Extraction method of tremella polysaccharide and application of tremella polysaccharide in tobacco

The use of a mixed solvent of ethanol and 1-propoxy-2-propanol was solved by the freezing-thawing wall breaking and alkali extraction and precipitation method, and the problem of low extraction yield and purity of Tremella polysaccharides was achieved, and efficient extraction was achieved in tobacco Improves smoke comfort when applied.

CN119462982AActive Publication Date: 2025-02-18CHINA TOBACCO HEBEI INDUSTRIAL CO LTD

Patent Information

Application Number
CN202411583837.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-07
Publication Date
2025-02-18
Estimated Expiration
2044-11-07

AI Technical Summary

Technical Problem

In the prior art, the extraction yield and purity of Tremella polysaccharides are relatively low, making it difficult to meet the needs of efficient extraction.

Method used

The freezing-thawing method was used to extract the Tremella polysaccharides by combining alkali extraction and precipitation. The precipitation was performed using a mixed solvent of ethanol and 1-propoxy-2-propanol. By adjusting the volume ratio and precipitation conditions of the precipitation solvent, the Efficient extraction of thremella polysaccharide.

Benefits of technology

The extraction yield and purity of Tremella polysaccharides was significantly improved, reaching a purity of 96.1% and a 35.2% yield, and when used in tobacco, the comfort of the smoke was improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of polysaccharide, and provides an extraction method of tremella polysaccharide and application of the tremella polysaccharide to tobacco, the extraction method of the tremella polysaccharide comprises the following steps: S1, freezing and melting tremella, adding a solvent, pulping, and centrifuging to obtain a mixed solution I; s2, alkali liquor is added into the mixed solution I for alkali extraction, acid adjustment and centrifugation, and a mixed solution II is obtained; s3, concentrating, precipitating, filtering and drying the mixed solution II to obtain tremella polysaccharide; the solvent of the precipitation comprises ethanol and 1-propoxy-2-propanol; the volume ratio of the ethanol to the 1-propoxy-2-propanol is (1: 20) to (20: 1). According to the technical scheme, the problems of low yield and purity of tremella polysaccharide extracted in related technologies are solved.
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Description

Technical Field

[0001] The invention relates to the technical field of polysaccharide extraction, and in particular to a method for extracting tremella polysaccharide and application thereof on tobacco. Background Art

[0002] Tremella polysaccharide is an acidic heteropolysaccharide obtained from Tremella fruiting bodies. Its main chain structure is mannan connected by glycosidic bonds, and its side chains are composed of glucuronic acid and xylose. Tremella polysaccharide is a basidiomycete polysaccharide immunopotentiator, which has the effect of improving the body's immune function and increasing white blood cells. The immune function of Tremella polysaccharide is mainly concentrated in two aspects. One is to target the non-immune system and promote the growth of beneficial microorganisms in the gastrointestinal tract; the other is to target the immune defense system, improve humoral immunity, and enhance the phagocytic ability of phagocytes; in addition to enhancing the body's immunity, Tremella polysaccharide can also promote protein and nucleic acid synthesis, increase its own repair ability, and maintain the function of various organs and tissues, especially the liver. Because Tremella polysaccharide contains a large number of hydroxyl groups, adding it to tobacco can maintain the moisture of tobacco, make the smoke softer, reduce the irritation and roughness caused by tobacco drying, and thus improve the comfort of cigarette smoke. At present, the traditional extraction method of Tremella fuciformis polysaccharide is hot water extraction, but the yield and purity of Tremella fuciformis polysaccharide obtained by this method are low. Therefore, how to improve the extraction yield and purity of Tremella fuciformis polysaccharide is a problem that needs to be solved at present. Summary of the invention

[0003] The invention provides a method for extracting tremella polysaccharide and application thereof on tobacco, thereby solving the problem of low yield and purity of tremella polysaccharide extraction in the related art.

[0004] The technical solution of the present invention is as follows: The present invention provides a method for extracting Tremella polysaccharide, comprising the following steps: S1, freezing and thawing Tremella fuciformis, adding a solvent to pulp, and centrifuging to obtain a mixed solution I; S2, adding alkali solution to the mixed solution I for alkali extraction, adjusting the acidity, and centrifuging to obtain a mixed solution II; S3, concentrating, precipitating, filtering and drying the mixed solution II to obtain Tremella polysaccharide; The precipitated solvent includes ethanol and 1-propoxy-2-propanol; the volume ratio of the ethanol to the 1-propoxy-2-propanol is 1:20 to 20:1.

[0005] As a further technical solution, the volume ratio of the ethanol to the 1-propoxy-2-propanol is 1:9~9:1.

[0006] As a further technical solution, in step S3, the mixed solution II is concentrated, precipitated for the first time, precipitated for the second time, filtered, and dried to obtain Tremella polysaccharide.

[0007] In the present invention, the Tremella polysaccharide is precipitated twice, thereby further improving the extraction yield and purity of the Tremella polysaccharide.

[0008] As a further technical solution, the volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the first precipitation and the solvent of the second precipitation is different.

[0009] In the present invention, the volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the first precipitation and the solvent of the second precipitation is different, thereby further improving the yield and purity of Tremella polysaccharide extraction.

[0010] As a further technical solution, the volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the first precipitation is 1:9; the volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the second precipitation is 9:1.

[0011] In the present invention, the volume ratio of ethanol and 1-propoxy-2-propanol in the solvent of the first precipitation is limited to 1:9, and the volume ratio of ethanol and 1-propoxy-2-propanol in the solvent of the second precipitation is limited to 9:1, thereby further improving the yield and purity of Tremella polysaccharide.

[0012] As a further technical solution, in step S1, the solvent includes 80-90 parts of water, 1-3 parts of sodium lauryl sulfate, and 3-8 parts of polyoxyethylene ether.

[0013] In the present invention, the extraction yield of Tremella polysaccharide is further improved by limiting the pulping solvent to consist of water, sodium lauryl sulfate and polyoxyethylene ether.

[0014] As a further technical solution, in step S2, the alkali solution is a 20wt% sodium carbonate aqueous solution; the acid adjustment reagent is 5mol / L HCl; and the acid is adjusted to a pH value of 5-6.

[0015] As a further technical solution, in step S2, the temperature of the alkali extraction is 70-80°C, and the time of the alkali extraction is 3-5h.

[0016] As a further technical solution, in step S3, the precipitation temperature is -10~-5°C, and the precipitation time is 2~5h.

[0017] The invention also provides an extraction method for tremella polysaccharide and application of the prepared tremella polysaccharide in tobacco.

[0018] The working principle and beneficial effects of the present invention are: The present invention provides a method for extracting tremella polysaccharide. Firstly, a freeze-thaw method is used to break the wall of tremella to release the tremella polysaccharide therein, and the tremella polysaccharide is extracted by alkali extraction and precipitation method, wherein the precipitating solvent is composed of ethanol and 1-propoxy-2-propanol, thereby improving the extraction yield and purity of the tremella polysaccharide, and applying the tremella polysaccharide to shredded tobacco has a better smoking effect. DETAILED DESCRIPTION

[0019] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] In the following embodiments and comparative examples: Polyoxyethylene ether, model: AEO-9.

[0021] Example 1 A method for extracting Tremella polysaccharide comprises the following steps: S1. Freeze and melt 1 kg of Tremella fuciformis, add 5 L of solvent (the solvent is water) to pulp, and centrifuge to obtain a mixed solution I; S2, adding 1L of 20wt% sodium carbonate aqueous solution to the mixed solution I, extracting at 70°C for 5h, adding 5mol / L HCl to adjust the pH to 5, and obtaining a mixed solution II after centrifugation; S3. Concentrate the mixed solution II to one fifth of its original volume, add 3 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 1:20, precipitate at -10°C for 2 h, filter and dry the precipitate to obtain 366.3 g of Tremella polysaccharide with a purity of 96.1% and a yield of 35.2%.

[0022] Example 2 A method for extracting Tremella polysaccharide comprises the following steps: S1. Freeze and melt 1 kg of Tremella fuciformis, add 5 L of solvent (the solvent is water) to pulp, and centrifuge to obtain a mixed solution I; S2, adding 1L of 20wt% sodium carbonate aqueous solution to the mixed solution I, extracting at 80°C for 3h, adding 5mol / L HCl to adjust the pH to 6, and obtaining a mixed solution II after centrifugation; S3. Concentrate the mixed solution II to one fifth of its original volume, add 3 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 20:1, precipitate at -5°C for 5 h, filter and dry the precipitate to obtain 360.5 g of Tremella polysaccharide with a purity of 96.8% and a yield of 34.9%.

[0023] Example 3 The only difference between this embodiment and embodiment 1 is that in step S3, the volume ratio of ethanol to 1-propoxy-2-propanol is 1:9.

[0024] Results: 374.7 g of Tremella polysaccharide was obtained with a purity of 96.6% and a yield of 36.2%.

[0025] Example 4 The only difference between this embodiment and embodiment 1 is that in step S3, the volume ratio of ethanol to 1-propoxy-2-propanol is 9:1.

[0026] Results: 381.5 g of Tremella polysaccharide was obtained with a purity of 96.2% and a yield of 36.7%.

[0027] Example 5 The only difference between this embodiment and embodiment 1 is that in step S3, the volume ratio of ethanol to 1-propoxy-2-propanol is 1:1.

[0028] Results: 379.0 g of Tremella polysaccharide was obtained with a purity of 96.3% and a yield of 36.5%.

[0029] Example 6 The present embodiment is different from the embodiment 3 only in that, in step S3, the mixed solution II is concentrated to one fifth of the original volume, 1.5 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 9:1 is added, and the mixture is precipitated at -10°C for 1 hour, and then 1.5 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 1:9 is added, and the mixture is precipitated again at -10°C for 1 hour. The precipitate is filtered and dried to obtain 387.7 g of Tremella polysaccharide with a purity of 97.5% and a yield of 37.8%.

[0030] Example 7 The present embodiment is different from the embodiment 3 only in that, in step S3, the mixed solution II is concentrated to one fifth of the original volume, 1.5 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 1:9 is added, and the mixture is precipitated at -10°C for 1 hour, and then 1.5 L of a mixed solution of ethanol and 1-propoxy-2-propanol in a volume ratio of 9:1 is added, and the mixture is precipitated again at -10°C for 1 hour. The precipitate is filtered and dried to obtain 391.2 g of Tremella polysaccharide with a purity of 97.9% and a yield of 38.3%.

[0031] Example 8 The only difference between this embodiment and embodiment 7 is that in step S1, the solvent is obtained by mixing 80 parts of water, 1 part of sodium lauryl sulfate, and 3 parts of polyoxyethylene ether.

[0032] Results: 415.1 g of Tremella polysaccharide was obtained with a purity of 97.8% and a yield of 40.6%.

[0033] Example 9 The difference between this embodiment and embodiment 7 is that in step S1, the solvent is obtained by mixing 90 parts of water, 3 parts of sodium lauryl sulfate, and 8 parts of polyoxyethylene ether.

[0034] Results: 416.9 g of Tremella polysaccharide was obtained with a purity of 98.1% and a yield of 40.9%.

[0035] Comparative Example 1 The only difference between this comparative example and Example 1 is that in step S3, 1-propoxy-2-propanol is replaced by an equal amount of ethanol.

[0036] Results: 303.8 g of Tremella polysaccharide was obtained with a purity of 92.5% and a yield of 28.1%.

[0037] Comparative Example 2 The only difference between this comparative example and Example 1 is that in step S3, ethanol is replaced by an equal amount of 1-propoxy-2-propanol.

[0038] Results: 320.6 g of Tremella polysaccharide was obtained with a purity of 91.4% and a yield of 29.3%.

[0039] Comparative Example 3 The only difference between this comparative example and Example 1 is that in step S3, 1-propoxy-2-propanol is replaced by an equal amount of isopropanol.

[0040] Results: 324.1 g of Tremella polysaccharide was obtained with a purity of 93.8% and a yield of 30.4%.

[0041] Compared with Comparative Examples 1 to 3, the solvent for precipitation in Example 1 consists of ethanol and 1-propoxy-2-propanol. As a result, the yield and purity of Tremella polysaccharide prepared in Example 1 are higher than those in Comparative Examples 1 to 3, indicating that adding a mixed solvent consisting of ethanol and 1-propoxy-2-propanol for precipitation can improve the yield and purity of Tremella polysaccharide.

[0042] Compared with Example 1, the volume ratio of ethanol and 1-propoxy-2-propanol was changed in Examples 3 to 5. As a result, the yield and purity of Tremella polysaccharide obtained in Examples 3 to 5 were higher than those in Example 1, indicating that when the volume ratio of ethanol and 1-propoxy-2-propanol was 1:9 to 9:1, the yield and purity of Tremella polysaccharide could be further improved.

[0043] Compared with Example 3, two precipitations were performed in Examples 6 and 7, and the yield and purity of the Tremella polysaccharide obtained in Examples 6 and 7 were higher than those in Example 3, indicating that performing two precipitations can further improve the yield and purity of Tremella polysaccharide; comparing Example 6 and Example 7, it was found that the yield and purity of Tremella polysaccharide in Example 7 were higher than those in Example 6, indicating that when the volume ratio of ethanol and 1-propoxy-2-propanol in the solvent of the first precipitation was 1:9 and the volume ratio of ethanol and 1-propoxy-2-propanol in the solvent of the second precipitation was 9:1, the yield and purity of Tremella polysaccharide can be further improved.

[0044] Compared with Example 7, the composition of the solvent in pulping was changed in Examples 8-9. As a result, the yield of Tremella polysaccharide obtained in Examples 8-9 was higher than that in Example 7, indicating that when the pulping solvent is composed of water, sodium dodecyl sulfate and polyoxyethylene ether, the yield of Tremella polysaccharide can be further improved.

[0045] The Tremella polysaccharide obtained in Example 9 was used as a sample. 5 g of Tremella polysaccharide was weighed and added to 10 g of ethanol (75%) for dilution and mixing. The mixture was then sprayed on the shredded tobacco with a micro-sprayer at an amount of 0.1% by weight of the shredded tobacco. After the cigarettes were made, they were subjected to sensory evaluation and smoking appraisal by professional smoking evaluation committee members. The cigarettes without Tremella polysaccharide were used as the blank control group. The evaluation method was based on the national standard GB5606.4-2005 "Cigarettes Part 4: Sensory Technical Requirements". The evaluation criteria and evaluation scoring results are shown in Tables 1-2: Table 1 Cigarette sensory quality evaluation criteria

[0046] Table 2 Cigarette smoking sensory evaluation scoring results

[0047] Evaluation results: Example 9 has a rich and delicate aroma, good harmony with the tobacco flavor, no impurities, no irritation, and a pure aftertaste; Control group: The aroma is faint and rough, with a slightly mixed smell and is irritating.

[0048] The smoking evaluation results show that adding the Tremella polysaccharide prepared by the present invention to shredded tobacco can improve the impurities generated in the smoke and the stimulation to the throat to a certain extent, has good harmony with the taste of the smoke, and improves the aroma of the smoke.

[0049] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting Tremella polysaccharide, characterized in that: The following steps are involved: S1, freezing and thawing Tremella fuciformis, adding a solvent to pulp, and centrifuging to obtain a mixed solution I; S2, adding alkali solution to the mixed solution I for alkali extraction, adjusting the acidity, and centrifuging to obtain a mixed solution II; S3, concentrating, precipitating, filtering and drying the mixed solution II to obtain Tremella polysaccharide; The precipitated solvent includes ethanol and 1-propoxy-2-propanol; the volume ratio of the ethanol to the 1-propoxy-2-propanol is 1:20 to 20:

1.

2. The method for extracting Tremella polysaccharide according to claim 1, wherein The volume ratio of the ethanol to the 1-propoxy-2-propanol is 1:9 to 9:

1.

3. The method for extracting Tremella polysaccharide according to claim 1, characterized in that: In step S3, the mixed solution II is concentrated, precipitated for the first time, precipitated for the second time, filtered, and dried to obtain Tremella polysaccharide.

4. The method for extracting Tremella polysaccharide according to claim 3, characterized in that: The volume ratios of ethanol and 1-propoxy-2-propanol in the solvent of the first precipitation and the solvent of the second precipitation are different.

5. The method for extracting Tremella polysaccharide according to claim 4, characterized in that: The volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the first precipitation is 1:9; the volume ratio of ethanol to 1-propoxy-2-propanol in the solvent of the second precipitation is 9:

1.

6. The method for extracting Tremella polysaccharide according to claim 1, characterized in that: In step S1, the solvent includes 80-90 parts of water, 1-3 parts of sodium lauryl sulfate, and 3-8 parts of polyoxyethylene ether.

7. The method for extracting Tremella polysaccharide according to claim 1, characterized in that: In step S2, the alkali solution is a 20wt% sodium carbonate aqueous solution; the acid adjustment reagent is 5mol / L HCl; and the acid is adjusted to a pH value of 5-6.

8. The method for extracting Tremella polysaccharide according to claim 1, characterized in that: In step S2, the temperature of the alkali extraction is 70-80° C., and the time of the alkali extraction is 3-5 hours.

9. The method for extracting Tremella polysaccharide according to claim 1, characterized in that: In step S3, the precipitation temperature is -10 to -5°C, and the precipitation time is 2 to 5 hours.

10. Use of the Tremella polysaccharide prepared by the Tremella polysaccharide extraction method according to any one of claims 1 to 9 in tobacco.

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