CN114163548A - Production process of yeast glucan - Google Patents
Production process of yeast glucan Download PDFInfo
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- CN114163548A CN114163548A CN202111529089.7A CN202111529089A CN114163548A CN 114163548 A CN114163548 A CN 114163548A CN 202111529089 A CN202111529089 A CN 202111529089A CN 114163548 A CN114163548 A CN 114163548A
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- 229920001503 Glucan Polymers 0.000 title claims abstract description 88
- 240000004808 Saccharomyces cerevisiae Species 0.000 title claims abstract description 88
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 70
- 229940070527 tourmaline Drugs 0.000 claims abstract description 64
- 229910052613 tourmaline Inorganic materials 0.000 claims abstract description 64
- 239000011032 tourmaline Substances 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 59
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 238000010438 heat treatment Methods 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012153 distilled water Substances 0.000 claims abstract description 28
- 239000000725 suspension Substances 0.000 claims abstract description 28
- PSLIMVZEAPALCD-UHFFFAOYSA-N ethanol;ethoxyethane Chemical compound CCO.CCOCC PSLIMVZEAPALCD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 20
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims abstract description 19
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 19
- 238000010992 reflux Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 238000007885 magnetic separation Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 13
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 4
- 238000000605 extraction Methods 0.000 abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 238000000498 ball milling Methods 0.000 description 26
- 229960002089 ferrous chloride Drugs 0.000 description 15
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000012298 atmosphere Substances 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 238000005245 sintering Methods 0.000 description 12
- 238000002386 leaching Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 239000002002 slurry Substances 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical group O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 5
- 238000007664 blowing Methods 0.000 description 4
- 238000010411 cooking Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 210000005253 yeast cell Anatomy 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000011218 segmentation Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- -1 yeast cells Substances 0.000 description 2
- 241001327634 Agaricus blazei Species 0.000 description 1
- 244000075850 Avena orientalis Species 0.000 description 1
- 235000007319 Avena orientalis Nutrition 0.000 description 1
- 229920002498 Beta-glucan Polymers 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000222336 Ganoderma Species 0.000 description 1
- 240000000599 Lentinula edodes Species 0.000 description 1
- 235000001715 Lentinula edodes Nutrition 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 235000013406 prebiotics Nutrition 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002137 ultrasound 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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
-
- 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)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the field of yeast glucan, and particularly relates to a production process of yeast glucan, which comprises the following steps: step 1, adding yeast glucan into distilled water, stirring uniformly, then adding high-substituted hydroxypropyl cellulose, and carrying out temperature cycle treatment to obtain a homogeneous suspension; step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, uniformly stirring, heating and uniformly stirring to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 8-9, carrying out microwave reaction for 2-4h, washing with water and centrifuging to obtain insoluble substances; step 3, adding the insoluble substances into distilled water, uniformly stirring, sealing and carrying out microwave treatment for 30-60min, and carrying out magnetic separation to obtain yeast glucan precursor powder; and 4, placing the yeast glucan precursor powder into the ethanol ethyl ether solution for low-temperature microwave reaction for 30-60min, sealing, heating up, refluxing for 1-2h, filtering and drying to obtain the yeast glucan. The method provided by the invention is simple, the extraction efficiency is high, and the purity of the obtained product is high.
Description
Technical Field
The invention belongs to the field of yeast glucan, and particularly relates to a production process of yeast glucan.
Background
Yeast glucan, yeast-beta glucan, also known as dextran, is a natural prebiotic widely distributed in fungal, bacterial and plant cell walls, such as American Agaricus blazei, Lentinus edodes, Ganoderma, oats, and the like. Not only can play a plurality of biological activities in various organisms, but also plays an important role in the interaction among various organisms, and is a main functional component playing a health care role. Based on the effects of resisting tumor and radiation, reducing blood fat and cholesterol, regulating blood sugar, preventing cardiovascular diseases, repairing cells, improving intestinal tracts and the like of yeast glucan, the yeast glucan can be used as a high-efficiency biological reaction regulating factor and is a research hotspot at present.
The current preparation method of yeast glucan mainly comprises acid extraction, alkaline extraction, acid-base combined extraction, organic solvent extraction, ultrasonic extraction, enzymatic extraction and the like. The physical method mainly comprising the acid-alkali leaching, the alkaline leaching and the acid-alkali combined leaching has large acid-alkali demand, so that the equipment requirement is improved, and the cost requirement is greatly improved; the chemical method mainly using organic solvent extraction requires the use of a large amount of organic solvent, which causes difficulty in recovery and environmental pollution.
In order to solve the above problems, the market needs to develop a green and environment-friendly production process of yeast glucan.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a production process of yeast glucan, which solves the defects of the prior art, utilizes high-substituted hydroxypropyl cellulose to perform regionalized gel segmentation of yeast cells, and is matched with the ternary synergistic effect of electrolyte, tourmaline catalysis and microwave in a gel region, so that the leaching efficiency is greatly improved, and meanwhile, the clean cooking leaching of tourmaline catalysis matched with microwave is utilized to achieve secondary extraction, so that the yield of the yeast glucan is greatly improved.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a production process of yeast glucan comprises the following steps:
step 1, putting yeast glucan into distilled water, stirring uniformly, adding high-substituted hydroxypropyl cellulose, and performing temperature cycle treatment to obtain a homogeneous suspension, wherein the concentration of the yeast glucan in the distilled water is 100-200g/L, the concentration of the high-substituted hydroxypropyl cellulose in the distilled water is 10-20g/L, the temperature cycle is that the temperature is increased from 20 ℃ to 80 ℃, then is reduced to 20 ℃, and the temperature is repeatedly increased and reduced in such a way, and the rate of temperature change is 2-4 ℃/min; the step is that the yeast glucan is put into distilled water to be uniformly stirred at the speed of 1000-2000r/min, and the high-substituted hydroxypropyl cellulose ensures that the yeast glucan suspension is continuously converted between a dissolving solution and gel under the temperature circulation, thereby achieving the effect of uniform dispersion and obtaining a homogeneous suspension;
step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, stirring uniformly, heating and stirring uniformly to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 8-9, carrying out microwave reaction for 2-4h, washing and centrifuging to obtain insoluble substances, wherein the texture wall separating agent adopts sodium chloride, the addition amount of the sodium chloride is 1-2% of the mass of the yeast glucan, the tourmaline-based magnetic body is a tourmaline-iron tetroxide complex, the addition amount of the tourmaline-based magnetic body is 3-7% of the mass of the yeast glucan, the stirring speed is 200r/min, the stirring temperature is 10-20 ℃, the temperature of heating and stirring is increased from 20 ℃ to 70 ℃, the alkali liquor adopts sodium hydroxide solution, the concentration is 1-2mol/L, and the dropwise adding speed is 1-3mL/min, the dropping temperature is 10-20 ℃, the microwave reaction adopts a stirring microwave system, the temperature of the microwave reaction is increased to 80 ℃, the temperature rising speed is 2-5 ℃/min, the stirring speed is 500-; in the step, based on a heating and stirring mode, the texture wall separating agent and the tourmaline-based magnetic body are uniformly dispersed into a homogeneous suspension, and along with the temperature rise and the self dispersion characteristic of the hydroxypropyl cellulose, the tourmaline-based magnetic body is uniformly dispersed into the high-substituted hydroxypropyl cellulose; along with the parallel of microwave and stirring in an alkaline environment, the whole system is gradually converted into gelation along with the reduction of the stirring speed and the increase of the microwave temperature, namely, sodium chloride, yeast cells, tourmaline-based magnetic bodies and sodium hydroxide are uniformly distributed in a unit area, the negative ion characteristics of tourmaline and a conductor of ferroferric oxide form a conductive negative ion system of a composite system, a large amount of negative ions generated by the system form efficient active oxygen free radicals under the microwave treatment, cell walls are quickly opened, internal substances are released, meanwhile, more hydroxyl radicals are generated under the alkaline condition, and the negative ions and the microwave are quickly converted into a free radical structure only under the action of the negative ions and the microwave, so that the effect of efficient extraction is achieved. Meanwhile, sodium chloride forms a low-concentration electrolyte system, so that the negative ion system of the tourmaline can be transmitted outwards, and a micro-electrolysis system is effectively formed; the tourmaline-based magnetic body is a ferroferric oxide coated tourmaline complex, the complex not only ensures the generation and conduction of negative ions, but also takes ferroferric oxide as a conductor, and simultaneously, the magnetic charge attraction property is realized, and at the moment, the negative ions and electrolyte form a local enrichment set, thereby realizing the promotion effect in a small range; further, the method for producing the tourmaline-based magnetic body includes: 1, adding tourmaline powder into the ethanol-ether mixed solution, stirring uniformly to form a suspension, adding ferrous chloride, and continuously stirring until the mixture is completely dissolved to obtain a mixed suspension, wherein the volume ratio of ethanol to ether in the ethanol-ether mixed solution is 2:3-5, the concentration of tourmaline in the mixed solution is 140g/L, and the adding amount of the ferrous chloride is 20-30% of the mass of the tourmaline powder; in the mixed suspension, ferrous chloride is dissolved in ethanol to form a stable solution state, and the dissolution characteristic of tourmaline powder can ensure that the tourmaline powder is kept in a good precipitation state; a2, placing the mixed suspension into a sealed ball mill for ball milling at low temperature for 10-20min, then heating and ball milling for 2-4h, relieving pressure and cooling to obtain fine powder slurry; the temperature of the low-temperature ball milling treatment is 5-10 ℃, the ball milling pressure is 0.7-0.9MPa, the temperature of the heating ball milling treatment is 50-70 ℃, the ball milling pressure is 1.2-1.4MPa, and based on the condition that ether is converted into gas under the temperature condition in the heating ball milling process, the solution of the whole system is converted into the ethanol solution of the ferrous chloride, therefore, the fine powder slurry after the ball milling treatment takes tourmaline powder as precipitation fine powder, takes the ferrous chloride as solute and takes the ethanol as solution; a3, heating and filtering the fine powder slurry, drying to obtain a precipitate, standing the precipitate in a reaction kettle for reacting for 1-3 hours at a constant temperature, and blowing to obtain precursor fine powder; the temperature of the heating filtration is 40-60 ℃, during the heating filtration, the self pyroelectricity of the tourmaline powder can release negative ions to attract ferrous ions in the solution and form surface adsorption, so that the ferrous ions form a liquid film on the surface of the tourmaline powder during the filtration; the drying temperature is 80-90 ℃, the atmosphere of the reaction kettle is a mixed system of ammonia gas, water vapor and nitrogen gas, the volume ratio of the ammonia gas to the water vapor to the nitrogen gas is 2:2:6-9, the temperature of the constant-temperature reaction is 90-100 ℃, under the temperature condition, ferrous chloride has water absorption characteristic and can absorb water vapor molecules containing ammonia molecules, so that the conversion of ferrous hydroxide is achieved, and based on the absorption of tourmaline powder negative ions under the temperature condition, the ferrous hydroxide is absorbed on the surface of the tourmaline powder; the purging adopts 100-120 ℃ nitrogen; 4, putting the precursor fine powder into a reaction kettle, introducing oxygen for reacting for 1-2 hours at constant temperature, heating and sintering for 30-50 minutes to obtain the tourmaline fine powder covered by ferroferric oxide, wherein the atmosphere of the reaction kettle is a nitrogen atmosphere, the introduction speed of the oxygen is 5-10mL/min, the temperature is 70-100 ℃, the volume ratio of the nitrogen to the oxygen and the water vapor in the heating and sintering atmosphere is 5:2:1, the sintering temperature is 100-.
Step 3, adding insoluble substances into distilled water, stirring uniformly, sealing and carrying out microwave treatment for 30-60min, obtaining yeast glucan precursor powder after magnetic separation, wherein the concentration of the insoluble substances in the distilled water is 140g/L (100-, thereby improving the extraction rate of the whole yeast glucan;
step 4, placing yeast glucan precursor powder into ethanol ethyl ether liquid for low-temperature microwave reaction for 30-60min, sealing, heating and refluxing for 1-2h, filtering and drying to obtain yeast glucan, wherein the volume ratio of ethanol to ether in the ethanol ethyl ether liquid is 5:2-3, the concentration of the yeast glucan precursor powder in the ethanol ethyl ether liquid is 30-80g/L, the temperature of the low-temperature microwave reaction is 10-20 ℃, the microwave power is 300-plus-one-500W, the temperature of the sealing, heating and refluxing is 50-60 ℃, the temperature of the top of a reflux pipe is 2-10 ℃, and the drying temperature is 100-plus-120 ℃; the method comprises the following steps of opening yeast glucan molecules temporarily by using the dissolution characteristic of ethanol ether solution and the high-frequency osmosis of microwave reaction, and primarily removing impurities; in the sealed heating reflux treatment process, the temperature causes ether to be converted into steam, the effect of internal pressurization is achieved, and meanwhile the temperature is increased to achieve a certain cooking effect on the yeast glucan, so that the effect of further releasing internal impurities is achieved, and the high-purity yeast glucan is obtained.
From the above description, it can be seen that the present invention has the following advantages:
1. the method overcomes the defects of the prior art, utilizes the highly-substituted hydroxypropyl cellulose to perform the regionalized gel segmentation of the yeast cells, and is matched with the ternary synergistic effect of electrolyte, tourmaline catalysis and microwave in the gel region, so that the leaching efficiency is greatly improved, and simultaneously, the tourmaline catalysis is matched with the clean cooking and leaching of the microwave to achieve secondary extraction, thereby greatly improving the yield of the yeast glucan.
2. According to the invention, tourmaline powder of a magnetic system is utilized, so that rapid separation can be achieved, and simultaneously, the activity enhancement effect of microwaves is matched, so that the efficiency of converting negative ions into active free radicals is improved, the extraction efficiency is effectively improved, and the process time is reduced.
3. The invention utilizes a regionalized independent reaction system of the high-substituted hydroxypropyl cellulose and the comprehensive permeability of microwave treatment, ensures the uniform speed of reaction without causing gel damage, and ensures that the first leaching effect is better.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A production process of yeast glucan comprises the following steps:
step 1, adding yeast glucan into distilled water, stirring uniformly, adding high-substituted hydroxypropyl cellulose, performing temperature circulation treatment to obtain a homogeneous suspension, wherein the concentration of the yeast glucan in the distilled water is 100g/L, the concentration of the high-substituted hydroxypropyl cellulose in the distilled water is 10g/L, the temperature is increased to 80 ℃ from 20 ℃ in the temperature circulation, then is reduced to 20 ℃, and the temperature is repeatedly increased and reduced in such a way, and the temperature change rate is 2 ℃/min;
step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, uniformly stirring, heating and uniformly stirring to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 8, carrying out microwave reaction for 2 hours, washing and centrifuging to obtain insoluble substances, wherein the texture wall separating agent adopts sodium chloride, the addition amount of the sodium chloride is 1% of the mass of the yeast glucan, the tourmaline-based magnetic body is a tourmaline-iron tetroxide complex, the addition amount of the tourmaline-based magnetic body is 3% of the mass of the yeast glucan, the stirring speed is 100r/min, the stirring temperature is 10 ℃, the temperature of heating and stirring is increased from 20 ℃ to 70 ℃, the alkali liquor adopts sodium hydroxide solution, the concentration is 1mol/L, the dropwise adding speed is 1mL/min, the dropwise adding temperature is 10 ℃, the microwave reaction adopts a stirring microwave system, the temperature of the microwave reaction is raised to 80 ℃, the temperature raising speed is 2 ℃/min, the stirring speed is 500r/min, the stirring speed is gradually reduced, and the stirring descending speed is 50 r/min; the tourmaline-based magnetic body is a ferroferric oxide coated tourmaline complex, and the preparation method of the tourmaline-based magnetic body comprises the following steps: 1, adding tourmaline powder into the ethanol-ether mixed solution, uniformly stirring to form a suspension, adding ferrous chloride, continuously stirring until the ferrous chloride is completely dissolved to obtain a mixed suspension, wherein the volume ratio of ethanol to ether in the ethanol-ether mixed solution is 2:3, the concentration of tourmaline in the mixed solution is 100g/L, and the adding amount of the ferrous chloride is 20% of the mass of the tourmaline powder; a2, placing the mixed suspension into a sealed ball mill for ball milling at low temperature for 10min, then heating and ball milling for 2h, and cooling after pressure relief to obtain fine powder slurry; the temperature of the low-temperature ball milling treatment is 5 ℃, the ball milling pressure is 0.7MPa, the temperature of the heating ball milling treatment is 50 ℃, and the ball milling pressure is 1.2 MPa; a3, heating and filtering the fine powder slurry, drying to obtain a precipitate, standing the precipitate in a reaction kettle for reacting for 1 hour at constant temperature, and blowing to obtain precursor fine powder; the temperature for heating and filtering is 40 ℃; the drying temperature is 80-90 ℃, the atmosphere of the reaction kettle is a mixed system of ammonia gas, water vapor and nitrogen gas, the volume ratio of the ammonia gas, the water vapor and the nitrogen gas is 2:2:6, and the constant temperature reaction temperature is 90 ℃; the purging adopts nitrogen at 100 ℃; 4, putting the precursor fine powder into a reaction kettle, introducing oxygen, reacting for 1 hour at constant temperature, heating and sintering for 30-50 minutes to obtain ferroferric oxide-covered tourmaline fine powder, wherein the atmosphere of the reaction kettle is a nitrogen atmosphere, the introduction speed of the oxygen is 5mL/min, the temperature is 70 ℃, the volume ratio of the nitrogen to the oxygen to the water vapor in the heating and sintering atmosphere is 5:2:1, and the sintering temperature is 100 ℃;
step 3, adding insoluble substances into distilled water, uniformly stirring, sealing and carrying out microwave treatment for 30-60min, and carrying out magnetic separation to obtain yeast glucan precursor powder, wherein the concentration of the insoluble substances in the distilled water is 100g/L, the stirring speed is 1000r/min, the temperature of the microwave treatment is 90 ℃, and the power is 400W;
and 4, placing the yeast glucan precursor powder into ethanol ether liquid for low-temperature microwave reaction for 30min, sealing, heating and refluxing for 1h, filtering and drying to obtain the yeast glucan, wherein the volume ratio of ethanol to ether in the ethanol ether liquid is 5:2, the concentration of the yeast glucan precursor powder in the ethanol ether liquid is 30g/L, the temperature of the low-temperature microwave reaction is 10 ℃, the microwave power is 300W, the temperature of the sealing, heating and refluxing is 50 ℃, the top temperature of a reflux pipe is 2 ℃, and the drying temperature is 100 ℃.
The yeast glucan obtained in this example was a pale yellow powder with a yeast glucan content of 86.1% and a yeast glucan yield of 25.33%.
Example 2
A production process of yeast glucan comprises the following steps:
step 1, adding yeast glucan into distilled water, stirring uniformly, adding high-substituted hydroxypropyl cellulose, performing temperature circulation treatment to obtain a homogeneous suspension, wherein the concentration of the yeast glucan in the distilled water is 200g/L, the concentration of the high-substituted hydroxypropyl cellulose in the distilled water is 20g/L, the temperature circulation is that the temperature is increased from 20 ℃ to 80 ℃, then is reduced to 20 ℃, and the temperature is repeatedly increased and reduced in such a way, and the temperature change rate is 4 ℃/min;
step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, uniformly stirring, heating and uniformly stirring to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 9, carrying out microwave reaction for 4 hours, washing and centrifuging to obtain insoluble substances, wherein the texture wall separating agent adopts sodium chloride, the addition amount of the sodium chloride is 2% of the mass of the yeast glucan, the tourmaline-based magnetic body is a tourmaline-iron tetroxide complex, the addition amount of the tourmaline-based magnetic body is 7% of the mass of the yeast glucan, the stirring speed is 200r/min, the stirring temperature is 20 ℃, the temperature of heating and stirring is increased from 20 ℃ to 70 ℃, the alkali liquor adopts sodium hydroxide solution, the concentration is 2mol/L, the dropwise adding speed is 3mL/min, the dropwise adding temperature is 20 ℃, the microwave reaction adopts a stirring microwave system, the temperature of the microwave reaction is increased to 80 ℃, the temperature rising speed is 5 ℃/min, the stirring speed is 800r/min, the stirring speed is gradually reduced, and the stirring descending speed is 100 r/min; the tourmaline-based magnetic body is a ferroferric oxide coated tourmaline complex, and the preparation method of the tourmaline-based magnetic body comprises the following steps: 1, adding tourmaline powder into the ethanol-ether mixed solution, uniformly stirring to form a suspension, adding ferrous chloride, continuously stirring until the ferrous chloride is completely dissolved to obtain a mixed suspension, wherein the volume ratio of ethanol to ether in the ethanol-ether mixed solution is 2:5, the concentration of tourmaline in the mixed solution is 140g/L, and the adding amount of the ferrous chloride is 30% of the mass of the tourmaline powder; a2, placing the mixed suspension into a sealed ball mill for ball milling at low temperature for 20min, then heating and ball milling for 4h, and cooling after pressure relief to obtain fine powder slurry; the temperature of the low-temperature ball milling treatment is 10 ℃, the ball milling pressure is 0.9MPa, the temperature of the heating ball milling treatment is 70 ℃, and the ball milling pressure is 1.4 MPa; a3, heating and filtering the fine powder slurry, drying to obtain a precipitate, standing the precipitate in a reaction kettle for reacting for 3 hours at a constant temperature, and blowing to obtain precursor fine powder; the temperature for heating and filtering is 60 ℃; the drying temperature is 90 ℃, the atmosphere of the reaction kettle is a mixed system of ammonia gas, water vapor and nitrogen, the volume ratio of the ammonia gas, the water vapor and the nitrogen is 2:2:9, and the temperature of the constant-temperature reaction is 100 ℃; the purging adopts nitrogen at 120 ℃; 4, putting the precursor fine powder into a reaction kettle, introducing oxygen, reacting for 2 hours at constant temperature, heating and sintering for 50 minutes to obtain ferroferric oxide-covered tourmaline fine powder, wherein the atmosphere of the reaction kettle is nitrogen atmosphere, the introduction speed of the oxygen is 10mL/min, the temperature is 100 ℃, the volume ratio of the nitrogen to the oxygen to the water vapor in the heating and sintering atmosphere is 5:2:1, and the sintering temperature is 120 ℃;
step 3, adding insoluble substances into distilled water, stirring uniformly, sealing and carrying out microwave treatment for 60min, and carrying out magnetic separation to obtain yeast glucan precursor powder, wherein the concentration of the insoluble substances in the distilled water is 140g/L, the stirring speed is 2000r/min, the temperature of the microwave treatment is 100 ℃, and the power is 600W;
and 4, placing the yeast glucan precursor powder into ethanol ether liquid for low-temperature microwave reaction for 60min, sealing, heating and refluxing for 2h, filtering and drying to obtain the yeast glucan, wherein the volume ratio of ethanol to ether in the ethanol ether liquid is 5:3, the concentration of the yeast glucan precursor powder in the ethanol ether liquid is 80g/L, the temperature of the low-temperature microwave reaction is 20 ℃, the microwave power is 500W, the temperature of the sealing, heating and refluxing is 60 ℃, the top temperature of a reflux pipe is 10 ℃, and the drying temperature is 120 ℃.
The yeast glucan obtained in this example was a pale yellow powder with a yeast glucan content of 88.9% and a yeast glucan yield of 26.72%.
Example 3
A production process of yeast glucan comprises the following steps:
step 1, adding yeast glucan into distilled water, stirring uniformly, adding high-substituted hydroxypropyl cellulose, performing temperature circulation treatment to obtain a homogeneous suspension, wherein the concentration of the yeast glucan in the distilled water is 150g/L, the concentration of the high-substituted hydroxypropyl cellulose in the distilled water is 15g/L, the temperature is increased to 80 ℃ from 20 ℃ in the temperature circulation, then is reduced to 20 ℃, and the temperature is repeatedly increased and reduced in such a way, and the temperature change rate is 3 ℃/min;
step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, uniformly stirring, heating and uniformly stirring to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 9, carrying out microwave reaction for 3 hours, washing and centrifuging to obtain insoluble substances, wherein the texture wall separating agent adopts sodium chloride, the addition amount of the sodium chloride is 2% of the mass of the yeast glucan, the tourmaline-based magnetic body is a tourmaline-iron tetroxide complex, the addition amount of the tourmaline-based magnetic body is 6% of the mass of the yeast glucan, the stirring speed is 150r/min, the stirring temperature is 15 ℃, the temperature of heating and stirring is increased from 20 ℃ to 70 ℃, the alkali liquor adopts sodium hydroxide solution, the concentration is 2mol/L, the dropwise adding speed is 2mL/min, the dropwise adding temperature is 15 ℃, the microwave reaction adopts a stirring microwave system, the temperature of the microwave reaction is increased to 80 ℃, the temperature rising speed is 4 ℃/min, the stirring speed is 700r/min, the stirring speed is gradually reduced, and the stirring descending speed is 60 r/min; the tourmaline-based magnetic body is a ferroferric oxide coated tourmaline complex, and the preparation method of the tourmaline-based magnetic body comprises the following steps: 1, adding tourmaline powder into the ethanol-ether mixed solution, uniformly stirring to form a suspension, adding ferrous chloride, continuously stirring until the ferrous chloride is completely dissolved to obtain a mixed suspension, wherein the volume ratio of ethanol to ether in the ethanol-ether mixed solution is 2:4, the concentration of tourmaline in the mixed solution is 120g/L, and the adding amount of the ferrous chloride is 25% of the mass of the tourmaline powder; a2, placing the mixed suspension into a sealed ball mill for low-temperature ball milling treatment for 15min, then heating and ball milling for 3h, and cooling after pressure relief to obtain fine powder slurry; the temperature of the low-temperature ball milling treatment is 8 ℃, the ball milling pressure is 0.8MPa, the temperature of the heating ball milling treatment is 60 ℃, and the ball milling pressure is 1.3 MPa; a3, heating and filtering the fine powder slurry, drying to obtain a precipitate, standing the precipitate in a reaction kettle for reacting for 2 hours at a constant temperature, and blowing to obtain precursor fine powder; the temperature for heating and filtering is 50 ℃; the drying temperature is 85 ℃, the atmosphere of the reaction kettle is a mixed system of ammonia gas, water vapor and nitrogen, the volume ratio of the ammonia gas, the water vapor and the nitrogen is 2:2:8, and the temperature of the constant-temperature reaction is 95 ℃; the purging adopts nitrogen at 110 ℃; 4, putting the precursor fine powder into a reaction kettle, introducing oxygen, reacting for 2 hours at constant temperature, heating and sintering for 40 minutes to obtain ferroferric oxide-covered tourmaline fine powder, wherein the atmosphere of the reaction kettle is a nitrogen atmosphere, the introduction speed of the oxygen is 8mL/min, the temperature is 80 ℃, the volume ratio of the nitrogen to the oxygen to the water vapor in the heating and sintering atmosphere is 5:2:1, and the sintering temperature is 110 ℃;
step 3, adding insoluble substances into distilled water, uniformly stirring, sealing and carrying out microwave treatment for 30-60min, and carrying out magnetic separation to obtain yeast glucan precursor powder, wherein the concentration of the insoluble substances in the distilled water is 120g/L, the stirring speed is 1500r/min, the temperature of the microwave treatment is 95 ℃, and the power is 500W;
and 4, placing the yeast glucan precursor powder into ethanol ether liquid for low-temperature microwave reaction for 50min, sealing, heating and refluxing for 2h, filtering and drying to obtain the yeast glucan, wherein the volume ratio of ethanol to ether in the ethanol ether liquid is 5:2, the concentration of the yeast glucan precursor powder in the ethanol ether liquid is 60g/L, the temperature of the low-temperature microwave reaction is 15 ℃, the microwave power is 400W, the temperature of the sealing, heating and refluxing is 55 ℃, the top temperature of a reflux pipe is 8 ℃, and the drying temperature is 110 ℃.
The yeast glucan obtained in this example was a pale yellow powder with a yeast glucan content of 87.3% and a yeast glucan yield of 26.17%.
In summary, the invention has the following advantages:
1. the method overcomes the defects of the prior art, utilizes the highly-substituted hydroxypropyl cellulose to perform the regionalized gel segmentation of the yeast cells, and is matched with the ternary synergistic effect of electrolyte, tourmaline catalysis and microwave in the gel region, so that the leaching efficiency is greatly improved, and simultaneously, the tourmaline catalysis is matched with the clean cooking and leaching of the microwave to achieve secondary extraction, thereby greatly improving the yield of the yeast glucan.
2. According to the invention, tourmaline powder of a magnetic system is utilized, so that rapid separation can be achieved, and simultaneously, the activity enhancement effect of microwaves is matched, so that the efficiency of converting negative ions into active free radicals is improved, the extraction efficiency is effectively improved, and the process time is reduced.
3. The invention utilizes a regionalized independent reaction system of the high-substituted hydroxypropyl cellulose and the comprehensive permeability of microwave treatment, ensures the uniform speed of reaction without causing gel damage, and ensures that the first leaching effect is better.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. A production process of yeast glucan is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding yeast glucan into distilled water, stirring uniformly, then adding high-substituted hydroxypropyl cellulose, and carrying out temperature cycle treatment to obtain a homogeneous suspension;
step 2, adding a texture wall separating agent and a tourmaline-based magnetic body into the homogeneous suspension, uniformly stirring, heating and uniformly stirring to obtain homogeneous gel, slowly dropwise adding alkali liquor until the pH value is 8-9, carrying out microwave reaction for 2-4h, washing with water and centrifuging to obtain insoluble substances;
step 3, adding the insoluble substances into distilled water, uniformly stirring, sealing and carrying out microwave treatment for 30-60min, and carrying out magnetic separation to obtain yeast glucan precursor powder;
and 4, placing the yeast glucan precursor powder into the ethanol ethyl ether solution for low-temperature microwave reaction for 30-60min, sealing, heating up, refluxing for 1-2h, filtering and drying to obtain the yeast glucan.
2. The process for producing yeast glucan according to claim 1, wherein: the concentration of the yeast glucan in the step 1 in the distilled water is 100-200g/L, and the concentration of the highly substituted hydroxypropyl cellulose in the distilled water is 10-20 g/L.
3. The process for producing yeast glucan according to claim 1, wherein: the temperature cycle in the step 1 is that the temperature is increased from 20 ℃ to 80 ℃, then is reduced to 20 ℃, and the temperature is repeatedly increased and reduced in such a way, wherein the rate of temperature change is 2-4 ℃/min.
4. The process for producing yeast glucan according to claim 1, wherein: the plasmolysis separating agent in the step 2 adopts sodium chloride, the addition amount of the sodium chloride is 1-2% of the mass of the yeast glucan, the tourmaline-based magnetic body is a tourmaline-iron tetroxide complex, the addition amount of the tourmaline-based magnetic body is 3-7% of the mass of the yeast glucan, the stirring speed is 100-200r/min, and the stirring temperature is 10-20 ℃.
5. The process for producing yeast glucan according to claim 1, wherein: the temperature of the heating and stirring in the step 2 is increased from 20 ℃ to 70 ℃, the alkali liquor adopts sodium hydroxide solution, the concentration is 1-2mol/L, the dropping speed is 1-3mL/min, and the dropping temperature is 10-20 ℃.
6. The process for producing yeast glucan according to claim 1, wherein: the microwave reaction in the step 2 adopts a stirring microwave system, the temperature of the microwave reaction is increased to 80 ℃, the temperature rising speed is 2-5 ℃/min, the stirring speed is 500-.
7. The process for producing yeast glucan according to claim 1, wherein: the concentration of the insoluble substances in the step 3 in the distilled water is 140g/L, and the stirring speed is 1000-2000 r/min.
8. The process for producing yeast glucan according to claim 1, wherein: the temperature of the microwave treatment in the step 3 is 90-100 ℃, and the power is 400-600W.
9. The process for producing yeast glucan according to claim 1, wherein: in the ethanol ether solution in the step 4, the volume ratio of ethanol to ether is 5:2-3, and the concentration of the yeast glucan precursor powder in the ethanol ether solution is 30-80 g/L.
10. The process for producing yeast glucan according to claim 1, wherein: the temperature of the low-temperature microwave reaction in the step 4 is 10-20 ℃, the microwave power is 300-500W, the temperature of the sealed heating reflux is 50-60 ℃, the temperature of the top of the reflux pipe is 2-10 ℃, and the drying temperature is 100-120 ℃.
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