CN111333746A - Extraction method of hericium erinaceus polysaccharide - Google Patents
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
The invention discloses a method for extracting hericium erinaceus polysaccharide, which comprises the following steps: pulverizing dried Hericium erinaceus raw material, and sieving to obtain Hericium erinaceus fine powder; soaking the hericium erinaceus fine powder in water, and performing pressure maintaining treatment under the ultrahigh pressure condition of 200-800 MPa to obtain a first mixture; and (3) quickly decompressing the first mixture, adding composite inorganic salt and water to obtain a second mixture, heating and leaching the second mixture, and performing separation and purification treatment to obtain the hericium erinaceus polysaccharide. According to the extraction method of the hericium erinaceus polysaccharide, the hericium erinaceus fine powder is subjected to ultrahigh-pressure wall breaking treatment to improve the dissolution rate of the polysaccharide; and then, hot inorganic salt solution is adopted for leaching, the process treatment flow is simple, the cost is lower, and the extraction rate of the polysaccharide is improved compared with a hot water leaching method.
Description
Technical Field
The invention relates to the technical field of edible mushroom deep processing,
in particular to a method for extracting hericium erinaceus polysaccharide.
Background
Hericium erinaceus is a large fleshy fungus commonly seen in the section or the tree hole of a broad-leaf trunk, turns yellow brown after being mature, is plush, is extremely similar to the brain bag of a mao monkey, and is a rare fungus with homology of medicine and food. The traditional Chinese medicine considers that the hericium erinaceus is neutral in nature and sweet in taste, is beneficial to five internal organs, helps digestion, has the effects of invigorating stomach, tonifying deficiency, resisting cancer and benefiting kidney essence, and is mainly used for treating symptoms such as loose stool, gastric and duodenal ulcer, superficial gastritis, neurasthenia, esophageal cancer, gastric cancer and the like. Hericium erinaceus is a medical and edible fungus, has been advocated by nutriologists and medical scientists all the time, and is a food deeply loved by consumers.
The hericium erinaceus polysaccharide is a main active ingredient of hericium erinaceus, has various physiological functions of improving immunity, resisting tumors, resisting aging, reducing blood fat and the like, is widely applied to the fields of medicines, functional foods, chemical industry and the like at present, and has wide market prospect.
At present, various extraction methods of hericium erinaceus polysaccharide are developed, such as hot water extraction, acid extraction, alkaline extraction, microwave-assisted extraction, ultrasonic-assisted extraction, enzymolysis and the like. The acid leaching method and the alkali leaching method have high polysaccharide extraction rate, but have high requirements on equipment, and the molecular structure of the polysaccharide is easily damaged by acid-base conditions; the hot water extraction method is most commonly used, but the polysaccharide yield obtained by single hot water extraction is low, and the molecular structure of the polysaccharide can be damaged by long-time high-temperature treatment; the reaction condition of the enzymolysis method is mild, the yield of the polysaccharide is relatively high, but the cost of the enzyme preparation is high, and the large-scale application of the enzyme preparation is limited. Although various extraction methods have been developed for extracting polysaccharide from Hericium erinaceus, these extraction methods have problems of high requirements for operation conditions, complex process, high energy consumption, high cost, or undesirable polysaccharide yield.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an extraction method of hericium erinaceus polysaccharide.
In order to solve the problems, the invention adopts the following technical scheme:
a method for extracting hericium erinaceus polysaccharide comprises the following steps:
pulverizing dried Hericium erinaceus raw material, and sieving to obtain Hericium erinaceus fine powder;
soaking the hericium erinaceus fine powder in water, and performing pressure maintaining treatment under the ultrahigh pressure condition of 200-800 MPa to obtain a first mixture;
and (3) quickly decompressing the first mixture, adding composite inorganic salt and water to obtain a second mixture, heating and leaching the second mixture, and performing separation and purification treatment to obtain the hericium erinaceus polysaccharide.
Preferably, the composite inorganic salt is a mixed salt of sodium chloride and potassium chloride, and the mass concentration of the sodium chloride in the second mixture is 0.5-1.2%, and the mass concentration of the potassium chloride in the second mixture is 0.3-0.8%.
Preferably, the feed-liquid ratio of the second mixture is 1: (16-30), wherein the heating temperature is 70-90 ℃, and the leaching time is 30-90 min.
Preferably, the feed-liquid ratio of the first mixture is 1: (10-15), wherein the ultrahigh pressure is 600MPa, and the pressure maintaining treatment time is 6 min.
Preferably, the mass concentration of the sodium chloride in the second mixture is 0.5-0.9%, and the mass concentration of the potassium chloride is 0.3-0.6%.
Preferably, the mass concentration of sodium chloride in the second mixture is 0.8%, and the mass concentration of potassium chloride in the second mixture is 0.3%.
Preferably, the feed-liquid ratio of the second mixture is 1: 20, the heating temperature is 80 ℃, and the leaching time is 90 min.
Preferably, the feed-liquid ratio of the first mixture is 1: 12, and the pressure maintaining treatment time is 6 min.
Preferably, the granularity of the hericium erinaceus fine powder is 40-80 meshes.
Preferably, the separation and purification treatment comprises the processes of solid-liquid separation, evaporation concentration, alcohol precipitation and vacuum freeze drying. Compared with the prior art, the invention has the technical effects that:
according to the extraction method of the hericium erinaceus polysaccharide, the hericium erinaceus fine powder is subjected to ultrahigh-pressure wall breaking treatment to improve the dissolution rate of the polysaccharide; and then, hot inorganic salt solution is adopted for leaching, the process treatment flow is simple, the cost is lower, and the extraction rate of the polysaccharide is improved compared with a hot water leaching method.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing dried Hericium erinaceus raw material, and sieving to obtain Hericium erinaceus fine powder;
(2) soaking the hericium erinaceus fine powder in water, and performing pressure maintaining treatment under the ultrahigh pressure condition of 200-800 MPa to obtain a first mixture;
(3) and (3) quickly decompressing the first mixture, adding composite inorganic salt and water into the mixture to obtain a second mixture, heating and leaching the second mixture, and separating and purifying to obtain the hericium erinaceus polysaccharide. The separation and purification treatment comprises the processes of solid-liquid separation, evaporation concentration, alcohol precipitation and vacuum freeze drying.
In the step (1), the granularity of the hericium erinaceus fine powder is 40-80 meshes.
In the step (2), 10-15 mL of water is added into each gram of hericium erinaceus fine powder, namely the material-liquid ratio of the first mixture is 1: (10-15), preferably, the material-liquid ratio of the first mixture is 1: 2. meanwhile, the pressure maintaining treatment time is controlled to be 5-10 min. Preferably, the ultrahigh pressure is 600MPa, and the pressure maintaining treatment time is 6 min. Under ultrahigh pressure, solvent water can quickly permeate into hericium erinaceus cells, and the ultrahigh pressure can cause the cells to be extruded to further cause cell membrane rupture, so that polysaccharide substances in the cells can be dissolved out easily. The hericium erinaceus fine powder is pretreated through ultrahigh pressure treatment, so that the wall breaking rate of cells is improved, and compared with simple mechanical wall breaking, the ultrahigh pressure treatment can improve the dissolution rate of polysaccharide.
In the step (3), the first mixture is rapidly decompressed within 3-5 s, then the compound inorganic salt of sodium chloride and potassium chloride is added, and a proper amount of water is added for blending, so that the mass concentration of the sodium chloride in the second mixture is 0.5% -1.2%, and the mass concentration of the potassium chloride in the second mixture is 0.3% -0.8%. The rapid pressure relief process can further improve the deformation and damage degree of cells and improve the dissolution rate of polysaccharide. The sodium chloride and potassium chloride are easily available, the cost is low, and no harmful substance is generated to the polysaccharide extraction system. The composite inorganic salt may be a mixed salt of sodium chloride and calcium chloride or a mixed salt of sodium chloride, potassium chloride and calcium chloride. Adding water to control the feed-liquid ratio of the second mixture to be 1: (16-30), preferably, the material-liquid ratio of the second mixture is 1: 20. and then, heating the second mixture at the temperature of 70-90 ℃ for 30-90 min. Preferably, the heating temperature is 80 ℃ and the leaching time is 90 min. The mass concentration of sodium chloride in the second mixture is 0.5-0.9%, and the mass concentration of potassium chloride is 0.3-0.6%. More preferably, the mass concentration of sodium chloride in the second mixture is 0.8% and the mass concentration of potassium chloride is 0.3%. The extraction rate of the polysaccharide can be improved by adjusting the mass concentration ratio of the sodium chloride to the potassium chloride in the second mixture. After the wall is broken by ultrasonic waves, the osmotic pressure inside and outside the hericium erinaceus cells can be adjusted by adding inorganic salt, the dissolution of polysaccharide is further promoted by utilizing the osmotic pressure difference inside and outside the cells, and the extraction rate of the polysaccharide is further improved.
According to the extraction method of the hericium erinaceus polysaccharide, the hericium erinaceus fine powder is subjected to ultrahigh-pressure wall breaking treatment to improve the dissolution rate of the polysaccharide; and then, hot inorganic salt solution is adopted for leaching, the process treatment flow is simple, the cost is lower, and the extraction rate of the polysaccharide is improved compared with a hot water leaching method.
The extraction rate of polysaccharide is determined by adopting a phenol-sulfuric acid method. The specific process is as follows: and (3) taking the polysaccharide solid after separation and purification in the step (3), dissolving in water, diluting to a certain multiple, measuring the absorbance value by adopting a phenol-sulfuric acid method, calculating the polysaccharide concentration in the diluent through a standard curve, calculating the polysaccharide content in the polysaccharide solid, and further calculating the polysaccharide extraction rate. Namely polysaccharide extraction rate = polysaccharide content/hericium erinaceus fine powder amount 100%.
Wherein, the standard curve drawing process is as follows: (1) drying a standard glucose sample at 105 ℃ for 2h to prepare a glucose standard solution of 40 ug/mL; (2) 25mL of 5% phenol solution is prepared; (3) accurately sucking 0, 0.1, 0.2, 0.3, 0.4, 0.5 and 0.6mL of glucose standard solution into a colorimetric tube by using a pipette, respectively adding 2mL of distilled water and 1mL of 5% phenol solution, uniformly mixing, respectively adding 5mL of concentrated sulfuric acid, standing for 5min, shaking uniformly, heating at 100 ℃ for 15min, cooling to room temperature, measuring an absorbance value at 490nm wavelength, and drawing a standard curve equation by taking the glucose concentration as a horizontal coordinate and the absorbance value as a vertical coordinate.
The following is a further description with reference to specific examples.
Example 1
The embodiment 1 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain Hericium erinaceus fine powder with particle size of 40 meshes;
(2) soaking Hericium erinaceus fine powder in 100mL of water, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing pressure to 200MPa, and maintaining pressure for 10min to obtain a first mixture;
(3) and (2) quickly decompressing the first mixture to normal pressure, adding 0.8g of sodium chloride, 1.28g of potassium chloride inorganic salt and 60mL of water into the first mixture to obtain a second mixture, heating the second mixture to 90 ℃, uniformly stirring and leaching the second mixture for 30min, centrifuging the second mixture to perform solid-liquid separation, performing rotary evaporation and concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 11.37% by phenol-sulfuric acid method.
Example 2
The embodiment 2 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) adding 120mL of water into the hericium erinaceus fine powder, soaking, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing the pressure to 400MPa, and carrying out pressure maintaining treatment for 8min under the condition to obtain a first mixture;
(3) and (2) rapidly decompressing the first mixture to normal pressure, adding 2g of sodium chloride, 2g of potassium chloride inorganic salt and 130mL of water into the first mixture to obtain a second mixture, heating the second mixture to 80 ℃, uniformly stirring and leaching for 60min, centrifuging to perform solid-liquid separation, performing rotary evaporation concentration, adding 95% ethanol with the volume being 3 times that of the second mixture to perform alcohol precipitation, and performing vacuum freeze drying to obtain the hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 13.79% as measured by the phenol-sulfuric acid method.
Example 3
The embodiment 3 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g dried Hericium erinaceus raw material, and sieving to obtain 80-mesh Hericium erinaceus fine powder;
(2) soaking Hericium erinaceus fine powder in 150mL of water, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing pressure to 800MPa, and maintaining pressure for 5min under the condition to obtain a first mixture;
(3) and (2) quickly relieving the pressure of the first mixture to normal pressure, adding 3.6g of sodium chloride, 0.9g of potassium chloride inorganic salt and 150mL of water into the first mixture to obtain a second mixture, heating the second mixture to 70 ℃, uniformly stirring and leaching the second mixture for 90min, centrifuging the second mixture to perform solid-liquid separation, performing rotary evaporation and concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 14.62% by phenol-sulfuric acid method.
Example 4
The embodiment 4 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) adding 120mL of water into the hericium erinaceus fine powder, soaking, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing the pressure to 600MPa, and carrying out pressure maintaining treatment for 6min under the condition to obtain a first mixture;
(3) and (2) quickly relieving the pressure of the first mixture to normal pressure, adding 1.6g of sodium chloride, 0.6g of potassium chloride inorganic salt and 80mL of water into the first mixture to obtain a second mixture, heating the second mixture to 80 ℃, uniformly stirring and leaching for 90min, centrifuging to perform solid-liquid separation, performing rotary evaporation concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 14.97% by phenol-sulfuric acid method.
Example 5
The embodiment 5 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) soaking Hericium erinaceus fine powder in 150mL of water, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing pressure to 500MPa, and maintaining pressure for 7min under the condition to obtain a first mixture;
(3) and (2) quickly decompressing the first mixture to normal pressure, adding 2.25g of sodium chloride, 1.0g of potassium chloride inorganic salt and 100mL of water into the first mixture to obtain a second mixture, heating the second mixture to 80 ℃, uniformly stirring and leaching the second mixture for 90min, centrifuging the second mixture to perform solid-liquid separation, performing rotary evaporation and concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 14.83% by phenol-sulfuric acid method.
Example 6
The embodiment 6 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) soaking Hericium erinaceus fine powder in 150mL of water, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing pressure to 600MPa, and maintaining pressure for 8min under the condition to obtain a first mixture;
(3) and (2) quickly decompressing the first mixture to normal pressure, adding 1.8g of sodium chloride, 1.5g of potassium chloride inorganic salt and 150mL of water into the first mixture to obtain a second mixture, heating the second mixture to 70 ℃, uniformly stirring and leaching the second mixture for 90min, centrifuging the second mixture to perform solid-liquid separation, performing rotary evaporation and concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 14.72% by phenol-sulfuric acid method.
Example 7
The embodiment 7 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) adding 120mL of water into the hericium erinaceus fine powder, soaking, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing the pressure to 600MPa, and carrying out pressure maintaining treatment for 6min under the condition to obtain a first mixture;
(3) and (2) quickly relieving the pressure of the first mixture to normal pressure, adding 1.6g of sodium chloride, 0.6g of calcium chloride inorganic salt and 80mL of water into the first mixture to obtain a second mixture, heating the second mixture to 80 ℃, uniformly stirring and leaching for 90min, centrifuging to perform solid-liquid separation, performing rotary evaporation concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of the polysaccharide was 14.58% by phenol-sulfuric acid method.
Example 8
The embodiment 8 of the invention provides an extraction method of hericium erinaceus polysaccharide, which comprises the following steps:
(1) pulverizing 10g of dried Hericium erinaceus raw material, and sieving to obtain 60-mesh Hericium erinaceus fine powder;
(2) adding 120mL of water into the hericium erinaceus fine powder, soaking, packaging, placing in ultrahigh pressure extraction equipment, rapidly increasing the pressure to 600MPa, and carrying out pressure maintaining treatment for 6min under the condition to obtain a first mixture;
(3) and (2) quickly relieving the pressure of the first mixture to normal pressure, adding 1g of sodium chloride, 0.6g of potassium chloride, 0.6g of calcium chloride inorganic salt and 80mL of water into the mixture to obtain a second mixture, heating the second mixture to 80 ℃, uniformly stirring and leaching the second mixture for 90min, centrifuging the second mixture to perform solid-liquid separation, performing rotary evaporation concentration, adding 3 times of volume of 95% ethanol to perform alcohol precipitation, and performing vacuum freeze drying to obtain a hericium erinaceus polysaccharide sample. The extraction rate of polysaccharide measured by phenol-sulfuric acid method was 15.03%.
Comparative example 1
The difference from example 1 is that in step (3), no inorganic salts such as sodium chloride and potassium chloride are added, and the other operation conditions are the same. The extraction rate of the polysaccharide was 9.86% by phenol-sulfuric acid method.
Comparative example 2
It is different from example 3 in that sodium chloride and potassium chloride inorganic salts are not added in step (3), and other operation conditions are the same. The extraction rate of the polysaccharide was 12.62% by phenol-sulfuric acid method.
Comparative example 3
The difference from example 5 is that in step (3), no inorganic salts such as sodium chloride and potassium chloride are added, and the other operating conditions are the same. The extraction rate of the polysaccharide was 12.94% by phenol-sulfuric acid method.
Comparative example 4
It is different from example 7 in that sodium chloride and calcium chloride inorganic salt are not added in step (3), and other operation conditions are the same. The extraction rate of polysaccharide was 12.77% by phenol-sulfuric acid method.
Comparative example 5
It is different from example 8 in that sodium chloride, potassium chloride and calcium chloride inorganic salt are not added in step (3), and other operation conditions are the same. The extraction rate of the polysaccharide was 12.83% by phenol-sulfuric acid method.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1. The extraction method of the hericium erinaceus polysaccharide is characterized by comprising the following steps:
pulverizing dried Hericium erinaceus raw material, and sieving to obtain Hericium erinaceus fine powder;
soaking the hericium erinaceus fine powder in water, and performing pressure maintaining treatment under the ultrahigh pressure condition of 200-800 MPa to obtain a first mixture;
and (3) quickly decompressing the first mixture, adding composite inorganic salt and water to obtain a second mixture, heating and leaching the second mixture, and performing separation and purification treatment to obtain the hericium erinaceus polysaccharide.
2. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, wherein the composite inorganic salt is a mixed salt of sodium chloride and potassium chloride, and the mass concentration of sodium chloride in the second mixture is 0.5% -1.2% and the mass concentration of potassium chloride in the second mixture is 0.3% -0.8%.
3. The extraction method of hericium erinaceus polysaccharide as claimed in claim 2, wherein the feed-liquid ratio of the second mixture is 1: (16-30), wherein the heating temperature is 70-90 ℃, and the leaching time is 30-90 min.
4. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, wherein the material-to-liquid ratio of the first mixture is 1: (10-15), and keeping the pressure for 5-10 min.
5. The extraction method of hericium erinaceus polysaccharide as claimed in claim 3, wherein the mass concentration of sodium chloride in the second mixture is 0.5-0.9%, and the mass concentration of potassium chloride is 0.3-0.6%.
6. The extraction method of hericium erinaceus polysaccharide according to claim 5, wherein the mass concentration of sodium chloride in the second mixture is 0.8%, and the mass concentration of potassium chloride is 0.3%.
7. The extraction method of hericium erinaceus polysaccharide as claimed in claim 3, wherein the feed-liquid ratio of the second mixture is 1: 20, the heating temperature is 80 ℃, and the leaching time is 90 min.
8. The extraction method of hericium erinaceus polysaccharide as claimed in claim 4, wherein the material-liquid ratio of the first mixture is 1: 12, the ultrahigh pressure is 600MPa, and the pressure maintaining treatment time is 6 min.
9. The method for extracting hericium erinaceus polysaccharide as claimed in claim 1, wherein the particle size of the hericium erinaceus fine powder is 40-80 meshes.
10. The method for extracting the hericium erinaceus polysaccharide as claimed in claim 1, wherein the separation and purification treatment comprises processes of solid-liquid separation, evaporation and concentration, alcohol precipitation and vacuum freeze drying.
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| CN112390897B (en) * | 2020-11-24 | 2022-09-30 | 邯郸学院 | Method for extracting and separating high-purity polysaccharide from plant flowers |
| CN113995069A (en) * | 2021-09-27 | 2022-02-01 | 邱成飞 | Hericium erinaceus and inulin composite beverage and preparation method thereof |
| CN114920857A (en) * | 2022-05-18 | 2022-08-19 | 徐州工程学院 | Method for extracting polysaccharide from hericium erinaceus spore powder |
| CN114920857B (en) * | 2022-05-18 | 2023-04-25 | 徐州工程学院 | Method for extracting polysaccharide from hericium erinaceus spore powder |
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