CN116023422A - Method for extracting ginsenoside from ginseng residue and utilizing residue after extraction - Google Patents
Method for extracting ginsenoside from ginseng residue and utilizing residue after extraction Download PDFInfo
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Abstract
The invention discloses a method for extracting ginsenoside from ginseng residue and utilizing residues after extraction, which is characterized in that the waste ginseng residue is used as a raw material, the ginseng residue is extracted by using a eutectic solvent of choline chloride/propionic acid, ethylene glycol or diethylene glycol and water to form an extraction solvent, the extraction liquid is collected to obtain the functional components of ginsenoside, ginseng polysaccharide and the like, and the residues after extraction are prepared into ginseng residue dietary fibers. The method has the advantages of high extraction rate of the total saponins of the ginseng, mild reaction conditions and short extraction time; the extraction process simultaneously improves the surface area of the ginseng residue dietary fiber, is favorable for adsorbing harmful substances in intestinal tracts, and has higher nutritive value. The method improves the utilization value of ginseng residue, and is easy for industrialized popularization.
Description
Technical Field
The invention relates to a method for extracting ginsenoside from ginseng residue and utilizing extracted residues at a high value, belonging to the technical field of resource utilization of waste biomass.
Technical Field
Ginseng is perennial herb of Panax of Araliaceae. Widely distributed in China, russian and Korea; in China, it is mainly distributed in the eastern Liaoning, the eastern Jilin and the eastern Heilongjiang. The fleshy root of ginseng is a tonic, is suitable for regulating blood pressure, restoring heart function, neurasthenia and asthenia, and has the effects of eliminating phlegm, invigorating stomach, promoting urination, and exciting. Stems, leaves, flowers, fruits and processing byproducts of ginseng are raw materials of the light industry, and commercial products such as cigarettes, wines, teas, crystals, pastes and the like containing ginseng components can be processed. The ginseng contains ginsenoside, ginseng polysaccharide, amino acid, volatile oil, vitamins, alkaloid, organic acid and other components, wherein the ginsenoside is considered as the most representative active component of the ginseng. The annual consumption of ginseng is more than 7 ten thousand tons, and most of the ginseng is used for extracting ginsenoside. Because the ginsenoside content in the ginseng root is only 4%, most of ginseng medicinal materials are converted into ginseng residues, and the discarded ginseng residues are generally used as feed or discarded at will, so that the ginseng root has low utilization value and is easy to pollute the environment.
Through analysis of ginseng residues, the ginseng dietary fiber (cellulose, hemicellulose, lignin, pectin and other substances) is found as the main component, and contains chemical active substances such as ginsenoside, ginseng polysaccharide, amino acid, volatile oil, vitamins, alkaloids, organic acid and the like. The ginseng polysaccharide accounts for 8% -10% of the dry weight of ginseng residue, and has the functions of enhancing immunity, promoting hematopoiesis, reducing blood sugar, resisting urination, resisting aging, resisting thrombus, resisting bacteria, resisting inflammation, resisting tumor and the like. The dietary fiber has the effects of reducing blood lipid and blood sugar, promoting gastrointestinal peristalsis, and preventing and treating constipation. If the part of resources can be reasonably utilized, not only can the reasonable utilization of ginseng residue resources be increased, but also the pollution to the environment can be reduced, and the development of other agricultural projects in the planting area can be driven.
In the literature report, most of ginseng residue is utilized for preparing feed and fermenting to produce sugar, and the report of comprehensive utilization of the ginseng residue is relatively few.
Patent publication No. CN 111184212A reports a preparation method of ginseng polysaccharide tablet, which adopts ginseng residue after extracting ginsenoside as main raw material, and prepares the ginseng polysaccharide tablet by crushing, granulating and tabletting steps, wherein the content of ginseng residue is 95% -98.5%. The process is complex in operation, time-consuming and poor in industrial utilization effect. And the ginseng polysaccharide content is low, and the product value is not high.
Patent publication No. CN 110150678A reports a ginseng dietary fiber chewing tablet and a preparation method thereof. Taking ginseng residues as raw materials, rinsing, drying and crushing the ginseng residues, adding water for soaking, and centrifugally separating to obtain ginseng dietary fiber powder; mixing with adjuvants, granulating, and tabletting to obtain the chewable tablet. The method has complicated preparation process, and ginsenoside and ginseng polysaccharide components in the ginseng residue are not recycled, so that energy waste is caused.
Patent publication No. CN 110922442A reports a green method for preparing ginseng extract rich in rare ginsenoside Rg3, rg 5. The method takes the roots of the ginseng plant as the raw material, the fruit acid in the fruit juice as the structure modifier, and the ginseng extract rich in rare ginsenoside Rg3 and Rg5 is prepared by integrating the efficient extraction of the ginsenoside, the structure modification of the ginsenoside, the solid-liquid separation of the ginseng extract and ginseng residue and the concentration of the ginseng extract through one-step operation. The method has high extraction efficiency, but has high reaction condition requirement, and the residue after extraction is not utilized.
Therefore, in the existing method for recycling ginseng residue, most of the single components concentrated in the method are utilized, the most valuable ginsenoside is not effectively utilized, in addition, the utilization of residue is not comprehensively considered, the process operation is complicated, the yield is low, the serious waste of resources is caused, and meanwhile, the pressure is brought to the environment.
The eutectic solvent (deep eutectic solvent, DES) is a green solvent which is found in recent years by Abbott et al to replace traditional organic solvents and ionic liquids, and refers to a two-component or three-component eutectic mixture formed by combining hydrogen bond acceptors (such as quaternary ammonium salts) and hydrogen bond donors (such as amide, carboxylic acid, polyalcohol and other compounds) in a stoichiometric ratio, and the freezing point of the two-component or three-component eutectic mixture is obviously lower than the melting point of pure substances of each component. The synthesis components of DESs are mostly natural products, are cheap and biodegradable, the preparation process is simple, and the eutectic mixed liquid solvent can be obtained by only mixing the corresponding components together according to a set proportion and stirring at a low temperature. The low cost, designability, biodegradability and environmental friendliness of DESs make them a versatile alternative to traditional organic solvents.
Disclosure of Invention
In order to realize high-value utilization of ginseng residue, the invention provides a method for comprehensively utilizing extracted ginsenoside from ginseng residue and extracted residue, which can rapidly and efficiently extract active ingredients in the ginseng residue, and the extracted residue is further prepared into ginseng residue dietary fiber, so that high-value utilization of ginseng residue is realized, and industrial popularization is easy.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for extracting ginsenoside from ginseng residue and utilizing residue after extraction is characterized by comprising the following steps:
1) Mixing choline chloride with propionic acid, ethylene glycol or diethylene glycol, and stirring at room temperature to obtain uniform transparent liquid to obtain eutectic solvent;
2) Adding an extraction solvent consisting of the eutectic solvent and water in the step 1) into the crushed ginseng residue, extracting, filtering and collecting an extracting solution to obtain a ginseng residue extracting solution and a solid residue;
3) Concentrating the extracting solution in the step 2), adding ethanol for precipitation, and centrifuging to obtain crude ginseng polysaccharide solid and ginseng saponin extracting solution;
4) Washing the solid residue extracted in the step 2) to be neutral by pure water, soaking in water, centrifuging, drying and crushing to obtain the ginseng residue dietary fiber.
In the method, the eutectic solvent composed of choline chloride and propionic acid is preferable in the step 1).
In the method, the molar ratio of choline chloride to propionic acid, ethylene glycol or diethylene glycol in the eutectic solvent in step 1) is preferably 1:3-1:5, most preferably the molar ratio is 1:3.
in the method, in the extraction solvent of the step 2), the volume percentage of the eutectic solvent is 50-90%, and the preferred volume percentage is 70%.
In the method, the solid-to-liquid ratio of the ginseng residue to the extraction solvent in the step 2) is 1:15 to 35 (g/mL), preferably 1:20 to 25 (g/mL).
In the method, the extraction time in the step 2) is preferably 20-40 min.
In the method, preferably, ultrasound-assisted extraction is used in step 2).
In the method, the addition amount of the ethanol in the step 3) is 3-4 times of the volume of the extracting solution.
In the method, the time of alcohol precipitation in the step 3) is 12-24 hours.
In the method, the mass ratio of the solid residue to water in the step 4) is 1: 20-1: 30.
in the method, the soaking time in the step 4) is 10-16 h.
The invention has the beneficial effects that: according to the method for extracting ginsenoside from ginseng residue and utilizing the residue after extraction, the waste ginseng residue is used as a raw material, and the ginsenoside and the ginseng polysaccharide are obtained through eutectic solvent extraction, and the dietary fiber of the ginseng residue is prepared from the residue after extraction, so that the utilization value of the ginseng residue is improved, and the industrial popularization is easy.
1) According to the invention, the green eutectic solvent choline chloride/propionic acid and the like are utilized to extract the ginseng residue to obtain the extracting solution containing the ginsenoside and the ginseng polysaccharide, compared with the traditional organic solvent extraction, the extracting solution can extract the ginsenoside from the ginseng residue, achieves higher ginsenoside extraction rate, has milder extraction conditions and shorter required time, and has the advantages of energy conservation, high efficiency, safety and environmental protection.
2) The ginsenoside extracting solution and the ginseng polysaccharide are obtained after the extracting solution extracted by the eutectic solvent is subjected to ethanol precipitation, and no additional extracting step is needed, so that the process flow is greatly simplified, and the method has the advantages of economy and simplicity.
3) The solid residues after extracting the ginsenoside and the ginseng polysaccharide are subjected to simple rinsing, soaking and drying to further obtain the ginseng residue dietary fiber, so that the surface area of the ginseng residue dietary fiber is increased, the absorption of harmful substances in intestinal tracts is facilitated, and the ginseng residue dietary fiber has higher nutritive value.
Drawings
FIG. 1 is a process flow diagram of a method for extracting ginsenoside from ginseng residue and utilizing residue after extraction;
FIG. 2 shows surface scanning electron microscope spectra before (a) and after (b) extraction of ginseng residue;
FIG. 3 influence of extraction solvent on total saponins extraction of ginseng residue;
FIG. 4 effect of molar ratio on total saponins extraction of ginseng residue;
FIG. 5 influence of water content on extraction of total saponins of ginseng residue;
FIG. 6 is a graph showing the effect of feed liquid comparison on total saponins extraction from ginseng residue;
FIG. 7 effect of time on total saponins extraction of ginseng residue;
FIG. 8 oxidation resistance of ginseng polysaccharides; a-hydroxy radical scavenging ability, b-DPPH scavenging ability.
Detailed Description
The following detailed description of the present invention is given by way of specific examples, which are given for illustrative purposes only and are not to be construed as limiting the scope of the present invention.
Example 1
A method for extracting ginsenoside from ginseng residue and utilizing residue after extraction comprises the following steps:
(1) Choline chloride and propionic acid are mixed according to a mole ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent.
(2) Taking a certain amount of (absolute dry) ginseng residue, crushing, sieving with a 80-mesh sieve, and placing into a container according to a feed-liquid ratio of 1: adding 20g/mL of a mixed solution of the eutectic solvent and water, wherein the mixed solution contains 70% (volume fraction) of the eutectic solvent; adding the mixed solution into the container for extraction for 1-3 times, ultrasonically extracting for 30min each time, centrifuging, and collecting the extract and solid residue.
The total content of ginsenoside in the extract is determined by vanillin-glacial acetic acid-concentrated sulfuric acid ultraviolet color development method, wherein the extraction rate of ginsenoside is 36.7mg/g (absolute dry ginseng residue).
(3) The supernatant was concentrated to a certain volume by rotary evaporation under reduced pressure. The volume ratio of the concentrated extracting solution is 1:4 adding ethanol for precipitation for 12h, centrifuging, collecting filtrate as ginsenoside extractive solution, precipitating to obtain crude Ginseng radix polysaccharide, drying, and grinding into powder.
(4) Washing the extracted solid residue in the step (2) to be neutral by pure water, adding water, mixing (the mass ratio is 1:20) to form a mixed solution, soaking for 12 hours, centrifuging the mixed solution, taking the precipitate, drying and crushing to obtain the ginseng residue dietary fiber.
The process flow of the method is shown in fig. 1. The surface scanning electron microscope spectra before and after the extraction of the ginseng residue are shown in figure 2, and the microstructure of the surface of the extracted ginseng residue is more loose and has more cracks and pores. The possible reason is that the ginseng residue removes a large amount of soluble substances during the extraction process, resulting in the destruction of a part of the structure of the ginseng fiber. After the extraction treatment, the ginseng residue shows relatively regular loose structures and cavities. The extraction treatment makes the structure of ginseng residue looser, the specific surface area is increased, and the absorption capacity of the ginseng residue on water, oil, heavy metal and salt ions is improved. In general, the microstructure of ginseng residue before and after extraction is not obviously different, and insoluble cellulose is still the main material.
Example 2 Effect of different solvents on extraction of ginsenoside from Ginseng radix residue
Choline chloride is respectively mixed with acetic acid, glycollic acid, lactic acid, propionic acid, glycerol, ethylene glycol, diethylene glycol and 1, 4-butanediol according to the mol ratio of 1:2, mixing, stirring for 30min at room temperature to form uniform transparent liquid, and preparing a group of eutectic solvents. Taking a certain amount of (absolute dry) ginseng residue, pulverizing, sieving with a 80-mesh sieve, placing into a container, respectively adding 80% (volume percent) of mixed solution of different eutectic solvents and 20% of water, and ethanol as extraction solvents, wherein the feed-liquid ratio is 1:20, ultrasonic extracting for 30min, extracting for 3 times, filtering, and collecting the extract and solid residue. The extraction rate of ginsenoside with different extraction solvents composed of the eutectic solvents is shown in figure 3.
When the system of the eutectic solvent is choline chloride/propionic acid, the extraction effect of ginsenoside in ginseng residue is optimal, and the extraction rate is 22.7mg/g. Compared with the traditional solvent ethanol (11.5 mg/g), the extraction rate is obviously improved.
Example 3 influence of molar ratio in eutectic solvent on extraction of ginsenoside from ginseng residue
Choline chloride and propionic acid are respectively mixed according to the mole ratio of 1: 2. 1:3. 1: 4. 1:5. 1:6, mixing, stirring for 30min at room temperature to form uniform transparent liquid, and preparing a group of eutectic solvents. Taking a certain amount of (absolute dry) ginseng residue, pulverizing, sieving with an 80-mesh sieve, placing into a container, and respectively adding mixed solution of 80% (volume percent) of eutectic solvent and 20% of water, wherein the feed-liquid ratio is 1:20, ultrasonic extracting for 30min, extracting for 3 times, filtering, and collecting the extract and solid residue. The extraction rate of ginsenoside in eutectic solvent with different molar ratios is shown in figure 4.
When the molar ratio of choline chloride to propionic acid is 1:3-1:5, the extraction rate of the total saponins of the ginseng exceeds 25mg/g. When the molar ratio of choline chloride to propionic acid is 1:3, the extraction effect is optimal, and the extraction rate of the ginsenoside is 31.7mg/g.
Example 4 influence of the Water content of the extraction solvent on the extraction of ginsenoside from ginseng residue
Choline chloride and propionic acid are mixed according to a mole ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent. Taking a certain amount of (absolute dry) licorice residues, crushing, sieving with a 80-mesh sieve, placing in a container, and respectively adding mixed liquid of 50%, 60%, 70%, 80% and 90% (volume percentage) of eutectic solvent and water, wherein the feed-liquid ratio is 1:20, ultrasonic extracting for 30min, extracting for 3 times, filtering, and collecting the extract and solid residue. The extraction rates of ginsenoside extracted from solvents with different water contents are shown in figure 5.
The extraction solvent with the water content of 10-50% can effectively extract the ginsenoside in the ginseng residue. When the volume percentage of the eutectic solvent is 70%, the optimal extraction rate of the total saponins of the ginseng is 33mg/g.
Example 5 Effect of feed liquid ratio on extraction of ginsenoside from Ginseng residue
Choline chloride and propionic acid are mixed according to a mole ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent. Taking a certain amount of (absolute dry) ginseng residues, crushing, sieving with a 80-mesh sieve, and placing into a container according to a feed-liquid ratio of 1: 15. 1: 20. 1: 25. 1:30. 1:35 adding extraction solvent, which is 70% (volume percentage) mixed solution of eutectic solvent and water, ultrasonic extracting for 30min, extracting for 3 times, filtering, and collecting extractive solution and solid residue. The extraction rate of ginsenoside with different feed liquid ratios is shown in figure 6.
The feed liquid ratio is 1:15-35g/mL can effectively extract ginsenoside in the ginseng residue. Feed liquid ratio 1:20-25g/mL has higher ginsenoside extraction rate, and the optimal extraction liquid-to-liquid ratio is 1:20, the extraction rate of the ginsenoside is 34.7mg/g.
Example 6 Effect of extraction time on extraction of ginsenoside from Ginseng radix residue
Choline chloride and propionic acid are mixed according to a mole ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent. Taking a certain amount of (absolute dry) ginseng residue, crushing, sieving with a 80-mesh sieve, and placing into a container according to a feed-liquid ratio of 1:20 adding 70% (volume percentage) mixed solution of eutectic solvent and water, respectively extracting with ultrasound for 10min, 20min, 30min, 40min, and 50min in a container for 3 times, filtering, and collecting extractive solution and solid residue. The extraction rate of ginsenoside is shown in figure 7.
Can effectively extract ginsenoside in the ginseng residue under the condition of 20-40 min. The optimal extraction time of the ginsenoside is 30min, and the extraction rate is 34.7mg/g.
Example 7
A method for extracting ginsenoside from ginseng residue and utilizing residue after extraction comprises the following steps:
(1) Choline chloride and ethylene glycol are mixed according to a mole ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent.
(2) Taking a certain amount of (absolute dry) ginseng residue, crushing, sieving with a 80-mesh sieve, and placing into a container according to a feed-liquid ratio of 1: adding 20g/mL of a mixed solution of the eutectic solvent and water, wherein the mixed solution contains 70% (volume fraction) of the eutectic solvent; ultrasonic extracting in a container for 30min, centrifuging, and collecting extractive solution and solid residue.
(3) The supernatant was concentrated to a certain volume by rotary evaporation under reduced pressure. The volume ratio of the concentrated extracting solution is 1:4 adding ethanol to precipitate for 16h, centrifuging, collecting filtrate as ginsenoside extractive solution, precipitating to obtain crude Ginseng radix polysaccharide, drying, and grinding into powder.
(4) Washing the extracted solid residue in the step (2) to be neutral by pure water, adding water, mixing (the mass ratio is 1:30) to form a mixed solution, soaking for 10 hours, centrifuging the mixed solution, taking the precipitate, and drying to obtain the ginseng residue dietary fiber.
Example 8
A method for extracting ginsenoside from ginseng residue and utilizing residue after extraction comprises the following steps:
(1) Choline chloride and diethylene glycol are mixed according to a molar ratio of 1:3 mixing, stirring for 30min at room temperature to form uniform transparent liquid, and obtaining the eutectic solvent.
(2) Taking a certain amount of (absolute dry) ginseng residue, crushing, sieving with a 80-mesh sieve, and placing into a container according to a feed-liquid ratio of 1: adding 20g/mL of a mixed solution of the eutectic solvent and water, wherein the mixed solution contains 70% (volume fraction) of the eutectic solvent; ultrasonic extracting in a container for 30min, centrifuging, and collecting extractive solution and solid residue.
(3) The supernatant was concentrated to a certain volume by rotary evaporation under reduced pressure. The volume ratio of the concentrated extracting solution is 1:3 adding ethanol for precipitation for 20h, centrifuging, collecting filtrate as ginsenoside extractive solution, precipitating to obtain crude ginseng polysaccharide, drying, and grinding into powder.
(4) The solid residue after the extraction in the step (2) is washed to be neutral with pure water and dried. Mixing with water (mass ratio of 1:25) to obtain mixed solution, soaking for 12 hr, centrifuging, collecting precipitate, and oven drying to obtain dietary fiber of Ginseng radix residue.
The oxidation resistance of the ginseng polysaccharide obtained in example 1, example 7, and example 8 is shown in fig. 8.
Claims (10)
1. A method for extracting ginsenoside from ginseng residue and utilizing residue after extraction is characterized by comprising the following steps:
1) Mixing choline chloride with propionic acid, ethylene glycol or diethylene glycol, and stirring at room temperature to obtain uniform transparent liquid to obtain eutectic solvent;
2) Adding an extraction solvent consisting of the eutectic solvent and water in the step 1) into the crushed ginseng residue, extracting, filtering and collecting an extracting solution to obtain a ginseng residue extracting solution and a solid residue;
3) Concentrating the extracting solution in the step 2), adding ethanol for precipitation, and centrifuging to obtain crude ginseng polysaccharide solid and ginseng saponin extracting solution;
4) Washing the solid residue extracted in the step 2) to be neutral by pure water, soaking in water, centrifuging, drying and crushing to obtain the ginseng residue dietary fiber.
2. The method for extracting ginsenoside from ginseng residue and utilizing residue after extraction of claim 1, wherein step 1) is performed to prepare a eutectic solvent composed of choline chloride and propionic acid.
3. The method for extracting ginsenoside from ginseng residue and utilizing residue after extraction according to claim 1, wherein the molar ratio of choline chloride to propionic acid, ethylene glycol or diethylene glycol in the eutectic solvent in step 1) is 1:3-1: 5.
4. the method for extracting ginsenoside from ginseng residue and utilizing residue after extraction of claim 1, wherein the volume percentage of the eutectic solvent in the extraction solvent of step 2) is 50-90%.
5. The method for extracting ginsenoside from ginseng residue and utilizing extracted residues according to claim 1, wherein the solid-to-liquid ratio of ginseng residue to extraction solvent in step 2) is 1:15-35 g/mL.
6. The method for extracting ginsenoside from ginseng residue and utilizing residue after extraction as claimed in claim 1, wherein the extraction time in the step 2) is 20-40 min.
7. The method for extracting ginsenoside from ginseng residue and utilizing residue after extraction of claim 1, wherein the ethanol added in the step 3) is 3-4 times of the volume of the extracting solution.
8. The method for extracting ginsenoside from ginseng residue and utilizing residue after extraction as claimed in claim 1, wherein the alcohol precipitation time in the step 3) is 12-24 hours.
9. The method for extracting ginsenoside from ginseng residue and utilizing extracted residues according to claim 1, wherein the mass ratio of solid residues to water in the step 4) is 1: 20-1: 30.
10. the method for extracting ginsenoside from ginseng residue and utilizing residue after extraction as claimed in claim 1, wherein the soaking time in the step 4) is 10-16 h.
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