CN115536759B - Method for extracting fucoidan by subcritical water - Google Patents
Method for extracting fucoidan by subcritical water Download PDFInfo
- Publication number
- CN115536759B CN115536759B CN202211285997.0A CN202211285997A CN115536759B CN 115536759 B CN115536759 B CN 115536759B CN 202211285997 A CN202211285997 A CN 202211285997A CN 115536759 B CN115536759 B CN 115536759B
- Authority
- CN
- China
- Prior art keywords
- extraction
- kelp
- drying
- fucan
- filtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229920000855 Fucoidan Polymers 0.000 title claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 103
- 238000000605 extraction Methods 0.000 claims abstract description 92
- 238000001035 drying Methods 0.000 claims abstract description 69
- 238000001914 filtration Methods 0.000 claims abstract description 69
- 238000001556 precipitation Methods 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 33
- 241000512259 Ascophyllum nodosum Species 0.000 claims description 112
- 239000000706 filtrate Substances 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 34
- 230000001376 precipitating effect Effects 0.000 claims description 31
- DBTMGCOVALSLOR-DEVYUCJPSA-N (2s,3r,4s,5r,6r)-4-[(2s,3r,4s,5r,6r)-3,5-dihydroxy-6-(hydroxymethyl)-4-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]oxy-6-(hydroxymethyl)oxane-2,3,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](CO)O[C@H](O)[C@@H]2O)O)O[C@H](CO)[C@H]1O DBTMGCOVALSLOR-DEVYUCJPSA-N 0.000 claims description 26
- 229920001543 Laminarin Polymers 0.000 claims description 26
- 239000005717 Laminarin Substances 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- 239000002518 antifoaming agent Substances 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 17
- 239000008399 tap water Substances 0.000 claims description 17
- 235000020679 tap water Nutrition 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- 238000010992 reflux Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 10
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 238000003809 water extraction Methods 0.000 claims 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 33
- 239000012043 crude product Substances 0.000 description 30
- 238000010298 pulverizing process Methods 0.000 description 16
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 15
- 229930195725 Mannitol Natural products 0.000 description 15
- 238000007605 air drying Methods 0.000 description 15
- 229920000615 alginic acid Polymers 0.000 description 15
- 235000010443 alginic acid Nutrition 0.000 description 15
- 239000004744 fabric Substances 0.000 description 15
- 238000007710 freezing Methods 0.000 description 15
- 230000008014 freezing Effects 0.000 description 15
- 150000002632 lipids Chemical class 0.000 description 15
- 239000000594 mannitol Substances 0.000 description 15
- 235000010355 mannitol Nutrition 0.000 description 15
- 238000004806 packaging method and process Methods 0.000 description 15
- 239000000049 pigment Substances 0.000 description 15
- 229910017053 inorganic salt Inorganic materials 0.000 description 14
- 230000000087 stabilizing effect Effects 0.000 description 14
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 12
- PNNNRSAQSRJVSB-SLPGGIOYSA-N Fucose Natural products C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C=O PNNNRSAQSRJVSB-SLPGGIOYSA-N 0.000 description 12
- SHZGCJCMOBCMKK-DHVFOXMCSA-N L-fucopyranose Chemical compound C[C@@H]1OC(O)[C@@H](O)[C@H](O)[C@@H]1O SHZGCJCMOBCMKK-DHVFOXMCSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 150000004676 glycans Chemical class 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 4
- 239000005017 polysaccharide Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011344 liquid material Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 241000015177 Saccharina japonica Species 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- -1 antiviral Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003097 mucus Anatomy 0.000 description 1
- 150000004804 polysaccharides Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- 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
Landscapes
- 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)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to the technical field of extraction processes of fucans, in particular to a method for extracting fucans by subcritical water, which comprises the following steps: subcritical extraction; cooling and filtering; removing impurities; concentrating; alcohol precipitation; centrifuging; and (5) drying. The method for extracting the fucan has the advantages that the fucan extraction rate can reach 5.38%, the total sugar content can reach 20.12% (taking the fucan as a standard product), the purity can reach 28.16%, the extraction yield is obviously higher than that of the traditional various extraction methods, the extraction time is short, the efficiency is high, the physicochemical property is excellent, the environment is protected, the sustainable development is realized, and the equipment requirement is low.
Description
Technical Field
The invention relates to the technical field of extraction processes of fucans, in particular to a method for extracting fucans by subcritical water.
Background
Kelp (Laminaria japonica) is a perennial large edible algae. Sporophytes are large, brown and flat. The blade, the handle and the fixing device are respectively provided, and the fixing device is in a pseudo-root shape. The leaf is composed of epidermis, cortex and medulla tissue, and sporangium is arranged under the leaf. Has a mucus cavity, and can secrete sliding substances. The tree-shaped branches of the anchor are used for attaching submarine rocks and growing in the sea with lower water temperature. Has great yield in coastal areas of China, is rich in various excellent components, and has wide application prospect.
Fucan, called fucan, fucan sulfate, fucoidan sulfate, etc., is mainly derived from brown algae, and is a polysaccharide containing fucose and sulfuric acid groups. It has various biological functions such as anticoagulation, anti-tumor, antithrombotic, antiviral, antioxidant and immunity enhancing, etc., and thus is widely used in the medical field and the modern food industry.
In recent years, researchers have adopted new technologies such as enzymolysis extraction, ultrasonic extraction and acid extraction, so that the extraction rate of fucans is improved to a certain extent, but the technologies have some limitations. For example: the enzymolysis extraction method has the advantages of high polysaccharide extraction rate, mild reaction condition and small damage to the polysaccharide structure, but the enzymolysis extraction method has high requirements on production reaction condition due to higher enzyme cost, and is not suitable for large-scale industrial production. The ultrasonic extraction method can improve the extraction rate of polysaccharide and shorten the extraction time, but sometimes can cause mixing of polysaccharide extraction product components, and aggravate the pressure of subsequent separation and purification. The acid extraction method has poor activity of the extracted components, and has great pollution to the environment, and more investment is required for environmental remediation engineering.
The water with temperature and pressure above the critical point (the temperature range is usually between 100 ℃ and 374 ℃ and the pressure range is usually between 0.1 and 22.1 MPa), called as supercritical water, has very different physical and chemical properties from common liquid water, has good solubility, and can realize mutual solubility among gas, liquid and organic solid. Because supercritical water has very high requirements on equipment and is extremely corrosive, in order to reduce the requirements on the equipment, part of research is started to perform related reactions under the subcritical condition.
The subcritical water (Subcritical water) is also an extraction method which is easy to repeat, green and environment-friendly and has sustainable development benefits, and has excellent application prospects for researching the selection of various parameters in fucan extraction.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for extracting fucoidan by subcritical water.
In order to solve the technical problems, the invention provides a method for extracting fucoidan by subcritical water, which comprises the following steps:
subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed liquid ratio of 1:10-1:50 g/mL, wherein the pressure of the extraction kettle is stabilized at 0.8Mpa, the extraction temperature is 150-200 ℃, and the extraction time is 15-35 min, so as to obtain kelp extract;
cooling and filtering: cooling the extract to below 80 ℃, transferring the extract into a centrifugal filter for filtering, collecting filtrate and refrigerating the filtrate at 2-8 ℃;
removing impurities: adding a calcium chloride solution into the refrigerated filtrate, standing, filtering floccules, and collecting a clear solution;
concentrating: concentrating the clarified liquid, and simultaneously adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, mixing thoroughly, and forming a mixture when fucan component is separated out;
and (3) centrifuging: centrifuging the flocculent mixture after alcohol precipitation, and collecting precipitate;
and (3) drying: and (3) drying the centrifugal precipitate at a low temperature in vacuum to obtain a crude laminarin product.
In a more preferred embodiment, the kelp powder is prepared from dry kelp by pretreatment.
In a more preferred embodiment, the kelp pretreatment comprises the steps of:
washing dry kelp with tap water and distilled water respectively, airing, pulverizing, adding 8 times of 95% ethanol solution in volume into the pulverized material, refluxing at 85 ℃ for 3-4 hours, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder.
In a more preferred embodiment, the concentration of the calcium chloride solution is 5% -20% and the addition amount is 1/3-1/5 of the volume of the refrigerated filtrate.
In a more preferred embodiment, the calcium chloride solution is at a concentration of 10% and is added in an amount of 1/4 of the volume of the refrigerated filtrate.
In a more preferred embodiment, the ratio of the kelp powder to deionized water is 1:30g/mL.
In a more preferred embodiment, the extraction temperature of the subcritical extraction is 160 to 190 ℃.
In a more preferred embodiment, the subcritical extraction is performed at a temperature of 160℃for a period of 25 minutes.
In a more preferred embodiment, the subcritical extraction is performed at a temperature of 170 ℃ for a time period of 25 minutes.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the highest extraction rate of the fucosan can reach 5.38 percent, the highest total sugar content can reach 20.12 percent (taking fucose as a standard product), and the highest purity can reach 28.16 percent.
2. The subcritical water is adopted to extract the fucoidan, the extraction yield is obviously higher than that of the traditional various extraction methods, the extraction time is short, the efficiency is high, the physicochemical properties are excellent, the environment is protected, the sustainable development is realized, and the equipment requirement is low.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the following description will be made in detail with reference to the technical solutions of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention; the technical features designed in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other; 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.
In the description of the present invention, it should be noted that all terms used in the present invention (including technical terms and scientific terms) have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs and are not to be construed as limiting the present invention; it will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The invention provides a method for extracting laminarin by subcritical water, which comprises the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding an ethanol solution with the volume of 95% which is 8 times of that of the crushed materials, refluxing for 3-4 hours at the temperature of 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, and placing filter residues in a drying box at the temperature of 45 ℃ to obtain kelp powder after drying.
(2) Subcritical extraction: putting kelp powder and deionized water into a subcritical extraction kettle according to a feed liquid ratio of 1:10-1:50 g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 150-200 ℃ for 15-35 min to obtain kelp extract;
in some preferred embodiments, the feed liquid ratio of the kelp powder to the deionized water is 1:10-1:50 g/mL, the extraction temperature is 160-180 ℃, the extraction time is 15-35 min, and the extraction rate is more than 2%; in some more preferred embodiments, the feed liquid ratio of the kelp powder to the deionized water is 1:30g/mL, the extraction temperature is 160-180 ℃, the extraction time is 25min, and the extraction rate is more than 3%; in some preferred embodiments, the ratio of the kelp powder to deionized water is 1:30g/mL, the extraction temperature is 160-170 ℃, the extraction time is 25min, and the extraction rate is more than 4%.
(3) Cooling and filtering: and cooling the extract to below 80 ℃ by utilizing a snake-shaped condensing tube in the reaction kettle, and transferring the extract into a centrifugal filter for filtering. Collecting filtrate, and refrigerating in a refrigerator at 2-8deg.C; the preferred temperature for refrigeration is 5 ℃.
(4) Removing impurities: taking out the refrigerated filtrate and adding 1/3-1/5 of CaCl with 10 percent of volume 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth to obtain clear solution;
(5) Concentrating: concentrating the clear liquid by adopting a rotary evaporator, adding a defoaming agent, and inhibiting bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the mixture after alcohol precipitation into a centrifuge, centrifuging at 10000r/min, collecting precipitate, and packaging with container.
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product.
The invention provides the following examples and comparative examples:
example 1
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. To the crushed material was added 8 times by volume of a 95% ethanol solution, and refluxed at 85 ℃ for 4 hours to remove most of pigments, lipids, mannitol, inorganic salts and the like. Filtering, and placing the filter residue in a drying box at 45 ℃ to obtain kelp powder after drying;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:10g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 160 ℃ for 15min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 2.07%, the total sugar content is 2.09% (taking fucose as standard substance) and the purity is 5.34%.
Example two
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:20g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 170 ℃ for 20min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 2.57%, the total sugar content is 2.67% (taking fucose as standard substance) and the purity is 8.33%.
Example III
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 180 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 3.40%, the total sugar content is 6.65% (taking fucose as standard substance), and the purity is 9.48%.
Example IV
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:40g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, and extracting at 190 ℃ for 30min to obtain kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clear liquid by adopting a rotary evaporator, adding a defoaming agent, and inhibiting bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 1.91%, the total sugar content is 4.32% (taking fucose as standard substance), and the purity is 6.14%.
Example five
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:50g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 180 ℃ for 35min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 2.39%, the total sugar content is 3.28% (taking fucose as standard substance), and the purity is 12.84%.
Example six
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 160 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 5.38%, the total sugar content is 7.37% (taking fucose as standard substance), and the purity is 9.70%.
Example seven
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 170 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clear liquid by adopting a rotary evaporator, adding a defoaming agent, and inhibiting bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of the kelp fucan is 4.46%, the total sugar content is 20.12% (taking the fucan as a standard product), and the purity is 28.16%.
Example eight
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 95% ethanol solution with volume of 8 times of that of the crushed materials, refluxing at 85 ℃ for 4 hours to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, and placing filter residues in a drying box at 45 ℃ to obtain kelp powder after drying;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 150 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth to obtain clear solution;
(5) Concentrating: concentrating the clear liquid by adopting a rotary evaporator, adding a defoaming agent, and inhibiting bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of the kelp fucan is 3.06%, the total sugar content is 6.38% (taking the fucan as a standard product), and the purity is 8.67%.
Example nine
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:20g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 160 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 2.47%, the total sugar content is 4.35% (taking fucose as standard substance), and the purity is 7.67%.
Examples ten
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:40g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 160 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of the kelp fucan is 2.39%, the total sugar content is 5.59% (taking the fucan as a standard product), and the purity is 6.98%.
Example eleven
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 95% ethanol solution with volume of 8 times of that of the crushed materials, refluxing at 85 ℃ for 4 hours to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, and placing filter residues in a drying box at 45 ℃ to obtain kelp powder after drying;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:20g/mL, stabilizing the pressure of the reaction kettle to 0.8Mpa, extracting at 170 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80deg.C by using a snake-shaped condenser tube in the reaction kettle, transferring into a centrifugal filter for filtration, and refrigerating the filtrate at 5deg.C;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin and fucose is 1.68%, the total sugar content is 3.65% (fucose is used as standard substance), and the purity is 5.13%.
Example twelve
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:40g/mL, and extracting at 170 ℃ for 25min under the condition that the pressure of the reaction kettle is stabilized at 0.8Mpa to obtain kelp extract;
(3) Cooling and filtering: cooling the extract to below 80 ℃ by using a snake-shaped condenser tube in the reaction kettle, transferring the extract into a continuous centrifugal filter for filtration, and then refrigerating the filtrate at 5 ℃;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth to obtain clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of laminarin is 2.11%, the total sugar content is 4.99% (taking fucose as standard substance), and the purity is 6.53%.
Comparative example one
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 8 times of 95% ethanol solution into the crushed materials, refluxing for 4 hours at 85 ℃ to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.7Mpa, extracting at 160 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80 ℃ by using a snake-shaped condenser tube in the reaction kettle, transferring the extract into a continuous centrifugal filter for filtration, and then refrigerating the filtrate at 5 ℃;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth, and collecting clear solution;
(5) Concentrating: concentrating the clarified liquid by adopting a rotary evaporator, and adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of the kelp fucan is 3.32%, the total sugar content is 5.89% (taking the fucan as a standard product), and the purity is 8.62%.
Comparative example two
A method for extracting laminarin by subcritical water, comprising the following steps:
(1) Pretreatment of kelp: washing dry kelp with tap water and distilled water, air drying, and pulverizing. Adding 95% ethanol solution with volume of 8 times of that of the crushed materials, refluxing at 85 ℃ for 4 hours to remove most of pigment, lipid, mannitol, inorganic salt and the like, filtering, and placing filter residues in a drying box at 45 ℃ to obtain kelp powder after drying;
(2) Subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, stabilizing the pressure of the reaction kettle to 0.9Mpa, extracting at 160 ℃ for 25min, and obtaining kelp extract;
(3) Cooling and filtering: cooling the extract to below 80 ℃ by using a snake-shaped condenser tube in the reaction kettle, transferring the extract into a continuous centrifugal filter for filtration, and then refrigerating the filtrate at 5 ℃;
(4) Removing impurities: taking out the refrigerated filtrate, adding 1/4 volume of 10% CaCl 2 Precipitating the solution for 30min to form floccules from impurities such as algin, filtering the floccules with filter cloth to obtain clear solution;
(5) Concentrating: concentrating the clear liquid by adopting a rotary evaporator, adding a defoaming agent, and inhibiting bubble generation in the concentration process to obtain a concentrated solution;
(6) Alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, precipitating fucoidan component, mixing thoroughly, standing overnight to form flocculent mixture;
(7) And (3) centrifuging: delivering the flocculent mixture subjected to the alcohol precipitation in the step (6) into a centrifugal machine, centrifuging at 10000r/min, collecting precipitate, and sub-packaging with a container;
(8) And (3) drying: and (3) after pre-freezing the subpackaged crude product, drying in a freeze dryer until the moisture is completely removed, and obtaining the kelp fucan crude product. The extraction rate of the kelp fucan is 4.08%, the total sugar content is 4.43% (taking the fucan as a standard product), and the purity is 9.33%.
It can be seen from the above experimental examples that the two conditions of temperature and liquid-to-material ratio are changed as the main influencing factors. Under the temperature change, the polarity of subcritical water is similar to that of fucan, so that the fucan component in kelp is promoted to be separated out. The change of the liquid-material ratio mainly changes the mixing property of subcritical water and raw materials, and the too high liquid-material ratio can cause too thin solution, so that the extraction purity is reduced, and meanwhile, the solvent and energy are wasted; the excessively low liquid-material ratio can lead to the reduction of the component precipitation degree of the fucosan, the reduction of the overall extraction rate and the waste of raw materials.
The specific parameters or reagents commonly used in the above embodiments are specific embodiments or preferred embodiments contemplated by the present invention, and are not limiting thereof; and can be adaptively adjusted by those skilled in the art within the concept and the protection scope of the invention. Unless otherwise indicated, the starting materials employed may also be commercially available products or may be prepared by methods conventional in the art.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (3)
1. A method for subcritical water extraction of fucoidan, comprising the steps of:
pretreatment: washing dry kelp with tap water and distilled water respectively, airing and crushing, adding 8 times of 95% ethanol solution by volume into crushed materials, refluxing for 3-4 hours at 85 ℃, filtering, placing filter residues into a drying box at 45 ℃, and drying to obtain kelp powder;
subcritical extraction: adding kelp powder and deionized water into a subcritical extraction kettle according to a feed-liquid ratio of 1:30g/mL, wherein the pressure of the extraction kettle is stabilized at 0.8Mpa, the extraction temperature is 170 ℃, and the extraction time is 25min, so as to obtain kelp extract;
cooling and filtering: cooling the extract to below 80 ℃, transferring the extract into a centrifugal filter for filtering, collecting filtrate and refrigerating the filtrate at 2-8 ℃;
removing impurities: adding a calcium chloride solution into the refrigerated filtrate, wherein the concentration of the calcium chloride solution is 10%, the adding amount is 1/4 of the volume of the refrigerated filtrate, precipitating for 30min, filtering floccules, and collecting a clear solution;
concentrating: concentrating the clarified liquid, and simultaneously adding a defoaming agent to inhibit bubble generation in the concentration process to obtain a concentrated solution;
alcohol precipitation: adding 3 times of 95% ethanol solution to the concentrated solution, mixing thoroughly, and forming flocculent mixture when fucan component is separated out;
and (3) centrifuging: centrifuging the flocculent mixture after alcohol precipitation, and collecting precipitate;
and (3) drying: and (3) drying the centrifugal precipitate at a low temperature in vacuum to obtain a crude laminarin product.
2. A fucan obtained from the subcritical water-extraction method of fucan of claim 1.
3. Fucan according to claim 2, wherein the total sugar content in the fucan is 20.12%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211285997.0A CN115536759B (en) | 2022-10-20 | 2022-10-20 | Method for extracting fucoidan by subcritical water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211285997.0A CN115536759B (en) | 2022-10-20 | 2022-10-20 | Method for extracting fucoidan by subcritical water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115536759A CN115536759A (en) | 2022-12-30 |
| CN115536759B true CN115536759B (en) | 2024-02-27 |
Family
ID=84736151
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211285997.0A Active CN115536759B (en) | 2022-10-20 | 2022-10-20 | Method for extracting fucoidan by subcritical water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115536759B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671399A (en) * | 2009-10-10 | 2010-03-17 | 山东大学威海分校 | Preparation method of fucoidan sulfuric ester with high purity and high-sulfate radical content |
| CN103387622A (en) * | 2013-08-23 | 2013-11-13 | 福建华尔康生物科技有限公司 | Method for extracting fucoidan and removing heavy metals from kelps |
| CN104403018A (en) * | 2014-11-26 | 2015-03-11 | 中国科学院海洋研究所 | Algal polysaccharide extraction method |
| KR101757776B1 (en) * | 2016-02-03 | 2017-07-26 | (주) 아이투비 | Film Manufacturing Method Using Fucoidan Extracted from Marine Algae |
-
2022
- 2022-10-20 CN CN202211285997.0A patent/CN115536759B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671399A (en) * | 2009-10-10 | 2010-03-17 | 山东大学威海分校 | Preparation method of fucoidan sulfuric ester with high purity and high-sulfate radical content |
| CN103387622A (en) * | 2013-08-23 | 2013-11-13 | 福建华尔康生物科技有限公司 | Method for extracting fucoidan and removing heavy metals from kelps |
| CN104403018A (en) * | 2014-11-26 | 2015-03-11 | 中国科学院海洋研究所 | Algal polysaccharide extraction method |
| KR101757776B1 (en) * | 2016-02-03 | 2017-07-26 | (주) 아이투비 | Film Manufacturing Method Using Fucoidan Extracted from Marine Algae |
Non-Patent Citations (1)
| Title |
|---|
| Subcritical water extraction of fucoidan from Saccharina japonica: optimization, characterization and biological studies;Periaswamy Sivagnanam Saravana等;《J Appl Phycol》;第30卷;579-590 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115536759A (en) | 2022-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8585863B2 (en) | Separation of lignin from hydrolyzate | |
| CN100491405C (en) | Extraction and preparation technology for pectin of orange pericarp | |
| WO2015010497A1 (en) | Method for preparing lycium ruthenicum polysaccharide | |
| CN102718668B (en) | Method for extracting synephrine and hesperidin from citrus aurantium | |
| CN110272932B (en) | Preparation method of ganoderma lucidum spore powder polysaccharide peptide | |
| CN106008739B (en) | The preparation method of oyster polysaccharide | |
| CN103204800B (en) | A kind of extracting method of 1 DNJ | |
| CN100522982C (en) | Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent | |
| CN102993328A (en) | Method for comprehensively extracting polysaccharides, polyphenol and saponin from camellia oleifera abel defatted cakes | |
| CN102002083B (en) | Method for extracting high-purity rutin with flash-extraction technology | |
| CN111471732A (en) | Novel selenium-rich tea source ACE inhibitory peptide and preparation method thereof | |
| CN101455291B (en) | Fructose and oligo-fructose production method using garlic fructosan hydrolase | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN113980153A (en) | Method for extracting high-viscosity peach gum polysaccharide | |
| CN115536759B (en) | Method for extracting fucoidan by subcritical water | |
| US10968470B2 (en) | Method for preparing rubusoside | |
| CN102784193A (en) | Method for preparing hedysarum polybotrys extract by adopting coupling technology | |
| CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
| CN110819444A (en) | Method for extracting tea oil and tea saponin from camellia seeds | |
| CN104292355A (en) | Method for extraction of platycodon grandiflorum polysaccharide | |
| CN112442136A (en) | Method for extracting functional components from tremella | |
| CN112047994A (en) | Method for extracting tea saponin from camellia seed meal | |
| CN1410424A (en) | Extraction technology of new stellerin A | |
| CN102775511A (en) | Method for extracting pepper polysaccharide from pepper residue | |
| CN107151259B (en) | The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |