CN114573725B - Extraction method of spine date seed polysaccharide extract - Google Patents
Extraction method of spine date seed polysaccharide extract Download PDFInfo
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 73
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 73
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 73
- 238000000605 extraction Methods 0.000 title claims abstract description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 37
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- 240000008866 Ziziphus nummularia Species 0.000 claims abstract description 23
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004365 Protease Substances 0.000 claims abstract description 17
- 238000005238 degreasing Methods 0.000 claims abstract description 17
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- 238000002156 mixing Methods 0.000 claims description 15
- 238000000874 microwave-assisted extraction Methods 0.000 claims description 14
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- 238000000926 separation method Methods 0.000 claims description 13
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 12
- 239000001509 sodium citrate Substances 0.000 claims description 12
- 238000001694 spray drying Methods 0.000 claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 11
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- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
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- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- VBGGLSWSRVDWHB-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 claims description 3
- 240000003584 Ziziphus jujuba Species 0.000 claims 1
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract 1
- 239000004480 active ingredient Substances 0.000 abstract 1
- 235000018102 proteins Nutrition 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- 239000003153 chemical reaction reagent Substances 0.000 description 10
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- 239000003921 oil Substances 0.000 description 6
- 108090000145 Bacillolysin Proteins 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 102000035092 Neutral proteases Human genes 0.000 description 5
- 108091005507 Neutral proteases Proteins 0.000 description 5
- 108090000526 Papain Proteins 0.000 description 5
- 229940088598 enzyme Drugs 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 5
- 229940055729 papain Drugs 0.000 description 5
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 2
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- 229930003944 flavone Natural products 0.000 description 2
- 150000002212 flavone derivatives Chemical class 0.000 description 2
- 235000011949 flavones Nutrition 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 150000001720 carbohydrates Chemical class 0.000 description 1
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- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 239000004615 ingredient Substances 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002772 monosaccharides Chemical group 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- 239000003208 petroleum 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
- 230000001766 physiological effect Effects 0.000 description 1
- 235000004252 protein component Nutrition 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004799 sedative–hypnotic effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 230000035922 thirst Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
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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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses an extraction method of a spine date seed polysaccharide extract, which comprises the steps of firstly crushing spine date seeds, promoting the active ingredients in the spine date seeds to be fully dissociated, fundamentally ensuring the full extraction of polysaccharide, and then using supercritical CO (carbon monoxide) 2 The extraction is carried out on the wild jujube seed powder to realize effective degreasing, then most of protein is removed by combination of protease enzymolysis and Sevag method, crude wild jujube seed polysaccharide is obtained by alcohol precipitation, and then the crude wild jujube seed polysaccharide is purified by utilizing fluorine modified magnetic microspheres to obtain the wild jujube seed polysaccharide extract. The method has high extraction rate, and the obtained polysaccharide has high purity and good quality, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of polysaccharide extraction, and particularly relates to an extraction method of a spine date seed polysaccharide extract.
Background
The polysaccharide is a polymeric sugar high molecular carbohydrate composed of at least 10 monosaccharides bonded by glycosidic bond, and can be represented by general formula (C 6 H 10 O 5 ) n And (3) representing. The polysaccharide is an important component of organisms, is an energy supply source and a tissue constituent of life bodies, can participate in biological processes such as intercellular recognition, regulation of organism immunity, transformation of cells, apoptosis of tumor cells and the like, and has important physiological effects of resisting tumors, regulating organism immunity, reducing blood sugar and blood fat, resisting oxidation, resisting inflammation, easing pain, resisting radiation and the like.
Semen Ziziphi Spinosae is dry mature seed of Zizyphi Spinosae semen of Rhamnaceae, harvesting in autumn, soaking the fruit for one time, removing pulp, taking out, grinding with stone mill, taking out seed, and sun drying. The wild jujube seed is sweet in taste and flat in nature, and has the effects of calming heart, soothing nerves, nourishing liver, arresting sweating and promoting fluid production. Is mainly used for treating dysphoria, insomnia, palpitation, dreaminess, deficiency of body, excessive sweat, body fluid impairment and thirst, and is a common traditional Chinese medicine. The wild jujube mainly contains effective ingredients of flavone, saponin and the like for sedative hypnotic, and clinically, the wild jujube is mainly used as a medicament by raw products and stir-fried products.
The semen ziziphi spinosae contains fatty oil, protein and the like besides polysaccharide, so that when the polysaccharide component is extracted from semen ziziphi spinosae, the most important is to separate the fatty oil and the protein and the like so as not to influence the purity of the polysaccharide and prevent the further utilization of the polysaccharide.
Patent application CN107674127A discloses a preparation method of semen Ziziphi Spinosae polysaccharide, which comprises the steps of adding solvent petroleum ether or diethyl ether into dry powder of semen Ziziphi Spinosae medicinal material, heating and refluxing at 70-90 ℃ for two times, each time for 1-2 hours, removing fatty substances, filtering, and drying residues; reflux-extracting the residue with 70% ethanol water solution for 2 hr, removing impurities such as flavone and saponin, filtering, and oven drying the residue; adding pure water into the residue solid, extracting with ultrasonic assistance at 40-70deg.C and 180-240W for 30-50min, and filtering to obtain filtrate; concentrating the filtrate under reduced pressure to obtain concentrated solution; adding 95% ethanol into the concentrated solution, refrigerating at 4deg.C overnight, filtering to obtain precipitate, washing the precipitate with ethanol for several times while stirring, washing with acetone for several times while stirring, and drying to obtain coarse polysaccharide of yellow brown semen Ziziphi Spinosae. The patent application has low extraction rate of polysaccharide in the spina date seeds, the purity of the obtained polysaccharide is low, and the production amplification effect exists, so that the large-scale production application is limited.
The patent application discloses that the spine date seed polysaccharide can be used for anti-tumor treatment, and the applicant discovers that the purity of the spine date seed polysaccharide extract directly relates to the anti-tumor effect, so that the improvement of the purity of the spine date seed polysaccharide extract has great significance for future clinical application.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the extraction method of the spine date seed polysaccharide extract, which has high extraction rate, high purity and good quality of the obtained polysaccharide and is suitable for large-scale production.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
an extraction method of semen Ziziphi Spinosae polysaccharide extract comprises the following specific steps:
(1) Crushing the spina date seeds into spina date seed powder with 80-100 meshes, adding the spina date seed powder into water, carrying out microwave extraction, concentrating under reduced pressure, transferring the solution into a spray drying tower, and drying the solution to obtain spina date seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen ziziphi spinosae powder obtained in the step (2) into water, carrying out microwave extraction, centrifuging to obtain a supernatant, continuously adding protease into the extract for enzymolysis, inactivating enzyme, concentrating to 1/4-1/3 of the original volume of the extract to obtain an enzymolysis solution, removing most of proteins in the enzymolysis solution by using a Sevag method to obtain a defatted deproteinized extract, and carrying out alcohol precipitation to obtain crude polysaccharide of semen ziphi spinosae;
(4) Adding the crude polysaccharide of the wild jujube seeds prepared in the step (3) into water, uniformly stirring, adding fluorine modified magnetic microspheres, uniformly dispersing by ultrasonic waves, adding absolute ethyl alcohol, shaking for 1-2 minutes, separating out precipitates, using magnet to adsorb and separate, dispersing the precipitates into water by ultrasonic waves, removing the magnetic microspheres by magnet adsorption, and spray-drying to obtain the wild jujube seed polysaccharide extract.
Preferably, the mass ratio of the spina date seed powder to the protease to the fluorine modified magnetic microsphere is 3-4: 0.2 to 0.3:0.02 to 0.03.
Further preferably, the protease is neutral protease and papain according to a mass ratio of 3:1 are uniformly mixed.
Preferably, in step (1), the process conditions of the microwave extraction are: and 300-400W microwave extraction for 5-10 min.
Preferably, in step (1), the process conditions of the supersonic jet are: 40-50 ℃, 0.05-0.07 MPa and 800-900 m/s.
Preferably, in step (2), supercritical CO 2 The extraction process conditions are as follows: extracting pressure is 38-40 MPa, extracting temperature is 50-52 ℃, CO 2 The flow is 10-15 kg/h, the extraction time is 2-3 hours, the separation pressure is 5-6 MPa, and the separation temperature is 55-57 ℃.
Preferably, in the step (3), the process conditions of the microwave extraction are as follows: extracting with 300-400W microwave for 25-30 min.
Preferably, in the step (3), the enzymolysis process conditions are as follows: enzymolysis is carried out for 3 to 4 hours at 55 to 60 ℃.
Preferably, in the step (3), the specific method of the Sevag method is as follows: adding an equal volume of Sevag reagent into the enzymolysis liquid, carrying out intense shaking, and centrifuging to obtain a supernatant, namely the degreasing deproteinized extract; wherein, the Sevag reagent is prepared by mixing chloroform and n-butanol according to a volume ratio of 5:1 are evenly mixed.
Preferably, in the step (3), the specific method of alcohol precipitation is as follows: adding a 90-95% ethanol aqueous solution with the volume fraction of 3-4 times of the volume into the degreasing deproteinized extracting solution, standing for 12-15 hours at the temperature of 0-4 ℃, and centrifuging to obtain a precipitate.
Preferably, in the step (4), the preparation method of the fluorine modified magnetic microsphere comprises the following steps of:
(A) Firstly, adding 1 part of nano ferroferric oxide into 30-40 parts of 0.2-0.3 mol/L sodium citrate solution, dispersing by 300-400W ultrasonic waves for 40-50 minutes, and magnetically separating to obtain sodium citrate modified nano ferroferric oxide;
(B) Ultrasonically dispersing sodium citrate modified nano ferroferric oxide in 4-5 parts of water, pouring into 25-30 parts of liquid sodium silicate, and uniformly stirring to obtain a water phase; then adding 1.5-2 parts of OP-10 and 5-6 parts of span-80 into 55-60 parts of dichloromethane, and stirring and uniformly mixing to obtain an oil phase; slowly dripping the water phase into the oil phase while stirring to obtain emulsion, slowly dripping the emulsion into 2-3 mol/L ammonium sulfate aqueous solution while stirring, stirring for 2-3 hours at 400-500 r/min, magnetically sucking out solid substances, and washing with water for 2-3 times to obtain magnetic microspheres;
(C) Finally, dispersing the magnetic microspheres in 35-45 parts of ethanol solution with the volume concentration of 70-80%, continuously adding 0.2-0.3 part of perfluorodecyl trimethoxy silane, heating to reflux, preserving heat and stirring for 4-5 hours, magnetically sucking out solid substances, washing with absolute ethanol, and drying to obtain the magnetic microsphere.
The invention also discloses a spine date seed polysaccharide extract obtained by the extraction method.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts supercritical CO 2 The extraction replaces the common organic solvent degreasing method, is safe and nontoxic, has good degreasing effect and thorough degreasing, provides a good foundation for the subsequent polysaccharide extraction, and improves the extraction rate and purity of the polysaccharide.
(2) The invention adopts the combination of protease and Sevag method to remove most proteins, and the protease enzymolysis can degrade macromolecular proteins contained in the extracting solution, reduce the entanglement and encapsulation of polysaccharide components, promote polysaccharide to be free, remove most proteins by combining Sevag method, and then carry out alcohol precipitation, thereby greatly reducing the adhesion of protein components on the surface of the polysaccharide and improving the purity of the polysaccharide.
(3) The crude polysaccharide of the wild jujube seed is further purified by the fluorine-modified magnetic microsphere which has magnetism, can be conveniently separated and removed by a magnet, and is simple to operate. The surface of the magnetic microsphere is modified by fluorine, and the surface of the fluorine modified magnetic microsphere is coated in the polysaccharide alcohol precipitation process, probably because the hydrogen bond formed by fluorine and the hydroxyl groups of the polysaccharide has stronger action, the phenomenon that a small amount of protein remained in a system is precipitated along with the polysaccharide alcohol is avoided, so that the polysaccharide is purified, and the high-purity polysaccharide is obtained. The applicant also tries to surface modify the magnetic microsphere by using epoxy groups and silicon hydroxyl groups instead of fluorine, and found that the purity of the obtained polysaccharide is inferior to that of the polysaccharide purified by the fluorine modified magnetic microsphere, which is probably because the hydrogen bonding between fluorine and polysaccharide is stronger compared with the epoxy groups and the silicon hydroxyl groups, thus being more beneficial to the separation of the polysaccharide and protein.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
The preparation method of the fluorine modified magnetic microsphere comprises the following specific steps:
(A) Firstly, adding 10g of nano ferroferric oxide into 300-400 g of 0.2-0.3 mol/L sodium citrate solution, performing 400W ultrasonic dispersion for 45 minutes, and performing magnetic separation to obtain sodium citrate modified nano ferroferric oxide;
(B) Then dispersing sodium citrate modified nano ferroferric oxide in 50g of water by ultrasonic, pouring into 300g of liquid sodium silicate, and stirring and uniformly mixing to obtain a water phase; then adding 20g of OP-10 and 60g of span-80 into 600g of dichloromethane, and stirring and uniformly mixing to obtain an oil phase; slowly dripping the water phase into the oil phase while stirring to obtain emulsion, slowly dripping the emulsion into 2.5mol/L ammonium sulfate water solution while stirring, stirring for 3 hours at 500r/min, magnetically sucking out solid substances, and washing with water for 3 times to obtain magnetic microspheres;
(C) Finally, dispersing the magnetic microspheres in 400g of 70% ethanol solution by volume concentration, continuously adding 2.5g of perfluorodecyl trimethoxy silane, heating to reflux, preserving heat and stirring for 4 hours, magnetically sucking out solid substances, washing with absolute ethanol, and drying to obtain the magnetic microsphere.
Example 1
An extraction method of semen Ziziphi Spinosae polysaccharide extract comprises the following specific steps:
(1) Firstly, 3g of spina date seeds are crushed into 80-mesh spina date seed powder, the powder is added into 30g of water, 300W of microwave extraction is carried out for 5 minutes, reduced pressure concentration is carried out, and the mixture is transferred into a spray drying tower for drying, thus obtaining the spina date seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen Ziziphi Spinosae powder into 28g water, extracting with 300W microwave for 25 min, centrifuging to obtain supernatant, adding 0.2g protease (obtained by uniformly mixing neutral protease and papain at mass ratio of 3:1) into the extractive solution, performing enzymolysis at 55deg.C for 3 hr, inactivating enzyme, concentrating to 1/4 of the original volume of the extractive solution to obtain enzymolysis solution, removing most proteins in the enzymolysis solution by Sevag method to obtain defatted deproteinized extractive solution, and precipitating with ethanol to obtain semen Ziziphi Spinosae crude polysaccharide;
(4) Adding the crude polysaccharide of the wild jujube seeds into 20g of water, uniformly stirring, adding 0.02g of fluorine modified magnetic microspheres, uniformly dispersing by ultrasonic waves, adding 20g of absolute ethyl alcohol, shaking for 1 minute, separating out precipitates, separating by using magnet adsorption, dispersing the precipitates into 30g of water by ultrasonic waves, removing the magnetic microspheres by using magnet adsorption, and spray-drying to obtain the polysaccharide extract of the wild jujube seeds.
In step (2), supercritical CO 2 The extraction process conditions are as follows: extracting pressure 38MPa, extracting temperature 50 ℃, CO 2 The flow is 10kg/h, the extraction time is 2 hours, the separation pressure is 5MPa, and the separation temperature is 55 ℃.
In the step (3), the specific method of the Sevag method is as follows: adding an equal volume of Sevag reagent into the enzymolysis liquid, carrying out intense shaking, and centrifuging to obtain a supernatant, namely the degreasing deproteinized extract; wherein, the Sevag reagent is prepared by mixing chloroform and n-butanol according to a volume ratio of 5:1 are evenly mixed.
In the step (3), the specific method of alcohol precipitation is as follows: adding 3 times volume of 90% ethanol water solution into the defatted deproteinized extract, standing at 0deg.C for 12 hr, centrifuging, and collecting precipitate.
Example 2
An extraction method of semen Ziziphi Spinosae polysaccharide extract comprises the following specific steps:
(1) Firstly, crushing 4g of spina date seeds into 100-mesh spina date seed powder, adding the powder into 35g of water, carrying out 400W microwave extraction for 10 minutes, concentrating under reduced pressure, and transferring the concentrated solution into a spray drying tower for drying to obtain spina date seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen Ziziphi Spinosae powder into 30g water, extracting with 400W microwave for 30 min, centrifuging to obtain supernatant, adding 0.3g protease (obtained by uniformly mixing neutral protease and papain at mass ratio of 3:1) into the extractive solution, performing enzymolysis at 60deg.C for 4 hr, inactivating enzyme, concentrating to 1/3 of the original volume of the extractive solution to obtain enzymolysis solution, removing most protein in the enzymolysis solution by Sevag method to obtain defatted deproteinized extractive solution, and precipitating with ethanol to obtain semen Ziziphi Spinosae crude polysaccharide;
(4) Adding the crude polysaccharide of the wild jujube seeds into 25g of water, uniformly stirring, adding 0.03g of fluorine modified magnetic microspheres (reference example), uniformly dispersing by ultrasonic waves, adding 25g of absolute ethyl alcohol, shaking for 2 minutes, separating out precipitates by using magnet adsorption, dispersing the precipitates into 35g of water by ultrasonic waves, removing the magnetic microspheres by magnet adsorption, and spray-drying to obtain the wild jujube seed polysaccharide extract.
In step (2), supercritical CO 2 The extraction process conditions are as follows: extraction pressure 40MPa, extraction temperature 52 ℃, CO 2 The flow is 15kg/h, the extraction time is 3 hours, the separation pressure is 6MPa, and the separation temperature is 57 ℃.
In the step (3), the specific method of the Sevag method is as follows: adding an equal volume of Sevag reagent into the enzymolysis liquid, carrying out intense shaking, and centrifuging to obtain a supernatant, namely the degreasing deproteinized extract; wherein, the Sevag reagent is prepared by mixing chloroform and n-butanol according to a volume ratio of 5:1 are evenly mixed.
In the step (3), the specific method of alcohol precipitation is as follows: adding 4 times volume of 95% ethanol water solution into the defatted deproteinized extract, standing at 4deg.C for 15 hr, centrifuging, and collecting precipitate.
Example 3
An extraction method of semen Ziziphi Spinosae polysaccharide extract comprises the following specific steps:
(1) Crushing 3.5g of wild jujube seeds into 90-mesh wild jujube seed powder, adding the powder into 33g of water, performing 400W microwave extraction for 8 minutes, concentrating under reduced pressure, transferring into a spray drying tower, and drying to obtain wild jujube seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen Ziziphi Spinosae powder into 29g, extracting with 400W microwave for 28 min, centrifuging to obtain supernatant, adding 0.25g protease (obtained by uniformly mixing neutral protease and papain at mass ratio of 3:1) into the extractive solution, performing enzymolysis at 58deg.C for 3.5 hr, inactivating enzyme, concentrating to 1/4 of the original volume of the extractive solution to obtain enzymolysis solution, removing most protein in the enzymolysis solution by Sevag method to obtain defatted deproteinized extractive solution, and precipitating with ethanol to obtain semen Ziziphi Spinosae crude polysaccharide;
(4) Adding the crude polysaccharide of the wild jujube seeds into 22g of water, uniformly stirring, adding 0.025g of fluorine modified magnetic microspheres (reference example), uniformly dispersing by ultrasonic waves, adding 23g of absolute ethyl alcohol, shaking for 2 minutes, separating out precipitates by using magnet adsorption, dispersing the precipitates into 34g of water by ultrasonic waves, removing the magnetic microspheres by magnet adsorption, and spray-drying to obtain the wild jujube seed polysaccharide extract.
In step (2), supercritical CO 2 The extraction process conditions are as follows: extraction pressure is 39MPa, extraction temperature is 51 ℃, and CO 2 The flow rate is 12kg/h, the extraction time is 2.5 hours, the separation pressure is 5.5MPa, and the separation temperature is 56 ℃.
In the step (3), the specific method of the Sevag method is as follows: adding an equal volume of Sevag reagent into the enzymolysis liquid, carrying out intense shaking, and centrifuging to obtain a supernatant, namely the degreasing deproteinized extract; wherein, the Sevag reagent is prepared by mixing chloroform and n-butanol according to a volume ratio of 5:1 are evenly mixed.
In the step (3), the specific method of alcohol precipitation is as follows: adding 3.5 times volume of 93% ethanol water solution into the defatted deproteinized extract, standing at 2deg.C for 13 hr, centrifuging, and collecting precipitate.
Comparative example 1
An extraction method of semen Ziziphi Spinosae polysaccharide extract comprises the following specific steps:
(1) Firstly, 3g of spina date seeds are crushed into 80-mesh spina date seed powder, the powder is added into 30g of water, 300W of microwave extraction is carried out for 5 minutes, reduced pressure concentration is carried out, and the mixture is transferred into a spray drying tower for drying, thus obtaining the spina date seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen Ziziphi Spinosae powder into 28g water, extracting with 300W microwave for 25 min, centrifuging to obtain supernatant, adding 0.2g protease (obtained by uniformly mixing neutral protease and papain at mass ratio of 3:1) into the extractive solution, performing enzymolysis at 55deg.C for 3 hr, inactivating enzyme, concentrating to 1/4 of the original volume of the extractive solution to obtain enzymolysis solution, removing most proteins in the enzymolysis solution by Sevag method to obtain defatted deproteinized extractive solution, and precipitating with ethanol to obtain semen Ziziphi Spinosae crude polysaccharide;
(4) Adding the crude polysaccharide of the wild jujube seeds into 20g of water, uniformly stirring, adding 0.02g of epoxy modified magnetic microspheres, uniformly dispersing by ultrasonic waves, adding 20g of absolute ethyl alcohol, shaking for 1 minute, separating out precipitates, separating out the precipitates by using magnet adsorption, dispersing the precipitates into 30g of water by ultrasonic waves, removing the magnetic microspheres by magnet adsorption, and spray-drying to obtain the polysaccharide extract of the wild jujube seeds.
In step (2), supercritical CO 2 The extraction process conditions are as follows: extracting pressure 38MPa, extracting temperature 50 ℃, CO 2 The flow is 10kg/h, the extraction time is 2 hours, the separation pressure is 5MPa, and the separation temperature is 55 ℃.
In the step (3), the specific method of the Sevag method is as follows: adding an equal volume of Sevag reagent into the enzymolysis liquid, carrying out intense shaking, and centrifuging to obtain a supernatant, namely the degreasing deproteinized extract; wherein, the Sevag reagent is prepared by mixing chloroform and n-butanol according to a volume ratio of 5:1 are evenly mixed.
In the step (3), the specific method of alcohol precipitation is as follows: adding 3 times volume of 90% ethanol water solution into the defatted deproteinized extract, standing at 0deg.C for 12 hr, centrifuging, and collecting precipitate.
In the step (4), the preparation method of the epoxy modified magnetic microsphere comprises the following steps:
(A) Firstly, adding 1g of nano ferroferric oxide into 30-40 g of 0.2-0.3 mol/L sodium citrate solution, dispersing by 300-400W ultrasonic waves for 40-50 minutes, and magnetically separating to obtain sodium citrate modified nano ferroferric oxide;
(B) Then dispersing sodium citrate modified nano ferroferric oxide in 4-5 g of water by ultrasonic, pouring into 25-30 g of liquid sodium silicate, and stirring and mixing uniformly to obtain a water phase; then adding 1.5-2 g OP-10 and 5-6 kg span-80 into 55-60 g methylene dichloride, stirring and mixing uniformly to obtain an oil phase; slowly dripping the water phase into the oil phase while stirring to obtain emulsion, slowly dripping the emulsion into 2-3 mol/L ammonium sulfate aqueous solution while stirring, stirring for 2-3 hours at 400-500 r/min, magnetically sucking out solid substances, and washing with water for 2-3 times to obtain magnetic microspheres;
(C) Finally, dispersing the magnetic microspheres in 35-45 g of ethanol solution with the volume concentration of 70-80%, continuously adding 0.2-0.3 g of gamma-glycidoxypropyl trimethoxysilane, heating to reflux, preserving heat, stirring for 4-5 hours, magnetically sucking out solid matters, washing with absolute ethanol, and drying to obtain the magnetic microsphere.
The extraction rates (based on the weight of the semen Ziziphi Spinosae powder) of examples 1 to 3 and comparative example 1 were measured, and the polysaccharide content in the obtained semen Ziziphi Spinosae polysaccharide extract was calculated by phenol-sulfuric acid method using the method for measuring polysaccharide of China pharmacopoeia 2015. The results are shown in Table 1.
TABLE 1 yield and polysaccharide purity of polysaccharide extract
| Extraction yield (%) | Purity (%) | |
| Example 1 | 0.782 | 90.95 |
| Example 2 | 0.780 | 92.96 |
| Example 3 | 0.789 | 88.98 |
| Comparative example 1 | 0.780 | 81.53 |
As can be seen from Table 1, examples 1 to 3 have high extraction rate and purity of polysaccharide from semen Ziziphi Spinosae.
The technical idea of the present invention is described by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must be implemented depending on the above embodiments. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of individual raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (8)
1. The extraction method of the spine date seed polysaccharide extract is characterized by comprising the following specific steps:
(1) Crushing the spina date seeds into spina date seed powder with 80-100 meshes, adding the spina date seed powder into water, carrying out microwave extraction, concentrating under reduced pressure, transferring the solution into a spray drying tower, and drying the solution to obtain spina date seed powder;
(2) Then utilizing supercritical CO 2 Degreasing the spina date seed powder by extraction to obtain de-oiled spina date seed powder;
(3) Adding the defatted semen ziziphi spinosae powder obtained in the step (2) into water, carrying out microwave extraction, centrifuging to obtain a supernatant, continuously adding protease into the extract for enzymolysis, inactivating enzyme, concentrating to 1/4-1/3 of the original volume of the extract to obtain an enzymolysis solution, removing most of proteins in the enzymolysis solution by using a Sevag method to obtain a defatted deproteinized extract, and carrying out alcohol precipitation to obtain crude polysaccharide of semen ziphi spinosae;
(4) Adding the crude polysaccharide of the wild jujube seeds prepared in the step (3) into water, uniformly stirring, adding fluorine modified magnetic microspheres, uniformly dispersing by ultrasonic waves, adding absolute ethyl alcohol, shaking for 1-2 minutes, separating out precipitates, using magnet to adsorb and separate, dispersing the precipitates into water by ultrasonic waves, removing the magnetic microspheres by magnet adsorption, and spray-drying to obtain the polysaccharide extract of the wild jujube seeds;
the preparation method of the fluorine modified magnetic microsphere comprises the following steps:
(A) Firstly, adding 1 part of nano ferroferric oxide into 30-40 parts of 0.2-0.3 mol/L sodium citrate solution, dispersing by 300-400W ultrasonic waves for 40-50 minutes, and magnetically separating to obtain sodium citrate modified nano ferroferric oxide;
(B) Ultrasonically dispersing sodium citrate modified nano ferroferric oxide in 4-5 parts of water, pouring into 25-30 parts of liquid sodium silicate, and uniformly stirring to obtain a water phase; then adding 1.5-2 parts of OP-10 and 5-6 parts of span-80 into 55-60 parts of dichloromethane, and stirring and uniformly mixing to obtain an oil phase; slowly dripping the water phase into the oil phase while stirring to obtain emulsion, slowly dripping the emulsion into 2-3 mol/L ammonium sulfate aqueous solution while stirring, stirring for 2-3 hours at 400-500 r/min, magnetically sucking out solid substances, and washing with water for 2-3 times to obtain magnetic microspheres;
(C) Finally, dispersing the magnetic microspheres in 35-45 parts of ethanol solution with the volume concentration of 70-80%, continuously adding 0.2-0.3 part of perfluorodecyl trimethoxy silane, heating to reflux, preserving heat and stirring for 4-5 hours, magnetically sucking out solid substances, washing with absolute ethanol, and drying to obtain the magnetic microsphere.
2. The extraction method according to claim 1, wherein the mass ratio of the semen zizyphi spinosae powder to the protease to the fluorine modified magnetic microsphere is 3-4: 0.2 to 0.3:0.02 to 0.03.
3. The extraction method according to claim 1, wherein in step (1), the process conditions of the microwave extraction are: and 300-400W microwave extraction for 5-10 min.
4. The method according to claim 1, wherein in the step (2), supercritical CO 2 The extraction process conditions are as follows: extracting pressure is 38-40 MPa, extracting temperature is 50-52 ℃, CO 2 The flow is 10-15 kg/h, the extraction time is 2-3 hours, the separation pressure is 5-6 MPa, and the separation temperature is 55-57 ℃.
5. The extraction method according to claim 1, wherein in step (3), the process conditions of microwave extraction are: extracting with 300-400W microwave for 25-30 min.
6. The extraction method according to claim 1, wherein in the step (3), the enzymatic hydrolysis is performed under the following conditions: enzymolysis is carried out for 3 to 4 hours at 55 to 60 ℃.
7. The extraction method according to claim 1, wherein in the step (3), the specific method of alcohol precipitation is as follows: adding a 90-95% ethanol aqueous solution with the volume fraction of 3-4 times of the volume into the degreasing deproteinized extracting solution, standing for 12-15 hours at the temperature of 0-4 ℃, and centrifuging to obtain a precipitate.
8. A polysaccharide extract of zizyphus jujuba obtained by the extraction method of any one of claims 1 to 7.
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