CN116535533B - Extraction process of selenium-containing Phellinus linteus polysaccharide - Google Patents
Extraction process of selenium-containing Phellinus linteus polysaccharide Download PDFInfo
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- CN116535533B CN116535533B CN202310481860.0A CN202310481860A CN116535533B CN 116535533 B CN116535533 B CN 116535533B CN 202310481860 A CN202310481860 A CN 202310481860A CN 116535533 B CN116535533 B CN 116535533B
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 161
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 161
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 161
- 241000001727 Tropicoporus linteus Species 0.000 title claims abstract description 156
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 90
- 239000011669 selenium Substances 0.000 title claims abstract description 90
- 238000000605 extraction Methods 0.000 title claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 229920001525 carrageenan Polymers 0.000 claims abstract description 18
- 229940113118 carrageenan Drugs 0.000 claims abstract description 18
- 235000010418 carrageenan Nutrition 0.000 claims abstract description 18
- 239000000679 carrageenan Substances 0.000 claims abstract description 18
- 239000000284 extract Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims abstract description 15
- 239000012265 solid product Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000287 crude extract Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 230000003544 deproteinization Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 2
- 239000003607 modifier Substances 0.000 abstract description 4
- 239000008681 Phellinus linteus extract Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 20
- 235000019441 ethanol Nutrition 0.000 description 14
- 230000014759 maintenance of location Effects 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 239000012530 fluid Substances 0.000 description 8
- 230000002496 gastric effect Effects 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 102000057297 Pepsin A Human genes 0.000 description 4
- 108090000284 Pepsin A Proteins 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 229940111202 pepsin Drugs 0.000 description 4
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- ZNOZWUKQPJXOIG-XSBHQQIPSA-L [(2r,3s,4r,5r,6s)-6-[[(1r,3s,4r,5r,8s)-3,4-dihydroxy-2,6-dioxabicyclo[3.2.1]octan-8-yl]oxy]-4-[[(1r,3r,4r,5r,8s)-8-[(2s,3r,4r,5r,6r)-3,4-dihydroxy-6-(hydroxymethyl)-5-sulfonatooxyoxan-2-yl]oxy-4-hydroxy-2,6-dioxabicyclo[3.2.1]octan-3-yl]oxy]-5-hydroxy-2-( Chemical compound O[C@@H]1[C@@H](O)[C@@H](OS([O-])(=O)=O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H]2OC[C@H]1O[C@H](O[C@H]1[C@H]([C@@H](CO)O[C@@H](O[C@@H]3[C@@H]4OC[C@H]3O[C@H](O)[C@@H]4O)[C@@H]1O)OS([O-])(=O)=O)[C@@H]2O ZNOZWUKQPJXOIG-XSBHQQIPSA-L 0.000 description 3
- -1 carrageenan selenide Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 210000002784 stomach Anatomy 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009169 immunotherapy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
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- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extraction process of selenium-containing Phellinus linteus polysaccharide, which comprises the following steps: (1) Pulverizing Phellinus linteus, mixing with clear water, stirring, and extracting under heating; and (5) removing Phellinus linteus residue in the extracting solution after the completion of the extraction, and obtaining the extracting solution for standby. (2) And (3) decoloring and deproteinizing the extracting solution to obtain a crude Phellinus linteus polysaccharide extracting solution. (3) Concentrating the crude Phellinus linteus polysaccharide extract to obtain concentrated solution; then adding selenized carrageenan into the concentrated solution and stirring to form a uniform mixed solution; and adding ethanol into the mixed solution, stirring uniformly, standing, performing solid-liquid separation, and drying the obtained solid product to obtain the selenium-containing Phellinus linteus polysaccharide. According to the invention, the Phellinus linteus extract is treated by using the selenylation carrageenan as the modifier, and the extracted Phellinus linteus polysaccharide contains a certain selenium element, so that the loss of the medical value of Phellinus linteus caused by the existing extraction process is compensated, and the selenium element is easy to be absorbed by human bodies.
Description
Technical Field
The invention relates to the field of Phellinus linteus polysaccharide extraction, in particular to a selenium-containing Phellinus linteus polysaccharide extraction process.
Background
Phellinus linteus polysaccharide is an active ingredient extracted from Phellinus linteus, which has been widely used in immunotherapy against tumor, oxidation, etc. The Phellinus linteus polysaccharide has the characteristics of small toxic and side effects, unique action mechanism and the like, and becomes a research hot spot at home and abroad. The extraction process of Phellinus linteus polysaccharide mainly comprises hot water extraction, dilute acid extraction, dilute alkali extraction, ultrasonic extraction, etc. Because the Phellinus linteus polysaccharide is easy to dissolve in water, the method has the advantages of low cost, simple and convenient operation and the like in the hot water extraction method, the method becomes the most extensive and economic process for extracting Phellinus linteus polysaccharide, the Phellinus linteus polysaccharide is dissolved in hot water after extraction to form a leaching solution, and then the Phellinus linteus polysaccharide in the leaching solution is extracted by a further extraction process to obtain a polysaccharide product. However, although Phellinus linteus contains abundant selenium elements, the current technology is difficult to effectively extract the selenium elements into Phellinus linteus polysaccharide products, and great loss is caused to the medicinal value of Phellinus linteus.
Disclosure of Invention
The invention provides an extraction process of selenium-containing Phellinus linteus polysaccharide, which contains a certain selenium element, and is not only helpful for compensating the loss of Phellinus linteus medicinal value caused by the existing extraction process, but also is easy to be absorbed by human body. Specifically, the extraction process of the selenium-containing Phellinus linteus polysaccharide comprises the following steps:
(1) Pulverizing Phellinus linteus, mixing with clear water, stirring, and extracting under heating. And (5) removing Phellinus linteus residue in the extracting solution after the completion of the extraction, and obtaining the extracting solution for standby.
(2) And (3) decoloring and deproteinizing the extracting solution to obtain a crude Phellinus linteus polysaccharide extracting solution.
(3) Concentrating the crude extract of Phellinus linteus polysaccharide to obtain concentrated solution. Then adding the selenized carrageenan into the concentrated solution and stirring to form a uniform mixed solution. And adding ethanol into the mixed solution, stirring uniformly, standing, performing solid-liquid separation, and drying the obtained solid product to obtain the selenium-containing Phellinus linteus polysaccharide.
In a further scheme, in the step (1), the ratio of Phellinus linteus to clear water is 1g: 30-50 mL. Optionally, mixing the two materials, and stirring for 10-15 min to fully infiltrate the Phellinus linteus with clear water.
In a further embodiment, in the step (1), the heating temperature is 80 to 90℃and the extraction is carried out under this condition for 2 to 3 hours.
In a further scheme, in the step (1), ultrasonic vibration with power of 200-300W is applied in the extraction process to assist in extraction, so that the extraction efficiency of Phellinus linteus polysaccharide is improved.
In a further scheme, in the step (2), a solid decoloring agent is added into the extracting solution according to the proportion of 3-5 g/L, the extracting solution is heated to a set temperature after being stirred uniformly, the temperature is kept, and the solid decoloring agent is removed by filtration after the completion of the stirring, so that the decoloring solution is obtained. Optionally, the heating temperature is 40-50 ℃, and the heat preservation time is 25-40 min.
In a further embodiment, the solid decolorizing agent includes any one of activated carbon, diatomaceous earth, an adsorption resin, and the like.
In a further scheme, in the step (2), deproteinization refers to that the decolorized solution is treated by adopting a Sevage method, and the crude extract of Phellinus linteus polysaccharide is obtained after the completion of the treatment. The method is a common method for removing protein in Phellinus linteus polysaccharide extract, and the invention is not described in detail.
In a further scheme, in the step (3), the crude Phellinus linteus polysaccharide extract is heated and concentrated to 40-50% of the initial volume, and the concentrated solution is obtained. Optionally, the heating temperature is 70-80 ℃.
In a further scheme, in the step (3), the ratio of the crude extract of Phellinus linteus polysaccharide to the selenized carrageenan is 1L: 0.5-0.72 g.
In a further scheme, in the step (3), the volume ratio of the mixed solution to the ethanol is 1:3 to 4.5. Preferably, the mass fraction of the ethanol is not less than 95%. And under the action of the ethanol, the Phellinus linteus polysaccharide and the selenylation carrageenan in the crude extract are separated out simultaneously to form the Phellinus linteus polysaccharide containing selenium.
In a further scheme, in the step (3), the standing time is 30-50 min, so that selenium-containing Phellinus linteus polysaccharide in the crude extract is fully separated out and precipitated.
In a further embodiment, in the step (3), the drying method includes any one of vacuum drying, freeze drying, and the like.
Compared with the prior art, the invention has at least the following beneficial effects: although the traditional hot water extraction process has the advantages of low cost, easy operation, more environmental protection and the like, the selenium element in the Phellinus linteus is difficult to be effectively extracted into Phellinus linteus polysaccharide products due to limited intensity of extraction, which leads to loss of medicinal value of Phellinus linteus. Therefore, the invention adopts the seleno carrageenan as the modifier to treat the Phellinus linteus extract, and the seleno carrageenan not only contains selenium element, but also has the characteristics of good water solubility and ethanol insolubility, and the seleno carrageenan is added into the extract to be dissolved so as to form the mixed solution containing Phellinus linteus polysaccharide and selenium-containing compounds. When the ethanol is further added into the mixed solution, the Phellinus linteus polysaccharide and the selenylation carrageenan are both indissolvable in the ethanol and are jointly separated out, and the selenylation carrageenan has the characteristic of gelation, and the Phellinus linteus polysaccharide is coated in the mixed solution after separation, so that a compact coating body is formed after further drying, the Phellinus linteus polysaccharide is effectively prevented from being contacted with external oxygen, and the problems of deterioration and failure of the Phellinus linteus polysaccharide due to oxidation in the storage process are solved, and the effect of Phellinus linteus polysaccharide products is reduced. In addition, the Phellinus linteus polysaccharide product prepared by the invention has a slow release function after entering human body, which is helpful for avoiding the problem that Phellinus linteus polysaccharide is easy to stimulate stomach to cause discomfort because of continuous high concentration in a short time, and can stably prolong the supply time of polysaccharide components and prolong the drug effect. In addition, the selenium element in the modifier adopted by the invention exists in the form of organic selenium, so that the selenium element is easier to be absorbed by human bodies, and the utilization rate of the selenium element in the selenium-containing Phellinus linteus polysaccharide prepared by the invention is ensured.
Detailed Description
It is to be noted that all terms of art and science used herein have the same meanings as those familiar to those skilled in the art unless otherwise defined. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. The invention will now be further described with reference to specific examples.
Example 1
An extraction process of selenium-containing Phellinus linteus polysaccharide comprises the following steps:
(1) Pulverizing Phellinus linteus fruiting body, mixing with clear water 1g: mixing at a ratio of 40mL, and mechanically stirring for 10min to fully infiltrate Phellinus linteus powder with clear water. Then the obtained mixed system is closed and heated to 85 ℃ in water bath for 2.5 hours. Filtering to remove Phellinus linteus residue, and collecting filtrate to obtain extractive solution.
(2) Adding active carbon into the extracting solution obtained in the step (1) according to the proportion of 4.5g/L, uniformly stirring, heating to 45 ℃ and preserving heat for 30min to decolorize the extracting solution, filtering to remove the active carbon after the decolorizing treatment is finished, and collecting a liquid phase to obtain the decolorizing solution. And adding a Sevage reagent (chloroform: n-butanol=5:1, volume ratio) into the decolorized solution, vibrating, standing, collecting supernatant after layering, and repeating the steps until the denatured protein layer of the middle layer disappears, thereby obtaining the crude polysaccharide extract of Phellinus linteus.
(3) Heating the crude Phellinus linteus polysaccharide extract obtained in the step (2) to 80 ℃ in water bath for concentration treatment, and concentrating to 45% of the initial volume to obtain a concentrated solution. Then adding carrageenan selenide powder (KAPPA-carrageenan, liaoning Congo. Technology Co., ltd.) into the concentrated solution according to the ratio of 0.65g/L, and stirring to form a uniform mixed solution. Then adding 4 times of ethanol (99% of mass fraction) into the mixed solution, stirring, and standing for 40min for alcohol precipitation. Finally filtering to separate out a precipitated solid product, and vacuum drying the solid product at 50 ℃ for 2 hours to obtain the selenium-containing Phellinus linteus polysaccharide.
1. The polysaccharide content of the selenium-containing Phellinus linteus polysaccharide prepared in this example was tested by sulfuric acid-phenol method. In addition, the content of selenium in the selenium-containing Phellinus linteus polysaccharide is tested by adopting an ICP-MS method, and the result is that: polysaccharide content=41.67%, selenium content 16.03 μg/g.
2. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in a sealed box with an oxygen concentration of 40%, the change in the content of polysaccharide component in the selenium-containing Phellinus linteus polysaccharide after 30 days of placement was measured, and the polysaccharide retention (%) was calculated to measure the oxidation resistance of the selenium-containing Phellinus linteus polysaccharide in air, the polysaccharide retention= (content of polysaccharide component in initial selenium-containing Phellinus linteus polysaccharide-content of polysaccharide component in selenium-containing Phellinus linteus polysaccharide after 30 days of placement)/content of polysaccharide component in initial selenium-containing Phellinus linteus polysaccharide was 99.31%.
3. Dilute hydrochloric acid of 1.5mol/ml concentration is taken, diluted with distilled water, for example, and then the pH is adjusted to 1.5. Then adding pepsin according to the proportion of 1g/100ml, uniformly mixing, and filtering to obtain the simulated gastric fluid. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in the simulated gastric fluid and the time for complete disintegration of the selenium-containing Phellinus linteus polysaccharide was tested and the result showed 78.2min.
Example 2
An extraction process of selenium-containing Phellinus linteus polysaccharide comprises the following steps:
(1) Pulverizing Phellinus linteus fruiting body, mixing with clear water 1g:50mL of the mixture is mixed, and then the mixture is mechanically stirred for 10min, so that the Phellinus linteus powder is fully soaked with clear water. And then sealing the obtained mixed system, heating to 90 ℃ in a water bath, keeping the temperature for 2.0 hours, and applying 200W of ultrasonic vibration in the extraction process to carry out auxiliary extraction. Filtering to remove Phellinus linteus residue, and collecting filtrate to obtain extractive solution.
(2) Adding diatomite into the extracting solution obtained in the step (1) according to the proportion of 5g/L, uniformly stirring, heating to 40 ℃ and preserving heat for 40min to decolorize the extracting solution, filtering to remove the diatomite after the decolorization treatment is finished, and collecting a liquid phase to obtain the decolorized solution. And adding a Sevage reagent (chloroform: n-butanol=5:1, volume ratio) into the decolorized solution, vibrating, standing, collecting supernatant after layering, and repeating the steps until the denatured protein layer of the middle layer disappears, thereby obtaining the crude polysaccharide extract of Phellinus linteus.
(3) And (3) heating the crude Phellinus linteus polysaccharide extract obtained in the step (2) to 75 ℃ in water bath, concentrating, and concentrating to 40% of the initial volume to obtain a concentrated solution. Then adding carrageenan selenide powder (KAPPA-carrageenan, liaoning Congo. Technology Co., ltd.) into the concentrated solution according to the ratio of 0.5g/L, and stirring to form a uniform mixed solution. Then adding 3 times of ethanol (95% of mass fraction) into the mixed solution, stirring, and standing for 30min for alcohol precipitation. Finally filtering to separate out a precipitated solid product, and vacuum drying the solid product at 50 ℃ for 2 hours to obtain the selenium-containing Phellinus linteus polysaccharide.
1. The polysaccharide content of the selenium-containing Phellinus linteus polysaccharide prepared in this example was tested by sulfuric acid-phenol method. In addition, the content of selenium in the selenium-containing Phellinus linteus polysaccharide is tested by adopting an ICP-MS method, and the result is that: polysaccharide content = 37.58%, selenium content 14.62 μg/g.
2. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in a sealed box with an oxygen concentration of 40%, the change in the content of polysaccharide component in the selenium-containing Phellinus linteus polysaccharide after 30 days of placement was measured, and the polysaccharide retention (%) was calculated to measure the oxidation resistance of the selenium-containing Phellinus linteus polysaccharide in air, the polysaccharide retention= (content of polysaccharide component in initial selenium-containing Phellinus linteus polysaccharide-content of polysaccharide component in selenium-containing Phellinus linteus polysaccharide after 30 days of placement)/content of polysaccharide component in initial selenium-containing Phellinus linteus polysaccharide was 99.56%.
3. Dilute hydrochloric acid of 1.5mol/ml concentration is taken, diluted with distilled water, for example, and then the pH is adjusted to 1.5. Then adding pepsin according to the proportion of 1g/100ml, uniformly mixing, and filtering to obtain the simulated gastric fluid. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in the simulated gastric fluid and the time for complete disintegration of the selenium-containing Phellinus linteus polysaccharide was tested and the result showed 73.7min.
Example 3
An extraction process of selenium-containing Phellinus linteus polysaccharide comprises the following steps:
(1) Pulverizing Phellinus linteus fruiting body, mixing with clear water 1g: mixing at a ratio of 30mL, and mechanically stirring for 15min to fully infiltrate Phellinus linteus powder with clear water. And then sealing the obtained mixed system, heating to 80 ℃ in a water bath, keeping for 3.0 hours, and applying ultrasonic vibration with power of 300W in the extraction process to carry out auxiliary extraction. Filtering to remove Phellinus linteus residue, and collecting filtrate to obtain extractive solution.
(2) Adding active carbon into the extracting solution obtained in the step (1) according to the proportion of 3g/L, uniformly stirring, heating to 50 ℃ and preserving heat for 25min to decolorize the extracting solution, filtering to remove the active carbon after the decolorization treatment is finished, and collecting a liquid phase to obtain the decolorized solution. And adding a Sevage reagent (chloroform: n-butanol=5:1, volume ratio) into the decolorized solution, vibrating, standing, collecting supernatant after layering, and repeating the steps until the denatured protein layer of the middle layer disappears, thereby obtaining the crude polysaccharide extract of Phellinus linteus.
(3) Heating the crude Phellinus linteus polysaccharide extract obtained in the step (2) to 70 ℃ in water bath for concentration treatment, and concentrating to 50% of the initial volume to obtain concentrated solution. Then adding carrageenan selenide powder (KAPPA-carrageenan, liaoning Congo. Technology Co., ltd.) into the concentrated solution according to the ratio of 0.72g/L, and stirring to form a uniform mixed solution. Then adding absolute ethyl alcohol with the volume of 4.5 times of that of the mixed solution, stirring, and standing for 50min for alcohol precipitation. Finally filtering to separate out a precipitated solid product, and vacuum drying the solid product at 50 ℃ for 2 hours to obtain the selenium-containing Phellinus linteus polysaccharide.
1. The polysaccharide content of the selenium-containing Phellinus linteus polysaccharide prepared in this example was tested by sulfuric acid-phenol method. In addition, the content of selenium in the selenium-containing Phellinus linteus polysaccharide is tested by adopting an ICP-MS method, and the result is that: polysaccharide content = 40.23%, selenium content 16.74 μg/g.
2. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in a sealed box with an oxygen concentration of 40%, the change in the content of polysaccharide component in the selenium-containing Phellinus linteus polysaccharide after 30 days of placement was measured, and the polysaccharide retention (%) was calculated to measure the oxidation resistance of the selenium-containing Phellinus linteus polysaccharide in air, the polysaccharide retention= (the content of polysaccharide component in the initial selenium-containing Phellinus linteus polysaccharide-the content of polysaccharide component in the selenium-containing Phellinus linteus polysaccharide after 30 days of placement)/the content of polysaccharide component in the initial selenium-containing Phellinus linteus polysaccharide, resulting in 99.24%.
3. Dilute hydrochloric acid of 1.5mol/ml concentration is taken, diluted with distilled water, for example, and then the pH is adjusted to 1.5. Then adding pepsin according to the proportion of 1g/100ml, uniformly mixing, and filtering to obtain the simulated gastric fluid. The selenium-containing Phellinus linteus polysaccharide prepared in this example was placed in the simulated gastric fluid and the time for complete disintegration of the selenium-containing Phellinus linteus polysaccharide was tested and the result showed 75.4min.
Example 4
An extraction process of selenium-containing Phellinus linteus polysaccharide comprises the following steps:
(1) Pulverizing Phellinus linteus fruiting body, mixing with clear water 1g: mixing at a ratio of 40mL, and mechanically stirring for 10min to fully infiltrate Phellinus linteus powder with clear water. Then the obtained mixed system is closed and heated to 85 ℃ in water bath for 2.5 hours. Filtering to remove Phellinus linteus residue, and collecting filtrate to obtain extractive solution.
(2) Adding active carbon into the extracting solution obtained in the step (1) according to the proportion of 4.5g/L, uniformly stirring, heating to 45 ℃ and preserving heat for 30min to decolorize the extracting solution, filtering to remove the active carbon after the decolorizing treatment is finished, and collecting a liquid phase to obtain the decolorizing solution. And adding a Sevage reagent (chloroform: n-butanol=5:1, volume ratio) into the decolorized solution, vibrating, standing, collecting supernatant after layering, and repeating the steps until the denatured protein layer of the middle layer disappears, thereby obtaining the crude polysaccharide extract of Phellinus linteus.
(3) Heating the crude Phellinus linteus polysaccharide extract obtained in the step (2) to 80 ℃ in water bath for concentration treatment, and concentrating to 45% of the initial volume to obtain a concentrated solution. Then adding 4 times of ethanol (99% of mass fraction) into the mixed solution, stirring, and standing for 40min for alcohol precipitation. Finally filtering to separate out a precipitated solid product, and vacuum drying the solid product at 50 ℃ for 2 hours to obtain the Phellinus linteus polysaccharide product.
1. The polysaccharide content of the Phellinus linteus polysaccharide product prepared in this example was tested by sulfuric acid-phenol method. In addition, the selenium content in the Phellinus linteus polysaccharide product is tested by ICP-MS method, and the result is: polysaccharide content = 82.96%, selenium content 0.24 μg/g.
2. The Phellinus linteus polysaccharide products prepared in this example were placed in a sealed box with an oxygen concentration of 40%, the change in the content of polysaccharide component in the Phellinus linteus polysaccharide products after 30 days of placement was measured, and the polysaccharide retention (%) was calculated to measure the oxidation resistance of the Phellinus linteus polysaccharide products in air, the polysaccharide retention= (content of polysaccharide component in initial Phellinus linteus polysaccharide product-content of polysaccharide component in Phellinus linteus polysaccharide product after 30 days of placement)/content of polysaccharide component in initial Phellinus linteus polysaccharide product, resulting in 97.13%.
3. Dilute hydrochloric acid of 1.5mol/ml concentration is taken, diluted with distilled water, for example, and then the pH is adjusted to 1.5. Then adding pepsin according to the proportion of 1g/100ml, uniformly mixing, and filtering to obtain the simulated gastric fluid. The Phellinus linteus polysaccharide product prepared in this example was placed in the simulated gastric fluid and the time for complete disintegration of the Phellinus linteus polysaccharide product was tested and the result showed 26.3min.
From the test results of the above examples, it can be seen that the selenium-containing Phellinus linteus polysaccharide obtained by treating Phellinus linteus extract with selenized carrageenan as modifier in examples 1-3 contains selenium element with a certain content, while the selenium content in Phellinus linteus polysaccharide product obtained by conventional hot water leaching method in example 4 is significantly lower than that in examples 1-3, which shows that the selenium content of Phellinus linteus polysaccharide product can be effectively improved by treating with the selenized carrageenan.
In addition, as can be seen from the test results, compared with the embodiment 4, the selenium-containing Phellinus linteus polysaccharide prepared in the embodiments 1-3 has better polysaccharide retention rate and complete disintegration time, which shows that the Phellinus linteus polysaccharide is coated in the selenium-containing Phellinus linteus polysaccharide by utilizing the gelation characteristic point of the selenized carrageenan, and the Phellinus linteus polysaccharide can be effectively prevented from contacting with external oxygen after further drying, so that the problems of deterioration and failure of Phellinus linteus polysaccharide due to oxidation during storage and further reduction of efficacy of Phellinus linteus polysaccharide products are overcome. Meanwhile, the Phellinus linteus polysaccharide product in the form has a slow release function after entering a human body, which is beneficial to avoiding the problem that the Phellinus linteus polysaccharide is easy to stimulate the stomach to cause discomfort because of continuous high concentration in a short time, and can stably prolong the supply time of polysaccharide components and prolong the drug effect.
The foregoing description is only of the preferred embodiments of the invention and is not intended to limit the invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (14)
1. An extraction process of selenium-containing Phellinus linteus polysaccharide is characterized by comprising the following steps:
(1) Pulverizing Phellinus linteus, mixing with clear water, stirring, and extracting under heating; removing Phellinus linteus residue in the extractive solution after completion to obtain extractive solution for use;
(2) Decolorizing and deproteinizing the extract to obtain crude Phellinus linteus polysaccharide extract;
(3) Concentrating the crude Phellinus linteus polysaccharide extract to obtain concentrated solution; then adding selenized carrageenan into the concentrated solution and stirring to form a uniform mixed solution; adding ethanol into the mixed solution, stirring uniformly, standing, performing solid-liquid separation, and drying the obtained solid product to obtain selenium-containing Phellinus linteus polysaccharide;
In the step (3), the ratio of the crude extract of Phellinus linteus polysaccharide to the selenized carrageenan is 1L: 0.5-0.72 g.
2. The extraction process of selenium-containing Phellinus linteus polysaccharide as set forth in claim 1, wherein in the step (1), the ratio of Phellinus linteus to clear water is 1g: 30-50 mL.
3. The process for extracting selenium-containing Phellinus linteus polysaccharide as claimed in claim 1, wherein in the step (1), the mixture is stirred for 10-15 min.
4. The process for extracting selenium-containing Phellinus linteus polysaccharide as set forth in claim 1, wherein in the step (1), the heating temperature is 80 to 90 ℃ and the extraction is carried out under the condition for 2 to 3 hours.
5. The extraction process of selenium-containing Phellinus linteus polysaccharide according to claim 1, wherein in the step (1), ultrasonic vibration with power of 200-300W is applied for auxiliary extraction.
6. The extraction process of selenium-containing Phellinus linteus polysaccharide according to claim 1, wherein in the step (2), a solid decolorizer is added into the extracting solution according to the proportion of 3-5 g/L, the extracting solution is heated to a set temperature after being stirred uniformly, the heating temperature is 40-50 ℃, the heat preservation time is 25-40 min, and the solid decolorizer is removed after the completion of the filtering, thus obtaining the decolorized solution.
7. The extraction process of selenium-containing Phellinus linteus polysaccharide as set forth in claim 6, wherein the solid decolorizer comprises any one of activated carbon, diatomaceous earth, and adsorption resin.
8. The extraction process of selenium-containing Phellinus linteus polysaccharide according to claim 1, wherein in the step (2), deproteinization means that the decolorized solution is treated by a Sevage method, and the crude Phellinus linteus polysaccharide extract is obtained after completion of the treatment.
9. The extraction process of selenium-containing Phellinus linteus polysaccharide according to claim 1, wherein in the step (3), the crude Phellinus linteus polysaccharide extract is heated and concentrated to 40-50% of the initial volume to obtain the concentrated solution.
10. The extraction process of selenium-containing Phellinus linteus polysaccharide as set forth in claim 9, wherein the heating temperature is 70-80 ℃.
11. The extraction process of selenium-containing Phellinus linteus polysaccharide according to claim 1, wherein in the step (3), the volume ratio of the mixed liquid to ethanol is 1:3 to 4.5.
12. The extraction process of selenium-containing Phellinus linteus polysaccharide as claimed in claim 11, wherein the mass fraction of ethanol is not less than 95%.
13. The process for extracting selenium-containing Phellinus linteus polysaccharide as set forth in any one of claims 1-12, wherein the standing time in the step (3) is 30-50 min, so that the selenium-containing Phellinus linteus polysaccharide in the crude extract is sufficiently separated out and precipitated.
14. The process for extracting selenium-containing Phellinus linteus polysaccharide as set forth in any one of claims 1 to 12, wherein the drying method in the step (3) comprises any one of vacuum drying and freeze drying.
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