CN114685691B - Low-temperature preparation method of lentinan polysaccharide powder - Google Patents
Low-temperature preparation method of lentinan polysaccharide powder Download PDFInfo
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- CN114685691B CN114685691B CN202210411868.5A CN202210411868A CN114685691B CN 114685691 B CN114685691 B CN 114685691B CN 202210411868 A CN202210411868 A CN 202210411868A CN 114685691 B CN114685691 B CN 114685691B
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- 229920001491 Lentinan Polymers 0.000 title claims abstract description 72
- 229940115286 lentinan Drugs 0.000 title claims abstract description 72
- 239000000843 powder Substances 0.000 title claims abstract description 51
- 150000004676 glycans Chemical class 0.000 title claims abstract description 34
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 34
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001694 spray drying Methods 0.000 claims abstract description 26
- 239000000706 filtrate Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000001715 Lentinula edodes Nutrition 0.000 claims abstract description 10
- 240000000599 Lentinula edodes Species 0.000 claims abstract description 10
- 238000002386 leaching Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 1
- 241000233866 Fungi Species 0.000 abstract description 2
- 230000005714 functional activity Effects 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 238000002390 rotary evaporation Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000004071 biological effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 208000036142 Viral infection Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000009098 adjuvant therapy Methods 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003544 deproteinization Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- 239000005417 food ingredient Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009385 viral infection Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Sustainable Development (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention provides a low-temperature preparation method of lentinan polysaccharide powder, and belongs to the technical field of edible fungus deep processing. The invention comprises the following steps: (1) Slicing Lentinus Edodes, leaching lentinan with hot water, and filtering to obtain filtrate; (2) concentrating the filtrate in vacuo; and (3) spray drying the concentrated solution at low temperature to obtain lentinan powder. The invention can obtain the functional component lentinan polysaccharide powder with a natural structure, and the preparation method is quick, simple and convenient, has dry inner wall and no wall sticking, can effectively retain the functional activity of lentinan, and has dry, fluffy and fine powder.
Description
Technical Field
The invention belongs to the technical field of edible fungus deep processing, and particularly relates to a low-temperature preparation method of lentinan polysaccharide powder.
Background
Lentinan has various biological activities including antitumor effect, immunity enhancing and antioxidant effect, has been used as injection and tablet for adjuvant treatment of malignant tumor and viral infection in the medical field, and has been developed and utilized later as a functional food ingredient in the food field. In addition, the structure and activity of lentinan can be affected and changed by external factors such as high temperature, organic reagents, acids and bases.
The lentinan is obtained by a hot water extraction method at present, namely, the lentinan is crushed and then extracted by hot water at 80-100 ℃, the extracting solution is concentrated in vacuum, ethanol with the volume of 1.5-3 times is added into the concentrated solution for standing, and then the lentinan is centrifugated to obtain a lentinan precipitate, and the lentinan precipitate is dried by hot air or frozen to obtain a lentinan product. The method consumes a large amount of ethanol, and has high preparation cost, complex procedure and large energy consumption.
The spray drying technology can be applied to the preparation of lentinan, namely, the lentinan is obtained by directly spray drying lentinan after the lentinan leaching solution is concentrated. The method is simple, convenient and quick, however, the air inlet temperature of the existing spray drying is generally higher. High temperature air consumes a lot of energy and high temperature is detrimental to lentinan structure and activity. The invention provides a low-temperature spray drying technology for lentinan, which controls the spray drying temperature to be less than 60 ℃ from leaching, is simple, convenient and quick, is beneficial to keeping the natural structure and activity of lentinan, and has low energy consumption for heating air.
Disclosure of Invention
The invention provides a low-temperature preparation method of lentinan polysaccharide powder, which comprises the following steps:
(1) Slicing Lentinus Edodes, and mixing with the materials according to a feed liquid ratio of 1: leaching the mixture with hot water at 60 ℃ for 2-3 times, each time for 3 hours, filtering, and collecting and combining filtrate;
(2) Rotary evaporation and vacuum concentration are carried out on the filtrate at the temperature of 60 ℃ until the solid content is about 10%;
(3) The inlet temperature of the spray dryer is 40-50 ℃, the air quantity is 90m 3/h, the liquid inlet quantity is 200 ml/h, and the concentrated solution is spray-dried to obtain the lentinan polysaccharide powder.
Preferably, the thickness of the mushroom slices in the step (1) is controlled within 1 mm.
Further, the filtration in the step (1) is 300 mesh nylon filter mesh bag filtration.
Further, the vacuum concentration in the step (2) has a vacuum degree of 0.085-0.1 MPa.
Further, the inlet temperature in the step (3) is 40-50 ℃, and the corresponding outlet temperatures are respectively: the inlet temperature of 40 ℃ corresponds to the outlet temperature of 33+/-1 ℃, and the inlet temperature of 50 ℃ corresponds to the outlet temperature of 41+/-1 ℃.
Further, the lentinan powder in the step (3) has the characteristics of dryness, fluffiness and fineness.
Further, the lentinan powder obtained in the step (3) has a yield of 50% -60%, a moisture content of 5% -6%, a polysaccharide content of 25% -29%, a solubility of >90% and a hygroscopicity of 26% -28%.
The invention has the advantages that: the lentinus edodes slices are cut, fine powder particles are not generated, the impurities are few, and solid-liquid separation is facilitated; the lentinan powder is obtained by directly applying a spray drying technology after the extracting solution is concentrated, the process flow is simple, and the operation is easy; the ethanol precipitation is avoided, and lentinan with good powder characteristics can be obtained without freeze drying; the whole preparation process of the lentinan polysaccharide powder is controlled within 60 ℃, the lentinan polysaccharide powder does not undergo a high-temperature process, and the biological activity of the lentinan polysaccharide powder serving as a functional component can be completely reserved; the lentinan is not deproteinized, exists in natural form, and is added as a functional ingredient of food, and the crude polysaccharide is obtained. In addition, researches show that deproteinization is unfavorable for the activity of lentinan, so that the lentinan prepared by the method has the advantages of undamaged structure and good activity.
Description of the embodiments
The following specific examples are set forth to illustrate the invention but are not to be construed as limiting the invention.
Example 1
The dried lentinus edodes is cut into slices with the thickness of less than 1 mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 50 ℃, the air quantity of a fan is 90 m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 5.51%, the yield of lentinan is 52.30%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
Example 2
The dried lentinus edodes is cut into slices with the thickness of less than 1 mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 40 ℃, the air quantity of a fan is 90 m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 5.74%, the yield of the lentinan is 50.33%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
Example 3: high temperature control group 1
The dried lentinus edodes is cut into slices with the thickness of less than 1mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 100 ℃, the air quantity of a fan is 90m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 4.65%, the yield of the lentinan is 68.27%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
Example 4: high temperature control group 2
The dried lentinus edodes is cut into slices with the thickness of less than 1 mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 120 ℃, the air quantity of a fan is 90 m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 4.2%, the yield of lentinan is 70.73%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
Example 5: high temperature control group 3
The dried lentinus edodes is cut into slices with the thickness of less than 1mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 160 ℃, the air quantity of a fan is 90m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 3.08%, the yield of the lentinan is 73.58%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
Example 6: high temperature control group 4
The dried lentinus edodes is cut into slices with the thickness of less than 1mm, lentinan is extracted by hot water at the temperature of 60 ℃, the feed liquid ratio is 1:20, the extraction is carried out for 3 hours, a 300-mesh filter screen bag is used for filtering to obtain filtrate, the extraction is carried out twice, and the filtrates are combined. The filtrate was concentrated by rotary evaporation to about 10% solids. Spray drying the concentrated solution, wherein the inlet temperature of a spray dryer is 200 ℃, the air quantity of a fan is 90m 3/h, the feeding quantity is 200 ml/h, and the lentinan polysaccharide powder is obtained in a collecting bottle after the spray drying is finished. Through tests, the moisture content of the lentinan powder is 2.37%, the yield of lentinan is 66.92%, the polysaccharide content is 25% -29%, the solubility is >90%, and the hygroscopicity of the lentinan powder is 26% -28%.
The invention carries out spray drying on the inlet temperature in the range of 40-200 ℃, wherein the air quantity of a fan is 90m 3/h, and the feeding quantity is 200 ml/h. The outlet temperatures corresponding to the respective inlet temperatures of the spray-drying are shown in Table 1 for the characteristics of the polysaccharide powder obtained.
TABLE 1
The powder characteristics were measured as follows: determining polysaccharide yield, namely dissolving lentinan powder obtained by spray drying at 200 ℃ serving as a raw material, spray drying at different temperatures to obtain powder, and calculating polysaccharide yield at different temperatures; measuring the moisture content, taking 1g of powder sample, drying at 105 ℃ to constant weight, and calculating the moisture content of the powder; the polysaccharide content is determined by a phenol-sulfuric acid method; the solubility measuring method comprises collecting 1g polysaccharide powder, placing in 100 mL distilled water, magnetically stirring for 5 min, centrifuging at 3000×g for 5 min, collecting supernatant 25 mL, drying at 105deg.C to constant weight, and calculating powder solubility; hygroscopicity was measured by taking 1g powder and placing it in a saturated NaCl solution (75% RH) environment and storing it at room temperature until it was constant, and calculating the hygroscopicity of the powder.
Claims (4)
1. The low-temperature preparation method of the lentinan polysaccharide powder is characterized by comprising the following steps of:
(1) The lentinus edodes slices with the thickness of 1mm are cut according to the feed liquid ratio of 1: leaching 20 with hot water at 60 ℃ for 2-3 times, each time for 3 hours, filtering with 300 mesh nylon filter bags to obtain filtrate, and collecting and combining the filtrate;
(2) Rotary evaporating the filtrate at 60deg.C, and vacuum concentrating until the solid content is about 10%;
(3) And setting the inlet temperature of the spray dryer to be 40-50 ℃, starting feeding after the inlet temperature and the outlet temperature of the equipment are stable, and spray-drying the concentrated solution to obtain the lentinan polysaccharide powder.
2. The low-temperature preparation method of lentinan polysaccharide powder according to claim 1, wherein the spray-drying inlet temperature in the step (3) is set to 40-50 ℃, and the corresponding outlet temperatures are respectively: the inlet temperature of 40 ℃ corresponds to the outlet temperature of 33+/-1 ℃, and the inlet temperature of 50 ℃ corresponds to the outlet temperature of 41+/-1 ℃.
3. The method for preparing lentinan polysaccharide powder at low temperature according to claim 1, wherein the fan air volume of the spray drying in the step (3) is 90 m 3/h, and the feeding amount is 200 ml/h.
4. The low-temperature preparation method of lentinan powder according to claim 1, wherein the lentinan powder in the step (3) has a yield of 50% -60%, a moisture content of 5% -6%, a polysaccharide content of 25% -29%, a solubility of >90% and a hygroscopicity of 26% -28%.
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Citations (7)
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CN1872991A (en) * | 2005-06-01 | 2006-12-06 | 主典兴业股份有限公司 | Spray drying method in low temperature for producing matters of containing biological activities |
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