the entire extraction process, no harmful substances are produced, and the physiological activity of the dandelion extract is not affected. In addition, the sample does not need to be subjected to high-temperature heating treatment during the extraction process, which reduces energy loss and avoids the adverse effects of long-term high-temperature heating on the active ingredients of the extract in conventional decoction and reflux extraction methods.

Claims

1. A method for extracting active ingredients from dandelion, characterized in that: The method for extracting the active ingredients from dandelion is carried out according to the following steps:

1. Preparation of low eutectic solvent: Choline chloride and solvent are mixed in a reactor with a drying tube at a molar ratio of 1:2, heated to 80°C, and stirred for 2 hours to form a transparent and uniform solvent; 2. Preparation of extraction solvent: adding deionized water to the low eutectic solvent prepared in step 1 to prepare an extraction solvent with a water content of 0-50%; 3. Extraction: Wash, dry and crush the dandelion to obtain dandelion powder, place the dandelion powder and the extraction solvent prepared in step 2 in a reaction container at a material-liquid ratio of 10-40:1 mg / mL; place the material in an ultrasonic-assisted extractor for ultrasonic extraction to obtain an extract, and filter the extract to obtain a dandelion crude extract; 4. Separation and purification: The dandelion crude extract obtained in step three is adsorbed by macroporous adsorption resin. After adsorption, impurities are eluted with 2-8 BV deionized water, and then eluted with 10-90% ethanol solution by volume, and the eluate is collected, concentrated and dried.

2. The method for extracting active ingredients from dandelion according to claim 1, characterized in that: The adsorption process is as follows: the resin column diameter-to-height ratio is 1:3, the sample loading volume is 40-50 BV, and the adsorption flow rate is 1-1.5 BV / h.

3. The method for extracting active ingredients from dandelion according to claim 1, characterized in that: The macroporous adsorption resin is AB-8, LX-218, XDA-6, D-101, LX-T28 or LX-26.

4. The method for extracting active ingredients from dandelion according to claim 1, characterized in that: The solvent is one of ethylene glycol, glycerol, triethanolamine, levulinic acid, malonic acid and trifluoroacetic acid.

5. The method for extracting active ingredients from dandelion according to claim 1, characterized in that: The ultrasonic process is carried out under the conditions of 40° C. and an ultrasonic power of 450 W, with ultrasonic-assisted extraction for 90 minutes.