CN118831347B - Composite ionic liquid and application thereof - Google Patents
Composite ionic liquid and application thereof Download PDFInfo
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- CN118831347B CN118831347B CN202410859411.XA CN202410859411A CN118831347B CN 118831347 B CN118831347 B CN 118831347B CN 202410859411 A CN202410859411 A CN 202410859411A CN 118831347 B CN118831347 B CN 118831347B
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 150000004676 glycans Chemical class 0.000 claims abstract description 101
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 101
- 239000005017 polysaccharide Substances 0.000 claims abstract description 101
- 238000000034 method Methods 0.000 claims abstract description 51
- 241000222640 Polyporus Species 0.000 claims abstract description 48
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000005703 Trimethylamine hydrochloride Substances 0.000 claims abstract description 36
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 56
- 239000000243 solution Substances 0.000 claims description 53
- 239000000706 filtrate Substances 0.000 claims description 35
- 239000011259 mixed solution Substances 0.000 claims description 31
- 244000171085 Polyporus umbellatus Species 0.000 claims description 29
- 235000004837 Polyporus umbellatus Nutrition 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 25
- 239000003153 chemical reaction reagent Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- XIYUIMLQTKODPS-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CC[N+]=1C=CN(C)C=1 XIYUIMLQTKODPS-UHFFFAOYSA-M 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 57
- 238000003809 water extraction Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000012634 fragment Substances 0.000 description 40
- 239000006228 supernatant Substances 0.000 description 40
- 239000002994 raw material Substances 0.000 description 31
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 20
- 238000004108 freeze drying Methods 0.000 description 20
- 238000011084 recovery Methods 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 241000222684 Grifola Species 0.000 description 13
- 230000008569 process Effects 0.000 description 12
- 238000002137 ultrasound extraction Methods 0.000 description 12
- 238000004821 distillation Methods 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 10
- NKLPQNGYXWVELD-UHFFFAOYSA-M coomassie brilliant blue Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=C1 NKLPQNGYXWVELD-UHFFFAOYSA-M 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 10
- 238000007781 pre-processing Methods 0.000 description 10
- 102000004169 proteins and genes Human genes 0.000 description 10
- 108090000623 proteins and genes Proteins 0.000 description 10
- 238000007873 sieving Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 210000004027 cell Anatomy 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- -1 acts Chemical compound 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 4
- 229920002521 macromolecule Polymers 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 3
- 230000007760 free radical scavenging Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- WWFKDEYBOOGHKL-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;bromide Chemical compound Br.CCN1CN(C)C=C1 WWFKDEYBOOGHKL-UHFFFAOYSA-N 0.000 description 2
- QGKOZWJXEMFEOW-UHFFFAOYSA-N CN1CN(C=C1)CC.[N+](=O)(O)[O-] Chemical compound CN1CN(C=C1)CC.[N+](=O)(O)[O-] QGKOZWJXEMFEOW-UHFFFAOYSA-N 0.000 description 2
- 241001558929 Sclerotium <basidiomycota> Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 230000002000 scavenging effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 241001489124 Boletus edulis Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000931143 Gleditsia sinensis Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 241000222341 Polyporaceae Species 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 230000002292 Radical scavenging effect Effects 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000002792 antioxidant assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 206010013990 dysuria Diseases 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000002366 mineral element 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
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Acoustics & Sound (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Mechanical Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to the technical field of polysaccharide extraction, and discloses a composite ionic liquid and application thereof, wherein the composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1-1.5:2-3.5. The compound ionic liquid is used for extracting polyporus polysaccharide. According to the invention, the compound ionic liquid trimethylamine hydrochloride and the 1-ethyl-3-methylimidazole acetate are firstly adopted to extract the polyporus polysaccharide, the extraction rate is 11.94% +/-0.36%, the extraction rate reaches 11.6-12.3 mg/100mg, and the extraction rate is 3-4 times of that of the polyporus polysaccharide by the traditional water extraction method.
Description
Technical Field
The invention belongs to the technical field of polysaccharide extraction, and particularly relates to a composite ionic liquid and application thereof.
Background
Polyporus [ Polyporus umbellatus (Pers.) Fries ] is dry sclerotium of Polyporaceae fungus Polyporus. The Chinese medicinal composition has sweet and light taste, has flat nature, enters kidney and bladder channels, has the effects of promoting diuresis and removing dampness, and is mainly used for treating symptoms such as edema, dysuria, diarrhea, stranguria with turbid urine, leukorrhagia and the like, and mainly contains chemical components such as polysaccharides, amino acids, ketones, mineral elements and the like; polyporus polysaccharide is one of its main bioactive components, and has effects of resisting tumor, regulating immunity, resisting radiation, protecting liver, etc.
The extraction method of polysaccharide mainly comprises water extraction, ultrasonic extraction, microwave extraction and the like, and the extraction process optimization relates to orthogonal design, response surface optimization method, regression orthogonal test design method and the like. For example, in Zhang Xiaoxia ' Zhu Ling polysaccharide extraction process optimization and antioxidant activity research ' published in China traditional Chinese medicine academic periodical ', a solvent method ultrasonic extraction process is adopted to extract Zhu Ling polysaccharide with an extraction rate of 1.773mg/100mg, and in Zheng Yiqi ' J.J.P.A. published in food industry science and technology ' response surface optimization Zhu Ling sclerotium polysaccharide ultrasonic auxiliary extraction process and antioxidant activity analysis ' in Zhang Xiaoxia's published paper, an ultrasonic auxiliary technology is adopted to extract Zhu Ling polysaccharide, and a single factor experiment is combined with a response surface method to optimize and examine the influence of extraction time, ultrasonic power, extraction temperature and liquid-material ratio on polysaccharide yield and determine the optimal extraction process, so that the maximum extraction rate is 2.50mg/100mg. The extraction rate of the polyporus polysaccharide obtained by the method is too low. Therefore, there is an urgent need to develop a substance for improving the extraction rate of polyporus polysaccharide.
Disclosure of Invention
The invention provides a composite ionic liquid and application thereof, and solves the problem that the extraction rate is too low when polyporus polysaccharide is extracted in the prior art.
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1-1.5:2-3.5.
The extraction rate of the polyporus polysaccharide is reduced when the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is too high or too low. At the initial stage of extraction, 1-ethyl-3-methylimidazole acetate mainly acts, but along with the progress of the reaction, the 1-ethyl-3-methylimidazole acetate is difficult to enter cells through cell wall channels of grifola cells, and extraction is difficult to carry out, at the moment, small-molecule trimethylamine hydrochloride starts to act, macromolecule dissolved matters adhered to the outer surfaces of grifola particles are broken under the action of ultrasonic waves, a channel is opened, the macromolecule dissolved matters enter the cells through the cell wall channels of the grifola cells, and polysaccharide is continuously dissolved, so that the extraction rate of the grifola polysaccharide is further improved.
Preferably, the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1-2:3.
The second purpose of the invention is to protect the application of the composite ionic liquid in extracting polyporus polysaccharide.
Preferably, the method for extracting polyporus polysaccharide specifically comprises the following steps:
Adding deionized water into the composite ionic liquid to prepare a composite ionic liquid aqueous solution, wherein the concentration of trimethylamine hydrochloride in the composite ionic liquid aqueous solution is 1.0-1.5 g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 2.0-3.5 g/L;
mixing Polyporus umbellatus powder with composite ionic liquid aqueous solution according to a feed-liquid ratio of 1 g:20-30 mL, adjusting the pH of the mixed solution to 6.5-7.0, heating to 70-75 ℃, carrying out ultrasonic treatment, filtering, and purifying the filtrate to obtain the Polyporus umbellatus polysaccharide.
Preferably, the concentration of trimethylamine hydrochloride in the aqueous solution of the composite ionic liquid is 1.0g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 2.0g/L.
Preferably, the ultrasonic conditions are 50-70 min and 40-80 kHz. The ultrasonic wave is used for promoting trimethylamine hydrochloride molecules to break up macromolecular dissolved matters adhered to the outer surface of the grifola granules.
Preferably, when the pH of the mixture is adjusted, HCl solution or NaOH solution is used.
Preferably, the concentration of the HCl solution or the NaOH solution is 0.1-0.2 mol/L.
Preferably, the purification method comprises the steps of concentrating filtrate to 1/3 of the original volume, adding ethanol to ensure that the volume concentration of the ethanol in the mixed solution is 80%, standing for 6-8 h, and centrifugally filtering to obtain a filter cake which is crude polysaccharide. Ethanol was added to precipitate the crude polysaccharide.
Preferably, the crude polysaccharide is purified by a Sevage reagent to obtain liquid with the protein content less than or equal to 0.49%, and the liquid is frozen and dried to obtain the refined polyporus polysaccharide.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the invention, the compound ionic liquid trimethylamine hydrochloride and the 1-ethyl-3-methylimidazole acetate are adopted for extracting the polyporus polysaccharide for the first time, the extraction rate is 11.94% +/-0.36%, the extraction rate reaches 11.4-12.3 mg/100mg, and the extraction rate is 3-4 times of that of the polysaccharide by the traditional water extraction method.
2. The invention uses trimethylamine hydrochloride as cationic liquid and 1-ethyl-3-methylimidazole acetate as anionic liquid. The method is characterized in that the method is carried out under the condition of a better level of single factor extraction, in the initial stage of the extraction, the Grifola powder is heated at 70-75 ℃ for a shorter time, no Grifola polysaccharide is softened, the Grifola powder is softened gradually along with the progress of the extraction process, other water-soluble components in cells are continuously released, small molecules can be rapidly diffused into an extracting solution, macromolecular substances are attached to the outer surfaces of Grifola particles and adsorb the 1-ethyl-3-methylimidazole acetate, the 1-ethyl-3-methylimidazole acetate is difficult to enter the cells through cell wall pores of Grifola cells, the dissolution rate of Grifola polysaccharide is reduced, and at the moment, the trimethylamine hydrochloride of the small molecules starts to act, is a cation, and has the property of promoting the dissolution of the polysaccharide, and under the hot environment, the trimethylamine hydrochloride molecules break down macromolecular dissolves out substances adhered to the outer surfaces of Grifola particle under the action of the ultrasonic wave, and enter the cells through cell wall channels of Grifola cell, so that the polysaccharide is further extracted by the polysaccharide is further limited by the method.
3. The ionic liquid has the characteristics of good solubility, zero vapor pressure, high stability, low volatility, low melting point, liquid state at normal temperature, wide solubility, good electrical conductivity, good thermal conductivity, environmental protection, stable property and high extraction rate.
4. The refined polysaccharide obtained by the crude polysaccharide extracted by the invention through the purification process is almost consistent with the refined polysaccharide extracted and purified by the traditional water extraction method in the aspect of oxidation resistance research, which shows that the composite ionic liquid adopted by the invention only plays a role in improving the extraction rate in the extraction of the polyporus polysaccharide, and has no influence on the structure and the performance of the polyporus polysaccharide.
Drawings
Fig. 1 is a process flow chart of extracting polyporus polysaccharide by using the composite ionic liquid.
Detailed Description
The following description of the embodiments of the present invention will be made in detail, but not necessarily with reference to the specific embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The methods described in the various embodiments of the present invention, unless otherwise specified, are all conventional. The materials, reagents and the like used, unless otherwise specified, are all commercially available.
The technological flow chart of the compound ionic liquid extraction of the polyporus polysaccharide provided by the embodiment of the invention is shown in figure 1.
Example 1
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1:2.
The extraction method of the polyporus polysaccharide comprises the following steps:
step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, adding deionized water into the composite ionic liquid to prepare a composite ionic liquid aqueous solution serving as an extracting agent, wherein the concentration of trimethylamine hydrochloride is 1.0g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 2.0g/L.
And step 3, weighing 100g of raw material powder, adding a composite ionic liquid extractant according to a ratio of 1g to 20mL, mixing and stirring for 5min, adjusting the pH of the mixed solution to 6.5 by using 0.1mol/L HCl or 0.1mol/LNaOH solution, heating to 70 ℃ and maintaining, and carrying out ultrasonic extraction for 50min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered through a centrifugal filter 1 at the rotating speed of 4000r/min, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution to ensure that the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 6 hours, the stood solution is centrifugally filtered through a centrifugal filter 2 (the centrifugal filters 1 and 2 are designed according to the flow and are defined for the different types, the types are the same) for 15 minutes, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery.
And 4, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 3 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.48mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 5, freeze drying, namely freeze drying the supernatant with the protein content of 0.48mg/100mg obtained in the step4 for 14 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Example 2
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1:3.5.
The extraction method of the polyporus polysaccharide comprises the following steps:
step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, adding deionized water into the composite ionic liquid to prepare a composite ionic liquid aqueous solution serving as an extracting agent, wherein the concentration of trimethylamine hydrochloride is 1.0g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 3.5g/L.
And step 3, weighing 100g of raw material powder, adding a composite ionic liquid extractant according to a ratio of 1g to 25mL, mixing and stirring for 8min, adjusting the pH of the mixed solution to 6.5 by using 0.2mol/L HCl solution, heating to 70 ℃ and maintaining, and carrying out ultrasonic extraction for 50min under the condition of 40 kHz. After the extraction is finished, carrying out centrifugal filtration on the suspension liquid at the rotating speed of 4000r/min through a centrifugal filter 1, concentrating the filtrate under reduced pressure until the filtrate is 1/3 of the liquid filtrate, cooling to normal temperature, adding 95% ethanol into the normal temperature concentrated liquid to ensure that the volume concentration of the ethanol in the mixed liquid is 80%, standing for 6h, carrying out centrifugal filtration on the standing liquid through the centrifugal filter 2 for 15min, obtaining a filter cake which is crude polysaccharide, and conveying the filtrate to a distillation recovery device for recovery. Centrifugal filters 1 and 2 are designed according to a flow scheme, the types of which are the same for the purpose of defining the differences.
And 4, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 3 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.46mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 5, freeze drying, namely freeze drying the supernatant with the protein content of 0.46mg/100mg obtained in the step4 for 14 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Example 3
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1.5:2.
The extraction method of the polyporus polysaccharide comprises the following steps:
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 3cm fragments, putting the fragments into an oven to be dried to constant weight at 90 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, adding deionized water into the composite ionic liquid to prepare a composite ionic liquid aqueous solution serving as an extracting agent, wherein the concentration of trimethylamine hydrochloride is 1.5g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 2.0g/L.
And step 3, weighing 100g of raw material powder, adding a composite ionic liquid extractant according to a ratio of 1g to 30mL, mixing and stirring for 10min, adjusting the pH of the mixed solution to 7.0 by using a 0.2mol/LNaOH solution, heating to 75 ℃ and maintaining, and performing ultrasonic extraction for 60min under the condition of 80 kHz. After the extraction is finished, the suspension is centrifugally filtered through a centrifugal filter 1 at the rotating speed of 4500r/min, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered through the centrifugal filter 2 for 20 minutes, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery. Centrifugal filters 1 and 2 are designed according to a flow scheme, the types of which are the same for the purpose of defining the differences.
And 4, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 3 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.44mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 5, freeze drying, namely freeze drying the supernatant with the protein content of 0.44mg/100mg obtained in the step4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Example 4
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1.5:3.5.
The extraction method of the polyporus polysaccharide comprises the following steps:
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 3cm fragments, putting the fragments into an oven to be dried to constant weight at 90 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, adding deionized water into the composite ionic liquid to prepare a composite ionic liquid aqueous solution serving as an extracting agent, wherein the concentration of trimethylamine hydrochloride is 1.5g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 3.5g/L.
And step 3, weighing 100g of raw material powder, adding a composite ionic liquid extractant according to a ratio of 1g to 30mL, mixing and stirring for 10min, adjusting the pH of the mixed solution to 7.0 by using 0.2mol/L HCl or 0.2mol/LNaOH solution, heating to 75 ℃ and maintaining, and performing ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered through a centrifugal filter 1 at the rotating speed of 4500r/min, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered through the centrifugal filter 2 for 20 minutes, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery. Centrifugal filters 1 and 2 are designed according to a flow scheme, the types of which are the same for the purpose of defining the differences.
And 4, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 3 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.49mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 5, freeze drying, namely freeze drying the supernatant with the protein content of 0.49mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 1
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And step 2, weighing 100g of raw material powder, adding deionized water as an extractant according to a ratio of 1g to 20mL, mixing and stirring for 5min, adjusting the pH of the mixed solution to 7.0 by using a 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and carrying out ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, centrifugally filtering the suspension in a centrifugal filter 1 at the rotating speed of 4500r/min by a centrifugal machine, concentrating the filtrate under reduced pressure, concentrating to 1/3 of the liquid filtrate, cooling to normal temperature, adding 95% ethanol into the normal temperature concentrated solution to ensure that the volume concentration of the ethanol in the mixed solution is 80%, standing for 8 hours, centrifugally filtering the standing solution by a centrifugal filter 2, and obtaining a filter cake which is crude polysaccharide.
And 3, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 4 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.43mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 4, freeze-drying, namely freeze-drying the supernatant with the protein content of 0.43mg/100mg obtained in the step 4 for 14 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 2
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, preparing an ionic liquid solution, namely accurately preparing a solution with the concentration of trimethylamine hydrochloride of 1.5 g/L.
And step 2, weighing 100g of raw material powder, adding trimethylamine hydrochloride ionic liquid solution as an extracting agent according to a ratio of 1g to 30mL, mixing and stirring for 10min, adjusting the pH of the mixed solution to 7.0 by using 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and carrying out ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered in a centrifugal filter 1 at the rotating speed of 4500r/min by a centrifugal machine, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered by a centrifugal filter 2, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery.
And 3, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 4 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.47mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 4, freeze-drying, namely freeze-drying the supernatant with the protein content of 0.47mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 3
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, preparing an ionic liquid solution, namely accurately preparing a solution with the concentration of 1-ethyl-3-methylimidazole acetate of 3.5 g/L.
And step 2, weighing 100g of raw material powder, adding 1-ethyl-3-methylimidazole acetate ionic liquid as an extracting agent according to a ratio of 1g to 30mL, mixing and stirring for 10min, regulating the pH of the mixed solution to 7.0 by using 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and carrying out ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered in a centrifugal filter 1 at the rotating speed of 4500r/min by a centrifugal machine, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered by a centrifugal filter 2, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery.
And 3, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 4 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.48mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 4, freeze drying, namely freeze drying the supernatant with the protein content of 0.48mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 4
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, preparing an ionic liquid solution, namely accurately preparing a solution with the concentration of 1-ethyl-3-methylimidazole bromide salt of 3.5 g/L.
And step 2, weighing 100g of raw material powder, adding 1-ethyl-3-methylimidazole bromide ionic liquid as an extracting agent according to a ratio of 1g to 30mL, mixing and stirring for 10min, regulating the pH of the mixed solution to 7.0 by using 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and carrying out ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered in a centrifugal filter 1 at the rotating speed of 4500r/min by a centrifugal machine, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered by a centrifugal filter 2, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery.
And 3, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 4 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.45mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 4, freeze drying, namely freeze drying the supernatant with the protein content of 0.45mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 5
Step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, preparing an ionic liquid solution, namely accurately preparing a solution with the concentration of 1-ethyl-3-methylimidazole nitrate of 3.5 g/L.
And step 2, weighing 100g of raw material powder, adding 1-ethyl-3-methylimidazole nitrate ionic liquid as an extracting agent according to a ratio of 1g to 30mL, mixing and stirring for 10min, regulating the pH of the mixed solution to 7.0 by using 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and carrying out ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered in a centrifugal filter 1 at the rotating speed of 4500r/min by a centrifugal machine, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered by a centrifugal filter 2, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery.
And 3, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 4 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.42mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 4, freeze-drying, namely freeze-drying the supernatant with the protein content of 0.42mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
Comparative example 6
The composite ionic liquid is a mixture of tetramethyl ammonium chloride and 1-ethyl-3-methylimidazole acetate, and the mass ratio of the tetramethyl ammonium chloride to the 1-ethyl-3-methylimidazole acetate is 1.5:3.5.
The extraction method of the polyporus polysaccharide comprises the following steps:
step 1, preprocessing raw materials, namely cleaning Polyporus umbellatus, cutting the Polyporus umbellatus into 2cm fragments, putting the fragments into an oven to be dried to constant weight at 80 ℃, crushing the fragments, and sieving the crushed fragments with a 60-mesh sieve to obtain raw material powder for later use.
And 2, preparing the composite ionic liquid into a composite ionic liquid solution, wherein the concentration of the tetramethyl ammonium chloride is 1.5g/L, and the concentration of the 1-ethyl-3-methylimidazole acetate is 3.5g/L.
And step 3, weighing 100g of raw material powder, adding a composite ionic liquid extractant according to a ratio of 1g to 30mL, mixing and stirring for 10min, adjusting the pH of the mixed solution to 7.0 by using 0.1mol/LNaOH solution, heating to 75 ℃ and maintaining, and performing ultrasonic extraction for 60min under the condition of 40 kHz. After the extraction is finished, the suspension is centrifugally filtered through a centrifugal filter 1 at the rotating speed of 4500r/min, the filtrate is decompressed and concentrated to 1/3 of the liquid filtrate, the temperature is reduced to normal temperature, 95 percent ethanol is added into the normal temperature concentrated solution, the volume concentration of the ethanol in the mixed solution is 80 percent, the mixed solution is stood for 8 hours, the stood solution is centrifugally filtered through the centrifugal filter 2 for 20 minutes, the filter cake is crude polysaccharide, and the filtrate is sent to a distillation recovery device for recovery. Centrifugal filters 1 and 2 are designed according to a flow scheme, the types of which are the same for the purpose of defining the differences.
And 4, purifying, namely adding 50mL of deionized water into the crude polysaccharide obtained in the step 3 for redissolving, adding 1/5 volume of Sevage reagent, namely chloroform: n-butanol=4:1, carrying out intense shaking for 25min, centrifuging and layering, removing middle deformation proteins and a lower organic reagent layer, repeating the operation process of supernatant until the protein content in the supernatant is 0.43mg/100mg, and measuring the protein content by adopting a Coomassie brilliant blue method.
And 5, freeze drying, namely freeze drying the supernatant with the protein content of 0.43mg/100mg obtained in the step 4 for 18 hours at the temperature of minus 50 ℃ and collecting the supernatant to obtain the refined polyporus polysaccharide.
And (3) result detection:
And (3) measuring the polysaccharide content in the concentrated solution by adopting a phenol-sulfuric acid method, and further calculating the raw material with the polysaccharide extraction rate of 11.6-12.3 mg/100 mg.
The calculation method is that the extraction rate=the obtained polysaccharide/Polyporus x 100%.
Table 1 extraction yields of Polyporus polysaccharide from different groups
As shown in Table 1, the extraction rate of the polyporus polysaccharide of examples 1-4 is 11.94% + -0.36%, reaching 11.6-12.3 mg/100mg, which is higher than that of comparative example 1 by conventional water extraction method, and is 3-4 times of that of comparative example 1. Comparative example 2 the extraction of polyporus polysaccharide with trimethylamine hydrochloride alone was only higher than comparative example 1. Comparative example 3 the extraction rate of polyporus polysaccharide was still low by using 1-ethyl-3-methylimidazole acetate alone to extract polyporus polysaccharide. Comparative examples 2 and 3 show that the extraction rate of the examples of the present invention is not achieved by using either of the composite ionic liquids alone. Comparative examples 4, 5 were extractions using other anionic liquids, but with less effectiveness. In comparative example 6, other cationic liquids and 1-ethyl-3-methylimidazole acetate are used to form a composite ionic liquid for extraction, but the extraction rate is still much lower than that of examples 1-5.
And (3) reagent recovery, namely carrying out reduced pressure distillation on the filtrate obtained by centrifugal filtration of the centrifugal filter 2, wherein the operation pressure is 60kPa, recovering ethanol, the concentration of the obtained ethanol solution can reach 90%, the ethanol solution can be recycled, and the kettle liquid obtained by the reduced pressure distillation mainly contains ionic liquid trimethylamine hydrochloride, 1-ethyl-3-methylimidazole acetate and water, and the concentration of the ionic liquid can be determined by liquid chromatography and can be recycled.
DPPH free radical scavenging study, report methods such as Wang Hongliang are adopted. Reference is Wang Hongliang, hui Zhezhe, liang, et al, gleditsia sinensis leaf polysaccharide extraction process and research on antioxidant activity [ J ] Chinese grain and oil journal 1-11[2024-02-27.Https:// doi.org/10.20048/j.cnki.issn.1003-0174.000254. DPPH free radical removal research of refined Polyporus polysaccharide is carried out, and the result shows that the DPPH free radical removal rate of Polyporus polysaccharide is 94.3+/-0.63% when the concentration is 4.0mg/mL, which is equivalent to Vc removal rate under the same concentration.
OH radical scavenging study by the method of Zhang et al. As a result of conducting OH free radical scavenging study on purified polyporus umbellatus polysaccharide in reference ：AQ Zhang,NN Xiao,P F He,et al.Chemical analysis and antioxi-dant activity in vitro ofpolysaccharides extracted from Boletus edulis[J].International Journal ofBiological Macromolecules,2011,49(5):1092-1095., it was shown that the scavenging rate of OH free radical of polyporus umbellatus polysaccharide at 3.6mg/mL was 88.9.+ -. 0.63%, which is equivalent to Vc scavenging rate at the same concentration.
Reduction ability measurement, reference Ma Liyuan and the like, the potassium ferricyanide reduction method proposed by the research. Reference is Ma Liyuan, yellow and snowy, shang Erkun, etc. ultrasonic assisted enzyme method for extracting polysaccharide from corn husk and its antioxidative assay [ J ]. Food and machinery, 2023,39 (5): 186-192,202. The reduction capacity of refined polyporus polysaccharide is measured, and the result shows that the reduction capacity is gradually increased with the increase of polyporus polysaccharide concentration.
TABLE 2 free radical scavenging and reducing Properties of Polyporus polysaccharide extracted from different groups
As can be seen from Table 2, the oxidation resistance studies show that the polyporus polysaccharide extracted by the composite ionic liquid provided in examples 1 to 4 is equivalent to the polyporus polysaccharide extracted in comparative examples 1 to 6 in terms of reducing power. The data in Table 2 shows that the performance of the extracted polyporus umbellatus refined polysaccharide is basically consistent whether in examples or comparative examples, and the use of the composite ionic liquid provided by the invention has no influence on the structure and performance of the polyporus umbellatus polysaccharide, and the data difference is caused by experimental errors.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The method for extracting polyporus polysaccharide by using the composite ionic liquid is characterized by comprising the following steps of:
The composite ionic liquid is a mixture of trimethylamine hydrochloride and 1-ethyl-3-methylimidazole acetate, wherein the mass ratio of the trimethylamine hydrochloride to the 1-ethyl-3-methylimidazole acetate is 1-1.5:2-3.5;
preparing the composite ionic liquid into a composite ionic liquid solution, wherein the concentration of trimethylamine hydrochloride in the composite ionic liquid solution is 1.0-1.5 g/L, and the concentration of 1-ethyl-3-methylimidazole acetate is 2.0-3.5 g/L;
Mixing Polyporus umbellatus powder with the composite ionic liquid solution according to the feed-liquid ratio of 1 g:20-30 mL, adjusting the pH of the mixed solution to 6.5-7.0, heating to 70-75 ℃, carrying out ultrasonic treatment, filtering, and purifying the filtrate to obtain the Polyporus umbellatus polysaccharide.
2. The method according to claim 1, wherein the mass ratio of trimethylamine hydrochloride to 1-ethyl-3-methylimidazole acetate is 1:2-3.
3. The method according to claim 1, wherein the concentration of trimethylamine hydrochloride in the composite ionic liquid is 1.0 g/L and the concentration of 1-ethyl-3-methylimidazolium acetate is 2.0 g/L.
4. The method according to claim 1, wherein the ultrasonic conditions are 50-70 min, 40-80 kHz.
5. The method according to claim 1, wherein the pH of the mixture is adjusted by using a HCl solution or a NaOH solution.
6. The method of claim 5, wherein the concentration of the HCl solution or NaOH solution is 0.1-0.2 mol/L.
7. The method according to claim 1, wherein the purification method comprises concentrating the filtrate to 1/3 of the original volume, adding ethanol to make the volume concentration of ethanol in the mixed solution 80%, standing for 6-8 h, centrifuging, and filtering to obtain a filter cake which is crude polysaccharide.
8. The method according to claim 7, wherein the crude polysaccharide is purified by Sevage reagent to obtain a liquid having a protein content of 0.49% or less, and freeze-dried to obtain purified polyporus polysaccharide.
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