CN114377039A - Extraction and separation method of multiple components of ganoderma lucidum and application of extraction and separation method in preparation of artificially-planted ganoderma lucidum extract - Google Patents
Extraction and separation method of multiple components of ganoderma lucidum and application of extraction and separation method in preparation of artificially-planted ganoderma lucidum extract Download PDFInfo
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Abstract
The invention discloses an extraction and separation method of ganoderma lucidum multicomponent and application thereof in preparation of artificially-planted ganoderma lucidum extracts, and belongs to the technical field of ganoderma lucidum deep processing. The extraction and separation method of the ganoderma lucidum multi-component comprises the following steps: crushing lucid ganoderma, extracting, and performing multistage separation on the extract to obtain a ganoderan enrichment substance and a ganoderan enrichment substance, wherein the ratio of extracted materials to extracted liquids is 1: 18-22, the extraction temperature is 60-80 ℃, the multistage separation is to separate the extract by adopting a nanofiltration membrane with the molecular weight of 1000 to obtain ganoderan, and the nanofiltration membrane with the molecular weight of 500 to obtain the ganoderan. The preparation method of the invention effectively improves the purity of the beneficial components, the purity of the ganoderma lucidum polysaccharide can reach about 10%, the production cost of ganoderma lucidum products is reduced, the heavy metal and pesticide residue are obviously reduced, and the safety of the products is good.
Description
Technical Field
The invention relates to the technical field of deep processing of lucid ganoderma, in particular to an extraction and separation method of lucid ganoderma multi-component and application of the lucid ganoderma multi-component in preparation of artificially-planted lucid ganoderma extracts.
Background
Ganoderma is umbrella-shaped, pileus kidney-shaped, semicircular or nearly circular, and is fruiting body of Ganoderma of Polyporaceae. Chemical analysis shows that the glossy ganoderma seed and mycelium contain polysaccharide, amino acids, organic germanium, steroid and triterpene, and pharmacological research shows that the glossy ganoderma has the functions of protecting liver, detoxicating, strengthening heart, tranquilizing, relieving pain, treating tinnitus, benefiting lung qi, benefiting joint, etc. The chemical properties of ganoderma lucidum, particularly the chemical components contained in ganoderma lucidum, are the material basis for determining the properties of ganoderma lucidum. Modern nutritional ingredient analysis results show that the ganoderma lucidum is rich in nutritional ingredients and high in nutritional value, contains amino acids, fatty acids, major and trace elements, vitamin C, E, carotene and bioactive polysaccharides which are necessary for human bodies, and is a good source of dietary fibers which are necessary for human health.
The traditional extraction method of the ganoderma lucidum has low extraction efficiency, low purity of polysaccharide, great influence on the biological activity of the ganoderma lucidum and unsatisfactory economic benefit. The prior art discloses a method for extracting and separating multiple components of ganoderma lucidum spore powder, which comprises the steps of taking ganoderma lucidum spore powder as a raw material, adding water for soaking, adding complex enzyme in proportion for enzymolysis, performing ultrasonic reflux extraction, and performing centrifugal filtration to respectively obtain filtrate and filter residue; sterilizing the filtrate with microfiltration membrane, separating the filtrate with ultrafiltration membrane, and collecting Ganoderma polysaccharide solution and amino acid solution respectively; adding 75% v/v ethanol into the residue, percolating, centrifuging the percolate, concentrating, recovering ethanol to obtain Ganoderma triterpene soft extract; respectively obtaining extracts after freeze drying: ganoderan, Ganoderma triterpene, and Ganoderma amino acid. The extraction method needs a complex enzyme treatment process, has high extraction cost and complex operation, and finally improves the extraction amount of the total ganoderma lucidum polysaccharide and the purity of the extracted ganoderma lucidum polysaccharide and ganoderma lucidum triterpene compared with the existing water extraction and alcohol extraction.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings that the extraction efficiency of components such as ganoderma lucidum polysaccharide and the like is low, the extraction purity of ganoderma lucidum polysaccharide is low, and high-quality artificial ganoderma lucidum products cannot be prepared in the existing ganoderma lucidum deep processing, and provides a method for extracting and separating multiple components of ganoderma lucidum.
The above purpose of the invention is realized by the following technical scheme:
a method for extracting and separating multiple components of Ganoderma comprises the following steps:
crushing Ganoderma, extracting, multi-stage separating extract to obtain ganoderan concentrate and Ganoderma triterpene concentrate,
wherein the ratio of the extracted material to the liquid is 1: 18-22, the extraction temperature is 60-80 ℃,
the multi-stage separation is to separate the extract by adopting a nanofiltration membrane with the molecular weight of 1000 to obtain the ganoderan enrichment and a nanofiltration membrane with the molecular weight of 500 to obtain the ganoderma triterpene enrichment.
In a specific manner, the extraction temperature of the extraction can affect the extraction purity of the relevant polysaccharide, and can also affect the extraction yield of the extracted product, i.e. the extraction yield and the subsequent separation effect.
The temperature of the nanofiltration membrane multistage separated substance after vacuum concentration and vacuum drying is lower than that of the traditional treatment process, so that the effective substances can be kept, and the extraction purity of the ganoderan and the ganoderma triterpene can be improved.
The selection of the molecular weight of the nanofiltration membrane for multistage separation is also crucial, and the ganoderma lucidum polysaccharide is separated by adopting the nanofiltration membrane with the molecular weight of 1000, so that the purity of the ganoderma lucidum polysaccharide in the ganoderma lucidum extract can be further improved.
Preferably, the extract is subjected to centrifugal microfiltration treatment before the multistage separation, and the microfiltration clear liquid is subjected to multistage separation through membrane separation.
Wherein, pure water with the mass of 5-10% of the extract is additionally added in the centrifugal treatment process. Residual feed liquid of the centrifugal machine can be exchanged through water replenishing treatment, and the purification effect of centrifugal separation treatment is better.
Preferably, the filtering pressure of the microfiltration treatment is less than or equal to 0.32MPa, and the filtering temperature is less than or equal to 55 ℃.
The pressure is controlled in order to ensure that the filtering effect is better, the aperture of the ceramic membrane is changed along with the increase of the temperature, the filtration rate of the material liquid is improved, but the filtration purity is reduced, and the product quality is influenced.
Wherein, pure water with the mass of 15-20% of the extract is additionally added in the microfiltration treatment process. Pure water is added in the microfiltration treatment, so that the microfiltration treatment temperature can be reduced to achieve better membrane filtration effect, and the concentration of the filtered liquid can be diluted to obtain effective components through separation to a greater extent.
The microfiltration process of the invention adopts an ultrafiltration membrane to remove a large amount of macromolecular impurities, so that the purity of the extract is improved, and the ganoderma lucidum effective components in the prepared ganoderma lucidum extract, such as ganoderma lucidum polysaccharide and ganoderma lucidum triterpene, are obviously higher than the standard.
Preferably, the multistage separation comprises vacuum concentration and vacuum drying after separation, wherein the vacuum concentration temperature is 65-75 ℃, and the vacuum concentration vacuum degree is less than or equal to-0.095 MPa.
Preferably, the temperature of the vacuum drying is 70-75 ℃, and the vacuum degree of the vacuum drying is less than or equal to-0.097 MP.
The temperature of the nanofiltration membrane multistage separation material after vacuum concentration and vacuum drying is lower than that of the traditional treatment process, and the retention of effective substances is facilitated.
In a specific embodiment, the extraction method of the present invention is preferably a wall-broken extraction.
In a specific embodiment, in order to further optimize the extraction effect, the cycle time of the wall-breaking extraction is preferably 15-20 min.
More preferably, the cycle time of the wall-breaking extraction is 18 min.
Preferably, the ratio of the extracted feed to the liquid is 1:20, and the extraction temperature is 60 ℃.
In a specific embodiment, the method for extracting the components of ganoderma lucidum can specifically refer to the following details:
(1) pulverizing (crushing), crushing wild Ganoderma, and pulverizing to obtain Ganoderma powder;
(2) feeding: putting the mixed raw materials into a feeding tank, adding water and stirring uniformly;
(3) extraction: conveying the feed liquid to an extraction and wall-breaking unit for extraction;
(4) centrifuging: centrifuging the material extracting solution to obtain a centrifugate;
(5) and (3) microfiltration: filtering the centrifugate by a ceramic membrane to obtain a microfiltration clear liquid;
(6) membrane separation: carrying out multi-stage separation on the microfiltration clear liquid of the wild ganoderma lucidum:
firstly, a nanofiltration membrane with the molecular weight of 1000 is selected for separation to obtain a beneficial component concentrate with the main component of ganoderma lucidum polysaccharide; then separating by using a nanofiltration membrane with the molecular weight of 500 to obtain a beneficial component concentrate of which the main component is ganoderma triterpene;
(7) and (3) vacuum concentration: carrying out vacuum concentration on the membrane separation liquid, and collecting when the concentration of the extract is controlled to be 28-32 Baume;
(8) vacuum drying to obtain the enrichment of beneficial components of wild Ganoderma.
The residual liquid of the extracting solution is abandoned in the membrane separation step, and the ganoderma lucidum extract prepared by the method has the advantages of obviously reduced heavy metal and pesticide residues and better product safety.
The invention also specifically protects the application of the multi-component extraction and separation method of the ganoderma lucidum in the preparation of artificially planted ganoderma lucidum extracts.
The application of the ganoderma lucidum essence can comprise preparation of instant ganoderma lucidum essence and can also comprise preparation of artificial ganoderma lucidum matched instant ganoderma lucidum essence.
The specific method for preparing the artificial ganoderma lucidum blended instant ganoderma lucidum essence can refer to the following steps:
extracting wild Ganoderma according to the above method, and performing multi-stage separation to obtain ganoderan concentrate and Ganoderma triterpene concentrate;
extracting artificial Ganoderma according to the above method, and performing multi-stage separation to obtain ganoderan concentrate and Ganoderma triterpene concentrate;
the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate of the artificial ganoderma lucidum are matched according to the mass ratio of the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate in the wild ganoderma lucidum to obtain the artificial planted ganoderma lucidum instant essence.
The wild ganoderma lucidum is expensive, the extraction purity of characteristic active ingredients of the wild ganoderma lucidum is low by the existing extraction method, the wild ganoderma lucidum cannot be effectively utilized, and the production cost of ganoderma lucidum products is increased. The lucid ganoderma instant essence uses artificially-planted lucid ganoderma as a raw material, but the characteristics of a brewed solution of the lucid ganoderma instant essence are very close to those of a wild lucid ganoderma solution, the lucid ganoderma instant essence can be used as a substitute of the wild lucid ganoderma, and the production cost of the lucid ganoderma instant essence is reduced.
The artificially-planted ganoderma lucidum instant essence prepared by the method has definite component proportion, can be produced in a standardized way, and obviously improves the batch consistency of products.
Compared with the prior art, the invention has the beneficial effects that:
the extraction and separation method of the ganoderma lucidum multicomponent disclosed by the invention has the advantages that the specific extraction process is combined with nanofiltration membranes of different molecular weight grades for filtration, the extraction purity of ganoderma lucidum polysaccharide and ganoderma lucidum triterpene in ganoderma lucidum is obviously improved, the content of ganoderma lucidum polysaccharide can reach about 10%, the content of ganoderma lucidum triterpene can reach more than 2.25mg/g, which is obviously higher than the standard of Chinese pharmacopoeia, the metal and pesticide residues in ganoderma lucidum extract are obviously reduced by further combining the separation and purification process, the biological safety is obviously improved, the high-quality manufacture of artificially-planted ganoderma lucidum extract is realized, and the production cost of ganoderma lucidum products is greatly reduced.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A method for extracting and separating multiple components of Ganoderma comprises the following steps:
crushing Ganoderma, extracting, and separating the extract to obtain Ganoderma polysaccharide concentrate and Ganoderma triterpene concentrate.
The specific operation is as follows:
1. crushing (breaking): crushing 5Kg of lucid ganoderma, and then crushing the lucid ganoderma to pass through a 30-mesh screen;
2. feeding: feeding 5Kg of mixed raw material into a feeding tank, adding 100L of hot water according to the material-water ratio of 1:20, keeping the temperature of the material liquid at 60 ℃, and uniformly stirring;
3. extraction: conveying the feed liquid to an extraction and wall-breaking machine set for extraction, wherein the extraction cycle time is 18 min;
4. centrifuging: centrifuging the material extracting solution, wherein the frequency of a main centrifugal machine is 42.0Hz, the frequency of an auxiliary machine is 32.0Hz, the feeding frequency is 11.0Hz, and 10 percent of pure water is additionally added in the centrifuging process;
5. and (3) microfiltration: filtering the centrifugate with ceramic membrane at 50 deg.C under 0.32MPa, and adding 15% pure water during microfiltration process;
6. membrane separation: performing multi-stage separation on the lucid ganoderma microfiltration clear liquid, and firstly selecting a nanofiltration membrane with the molecular weight of 1000 for separation to obtain a beneficial component concentrate with the main component of ganoderma lucidum polysaccharide; then separating by using a nanofiltration membrane with the molecular weight of 500 to obtain a beneficial component concentrate of which the main component is ganoderma triterpene; discarding the extraction residue;
7. vacuum concentration, namely performing vacuum concentration on the membrane concentrated solution at the concentration temperature of 70 ℃ and the vacuum degree of-0.090 MPa, and collecting when the concentration of the extract is controlled at 30 Baume.
8. Vacuum drying, namely performing vacuum drying on the concentrated extract at the drying temperature of 70 ℃ and the vacuum degree of-0.090 MPa.
Example 2
A method for preparing artificial Ganoderma compounded instant Ganoderma essence comprises:
extracting wild ganoderma according to the method for extracting and separating the ganoderma multicomponent of the embodiment 1, and performing multi-stage separation to obtain ganoderma polysaccharide concentrate and ganoderma triterpene concentrate;
extracting artificial ganoderma according to the method for extracting and separating the ganoderma multi-component in the embodiment 1, and performing multi-stage separation to obtain ganoderma polysaccharide concentrate and ganoderma triterpene concentrate;
the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate of the artificial ganoderma lucidum are matched according to the mass ratio of the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate in the wild ganoderma lucidum to obtain the artificial planted ganoderma lucidum instant essence.
Example 3
A method for extracting and separating multiple components of Ganoderma comprises the following steps:
crushing Ganoderma, extracting, and separating the extract to obtain Ganoderma polysaccharide concentrate and Ganoderma triterpene concentrate.
The specific operation is as follows:
1. crushing (breaking): crushing 5Kg of lucid ganoderma, and then crushing the lucid ganoderma until the lucid ganoderma can pass through a 30-mesh screen.
2. Feeding: 5Kg of mixed raw material is put into a feeding tank, 100L of hot water is added according to the material-water ratio of 1:20, the temperature of the material liquid is controlled at 80 ℃, and the mixture is stirred uniformly.
3. Extraction: and (3) conveying the feed liquid to an extraction and wall-breaking machine set for extraction, wherein the extraction cycle time is 20 min.
4. Centrifuging: centrifuging the material extractive solution with main centrifugal machine frequency of 42.0Hz, auxiliary machine frequency of 32.0Hz, and feeding frequency of 14.0Hz, and supplementing 5% pure water in the centrifuging process.
5. And (3) microfiltration: and (3) filtering the centrifugate by using a ceramic membrane, wherein the operating pressure is 0.32MPa, the temperature is 55 ℃, and 20 percent of pure water is additionally added in the microfiltration process.
6. Membrane separation: performing multi-stage separation on the lucid ganoderma microfiltration clear liquid, and firstly selecting a nanofiltration membrane with the molecular weight of 1000 for separation to obtain a beneficial component concentrate with the main component of ganoderma lucidum polysaccharide; then separating by using a nanofiltration membrane with the molecular weight of 500 to obtain a beneficial component concentrate of which the main component is ganoderma triterpene; discarding the extraction residue;
7. vacuum concentration, namely performing vacuum concentration on the membrane concentrated solution at the concentration temperature of 65 ℃ and the vacuum degree of-0.095 MPa, and collecting when the concentration of the extract is controlled to be 30 Baume.
8. And (3) vacuum drying: vacuum drying the concentrated extract at 75 deg.C under-0.097 MPa.
Example 4
A method for preparing artificial Ganoderma compounded instant Ganoderma essence comprises:
extracting wild ganoderma lucidum according to the method for extracting and separating the ganoderma lucidum multicomponent in the embodiment 2, and performing multi-stage separation to obtain ganoderma lucidum polysaccharide concentrate and ganoderma lucidum triterpene concentrate;
extracting artificial ganoderma lucidum according to the method for extracting and separating the ganoderma lucidum multicomponent in the embodiment 2, and performing multi-stage separation to obtain ganoderma lucidum polysaccharide concentrate and ganoderma lucidum triterpene concentrate;
the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate of the artificial ganoderma lucidum are matched according to the mass ratio of the ganoderma lucidum polysaccharide concentrate and the ganoderma lucidum triterpene concentrate in the wild ganoderma lucidum to obtain the artificial planted ganoderma lucidum instant essence.
Comparative example 1
A Ganoderma extract prepared according to CN 106072632A in example 1 and its preparation method are provided.
Result detection
(1) Detection of ganoderan
Configuring a to-be-tested product: taking about 2g of powder, precisely weighing, placing in a round-bottom flask, adding 50mL of boiling water bath, heating for 1 hour, filtering while hot, washing the filter paper with boiling water for multiple times, cooling the filtrate, fixing the volume to 100mL, shaking up, precisely measuring 5mL, slowly adding 75mL of ethanol dropwise while stirring, shaking up, placing at 4 ℃ for 12 hours, centrifuging, discarding the supernatant, dissolving the precipitate with hot water, transferring to a 50mL measuring flask, cooling, adding water to the scale, shaking up, taking a proper amount of solution, centrifuging, precisely measuring 3mL of the supernatant, placing in a 25mL measuring flask, adding water to the scale, and shaking up to obtain the product.
Preparation of control solutions: taking a proper amount of anhydrous glucose reference substance, precisely weighing, and adding water to obtain a solution containing 0.12mg per 1 mL.
Preparation of a standard curve: precisely measuring reference substance solutions 0.2mL, 0.4mL, 0.6 mL, 0.8mL, 1.0 mL and 1.2mL, respectively placing in 10mL test tubes with plugs, respectively adding water to 2.0mL, rapidly and precisely adding anthrone sulfate solution (precisely weighing 0.1g anthrone, adding 100mL sulfuric acid to dissolve and shake) 6mL, immediately shaking, standing for 15 minutes, immediately placing in ice bath for cooling for 15 minutes, taking out, taking corresponding reagents as blank, irradiating with ultraviolet-visible spectrophotometry (general rule 0401), measuring absorbance at 625nm wavelength, and drawing standard curve with absorbance as ordinate and concentration as abscissa.
The determination method comprises the following steps: precisely measuring 2mL of the test solution, placing the test solution into a 10mL test tube with a plug, operating the method according to the standard curve preparation item from the step of rapidly and precisely adding 6mL of the anthrone sulfate solution, measuring absorbance, reading the content of the anhydrous glucose in the test solution from the standard curve, and calculating to obtain the test solution.
The content of the sample contains ganoderan and anhydrous glucose (C) calculated according to the dry product6H12O6) And (6) counting.
(2) Detection of ganoderma triterpene
Configuring a to-be-tested product: taking about 2g of the powder, precisely weighing, adding into a 250mL conical flask with a plug, accurately adding 50mL of absolute ethanol, tightly covering the plug, shaking, placing in an ultrasonic extractor for ultrasonic extraction for 1h, frequently shaking, mixing uniformly after extraction, centrifuging in a centrifuge with a proper volume of 8000r/min for 10min, and taking the supernatant as a sample extracting solution for later use.
Standard curve: accurately transferring oleanolic acid standard stock solutions of 0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL and 0.5mL, placing in a 10mL test tube, wherein the standard quality amounts are 0 μ g, 20 μ g, 40 μ g, 60 μ g, 80 μ g and 100 μ g respectively. Placing the test tube in a water bath kettle at the temperature of 90-100 ℃ to volatilize the solvent, adding 0.1mL of 5% vanillin glacial acetic acid solution and 0.8mL of perchloric acid, uniformly mixing, and then carrying out heat preservation and color development in a water bath at the temperature of 60 ℃ for 20 min. Taking out, rapidly placing in an ice water bath, cooling for 3-5 min, stopping the color reaction, adding 5.0mL of glacial acetic acid, uniformly mixing, placing at room temperature for 10min, immediately using a 1cm cuvette, adjusting the zero point by using a 0 tube, and measuring the absorbance at the wavelength of 550 nm. And drawing a standard curve by taking the mass of the oleanolic acid standard product as a vertical coordinate and the corresponding absorbance as a horizontal coordinate.
And (3) sample determination: accurately transferring 0.3mL of sample extracting solution into a 10mL test tube, placing the test tube in a water bath kettle at the temperature of 90-100 ℃ to volatilize the solvent, simultaneously making a reagent blank, and calculating the total triterpene content according to the absorbance of the sample extracting solution. If the total triterpene content of the sample is determined to be out of the range of the standard curve, the sample is diluted appropriately or the volume of the sample removed is increased and then the total triterpene content is determined again.
Wherein the test results of the examples and comparative examples are described in the following table 1:
table 1.
| Composition (I) | Example 1 | Example 2 | Comparative example 1 | Standard requirements |
| Ganoderma lucidum polysaccharide (%) | 9.31 | 8.93 | 4.19 | Chinese pharmacopoeia (more than or equal to 0.9%) |
| Ganoderma triterpene (%) | 2.29 | 2.25 | 2.15 | Chinese pharmacopoeia (more than or equal to 0.5%) |
As can be seen from the above table, the effective components of the ganoderma lucidum obtained by the preparation method of the invention are enriched and are obviously higher than the products prepared by the standard and common methods.
In order to further determine the safety of the artificial ganoderma lucidum extract, relevant heavy metal and pesticide residue indexes are detected, and the detection results are shown in the following table 2:
TABLE 2 indexes of heavy metals and pesticide residues
As can be seen from the detection results in Table 2, the Ganoderma lucidum extract prepared by the method of the present invention has significantly low heavy metal and pesticide residues, is lower than the relevant standard requirements, and has good safety.
(4) Economy of use
The ganoderma lucidum extract prepared by the multi-component ganoderma lucidum extraction method can be prepared by taking artificially planted ganoderma lucidum as a raw material, extracting the ganoderma lucidum extract with high ganoderma lucidum polysaccharide and ganoderma lucidum triterpene contents, and the requirements of wild ganoderma lucidum extract products are met by blending the ganoderma lucidum extract, so that the quality requirements of the wild ganoderma lucidum products can be met in component quality, the production cost is greatly reduced by the blending of the artificial ganoderma lucidum extract, and the specific cost reduction condition is shown in table 3.
TABLE 3
| Item | Price |
| Price of wild Ganoderma | 180 yuan/kg |
| Price of artificial glossy ganoderma | 48 yuan/kg |
| The amount of wild Ganoderma required for single product | 6g |
| The amount of artificial Ganoderma required for single product | 10g |
From the above table, it can be seen that the cost price of the amount of wild ganoderma lucidum required for producing a single specification product can be calculated according to the amount of wild ganoderma lucidum required for producing a single specification product as follows: 180 x 6 ═ 1080 units.
The cost price of the artificial ganoderma lucidum required by producing the single specification product can be calculated according to the artificial ganoderma lucidum required by producing the single specification product as follows: 48 x 10 ═ 480 element
The cost price comparison shows that the production cost of the artificial planted ganoderma lucidum instant essence can be reduced by 600 yuan, and the cost of the artificial ganoderma lucidum instant essence produced by adopting the artificial ganoderma lucidum instant essence has the same effect as that of wild ganoderma lucidum is only 44.4 percent of that of the wild ganoderma lucidum, so that the cost is obviously reduced, and the economic benefit is improved.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The extraction and separation method of the ganoderma lucidum multicomponent is characterized by comprising the following steps:
breaking cell wall of Ganoderma, extracting, separating the extract at multiple stages to obtain ganoderan concentrate and Ganoderma triterpene concentrate,
wherein the ratio of the extracted material to the liquid is 1: 18-22, the extraction temperature is 60-80 ℃,
the multi-stage separation is to separate the extract by adopting a nanofiltration membrane with the molecular weight of 1000 to obtain the ganoderan enrichment and a nanofiltration membrane with the molecular weight of 500 to obtain the ganoderma triterpene enrichment.
2. The method for multi-component extraction and separation of ganoderma lucidum according to claim 1, wherein the extract is subjected to centrifugal microfiltration before multi-stage separation, and the microfiltration clear solution is subjected to multi-stage separation by a nanofiltration membrane.
3. The method for extracting and separating the components from the ganoderma lucidum as claimed in claim 2, wherein the microfiltration pressure is less than or equal to 0.32MPa and the filtration temperature is less than or equal to 55 ℃.
4. The method for extracting and separating the multiple components of the ganoderma lucidum as claimed in claim 2, wherein pure water accounting for 15-20% of the mass of the extract is added in the microfiltration process.
5. The method for extracting and separating the components of the ganoderma lucidum as claimed in claim 1, wherein the multi-stage separation comprises vacuum concentration and vacuum drying after separation, wherein the temperature of the vacuum concentration is 65-75 ℃, and the vacuum degree of the vacuum concentration is less than or equal to-0.095 MPa.
6. The method for extracting and separating the components of the ganoderma lucidum as claimed in claim 4, wherein the temperature of the vacuum drying is 70-75 ℃, and the vacuum degree of the vacuum drying is less than or equal to-0.097 MP.
7. The extraction and separation method of the ganoderma lucidum multicomponent, according to claim 6, wherein the wall-breaking extraction is a cycle extraction, and the cycle time is 15-20 min.
8. The method for extracting and separating the components from the ganoderma lucidum as claimed in claim 7, wherein the cycle time of the wall-breaking extraction is 18 min.
9. The method for extracting and separating the components of the ganoderma lucidum as claimed in claim 1, wherein the ratio of the extracted material liquid of the wall-breaking extraction is 1:20, and the extraction temperature is 60 ℃.
10. An application of the multi-component extraction and separation method of ganoderma lucidum as claimed in any one of claims 1-9 in preparation of artificially planted ganoderma lucidum extracts.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903331A (en) * | 2017-12-22 | 2018-04-13 | 福建农大菌草技术开发公司 | The method of disposable quick separating ganoderma active polysaccharide peptide and triterpenic acid |
| CN110330575A (en) * | 2019-07-15 | 2019-10-15 | 浏阳朗林生物科技有限公司 | A kind of preparation method of Ganodenna Lucidum P.E |
| CN110833567A (en) * | 2019-11-28 | 2020-02-25 | 福建省幸福生物科技有限公司 | Method for multi-component extraction and separation of ganoderma lucidum spore powder |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903331A (en) * | 2017-12-22 | 2018-04-13 | 福建农大菌草技术开发公司 | The method of disposable quick separating ganoderma active polysaccharide peptide and triterpenic acid |
| CN110330575A (en) * | 2019-07-15 | 2019-10-15 | 浏阳朗林生物科技有限公司 | A kind of preparation method of Ganodenna Lucidum P.E |
| CN110833567A (en) * | 2019-11-28 | 2020-02-25 | 福建省幸福生物科技有限公司 | Method for multi-component extraction and separation of ganoderma lucidum spore powder |
Non-Patent Citations (4)
| Title |
|---|
| 宋伟杰: "膜分离技术在食用菌多糖分离纯化中的应用研究进展", 《食用菌》 * |
| 李艳: "灵芝多糖提取工艺研究" * |
| 王博: "响应面优化超滤膜分离灵芝多糖工艺" * |
| 蔡铭: "基于膜技术的灵芝粗多糖分级分离及抗氧化活性比较", 《食品工业科技》 * |
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