CN107814852B - Method for extracting atractylodes macrocephala polysaccharide - Google Patents
Method for extracting atractylodes macrocephala polysaccharide Download PDFInfo
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- CN107814852B CN107814852B CN201711094503.XA CN201711094503A CN107814852B CN 107814852 B CN107814852 B CN 107814852B CN 201711094503 A CN201711094503 A CN 201711094503A CN 107814852 B CN107814852 B CN 107814852B
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- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 97
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 97
- 150000004676 glycans Chemical class 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 37
- 241000092665 Atractylodes macrocephala Species 0.000 title claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 241000132012 Atractylodes Species 0.000 claims abstract description 41
- 239000012153 distilled water Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- 238000002386 leaching Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- -1 polysaccharide metal complex Chemical class 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 9
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 9
- 239000002808 molecular sieve Substances 0.000 claims description 9
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000000605 extraction Methods 0.000 abstract description 28
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 11
- 239000012043 crude product Substances 0.000 abstract description 9
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 230000004071 biological effect Effects 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 238000012423 maintenance Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 54
- 238000012360 testing method Methods 0.000 description 38
- 238000004090 dissolution Methods 0.000 description 32
- 239000000523 sample Substances 0.000 description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- 229910052725 zinc Inorganic materials 0.000 description 14
- 239000011701 zinc Substances 0.000 description 14
- 229910052742 iron Inorganic materials 0.000 description 12
- 239000010949 copper Substances 0.000 description 11
- 229910052802 copper Inorganic materials 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000011790 ferrous sulphate Substances 0.000 description 6
- 235000003891 ferrous sulphate Nutrition 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 6
- 238000005457 optimization Methods 0.000 description 6
- 239000012086 standard solution Substances 0.000 description 6
- 238000004448 titration Methods 0.000 description 6
- 238000003809 water extraction Methods 0.000 description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000013522 chelant Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000011573 trace mineral Substances 0.000 description 5
- 235000013619 trace mineral Nutrition 0.000 description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 5
- 229960001763 zinc sulfate Drugs 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000013589 supplement Substances 0.000 description 4
- 229920001661 Chitosan Polymers 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 230000009920 chelation Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 241000132011 Atractylodes lancea Species 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 description 2
- 241001149107 Limonium bicolor Species 0.000 description 2
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 235000010703 Modiola caroliniana Nutrition 0.000 description 2
- 244000038561 Modiola caroliniana Species 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 229920001542 oligosaccharide Polymers 0.000 description 2
- 229940078042 polysaccharide iron complex Drugs 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 102100021587 Embryonic testis differentiation protein homolog A Human genes 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 101000898120 Homo sapiens Embryonic testis differentiation protein homolog A Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 235000013622 meat product Nutrition 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 1
- 239000011686 zinc sulphate 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/16—Inorganic salts, minerals or trace elements
- A23L33/165—Complexes or chelates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Mycology (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Botany (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses an extraction method of bighead atractylodes rhizome polysaccharide, which comprises the following steps: (1) taking powder of dry rhizoma atractylodis macrocephalae roots or/and stems, adding distilled water with the temperature of more than 85 ℃ for extraction to obtain an extract, and then adjusting the temperature of the extract to 30-80 ℃; (2) adding distilled water into the leaching liquor obtained in the step (1), adding a sulfate solution, adjusting the pH value to 3-8, reacting for 0.5-3.0h, and filtering to obtain a first extracting solution and filter residues; (3) and (3) repeatedly extracting the obtained filter residue at least once according to the steps (1) and (2) to obtain multiple extracting solutions, combining the multiple extracting solutions, evaporating and concentrating, adding absolute ethyl alcohol, standing overnight, filtering to obtain a precipitate, washing and drying the precipitate to obtain a crude product of the atractylenovata polysaccharide chelated with metal ions. The extraction method has the advantages of low process difficulty, milder extraction conditions, higher yield and better maintenance of the biological activity of the polysaccharide.
Description
Technical Field
The invention relates to a plant polysaccharide method, in particular to an extraction method of atractylodes macrocephala polysaccharide.
Background
At present, the extraction method of the atractylodes macrocephala polysaccharide mainly comprises a hot water extraction method, an enzyme method, a microwave-assisted extraction method, a supercritical extraction method and an ultrasonic-assisted extraction method. The most used extraction method among them is the hot water extraction method.
Root of Yuan Hai Mei[1]The method adopts orthogonal test optimization design and water extraction and alcohol precipitationExtracting to obtain crude polysaccharide of rhizoma Atractylodis Macrocephalae.
The polysaccharide iron complex is generally synthesized by preparing refined polysaccharide into aqueous solution with a certain concentration, adding trisodium citrate, uniformly mixing, adding ferric trichloride, controlling the pH value to be about 8.0, reacting for a period of time, filtering, taking supernatant, precipitating with ethanol to obtain an ethanol precipitate, dialyzing with running water, and freeze-drying to obtain the polysaccharide iron complex. Zhao Peng (Zhao Peng)[2]The iron (III) complex of the limonium bicolor polysaccharide is prepared by the method, and the hydroxyl and iron ions in the polysaccharide are found to be coordinated, so that the thermal stability of the complex product is better.
The general method for synthesizing the polysaccharide zinc complex is to prepare the polysaccharide into a certain aqueous solution, then dropwise add a certain amount of metal ion solution, stir and react for a period of time at a certain temperature and pH, then add ethanol solution to obtain an alcohol precipitate, and freeze-dry the alcohol precipitate to obtain the product. Hair heel year[3]The zinc complex of the manno-oligosaccharide is prepared by the method, and the characterization of the complex shows that the part of the manno-oligosaccharide, which is combined with zinc ions, is on a hydroxyl group.
Grandson macro[4]And synthesizing the chitosan copper (II) complex. The synthesis process of the complex comprises the following steps: adding a small amount of glacial acetic acid into a certain amount of water, then dropwise adding a proper amount of chitosan solution, reacting for 3 hours at 40 ℃, adding 1% of sodium hydroxide until the solution is neutral, washing formed blue precipitates with deionized water and 95% of ethanol respectively, and drying at 60 ℃ to obtain a complex product.
In the prior art, the synthesis of metal polysaccharide complexes is generally to obtain refined polysaccharides by leaching raw materials, and then to chelate with specific metal ions under proper conditions to obtain polysaccharide metal complexes; wherein the refined polysaccharide is obtained by hot water extraction and separation purification; the hot water extraction method usually requires high extraction temperature and more extraction times, so that the energy loss in production is large, the preparation process of the complex is complex, and the energy loss in production is increased.
Although there are some researches on the synthesis of polysaccharide metal complex, no report is found in the literature on the synthesis and preparation process of polysaccharide metal complex of Atractylodes macrocephala.
Reference documents:
[1] yuan Hai Mei, Li hong Xiang and Peng Teng, orthogonal test method prefers the extraction process of rhizoma Atractylodis Macrocephalae polysaccharide, university of Chengdu university (Nature science edition), 2015(03), page 217-;
[2] zhao Peng et al, synthesis and adsorption kinetics of Limonium bicolor polysaccharide iron (III) complex, chemical engineering 2014(11) pp 6-9;
[3] haorennia et al, preparation technology of zinc mannooligosaccharide complex, food research and development, 2010(03), pages 1-4;
[4] sunwhong, Zhang and Guangdong, chitosan copper (II) complex catalytic oxidation of rhodamine B in water printing and dyeing auxiliary agent 2016(09) pages 45-48.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide the method for extracting the atractylodes macrocephala koidz polysaccharide, which has the advantages of low process difficulty, milder extraction conditions, higher yield and better retention of the biological activity of the atractylodes macrocephala koidz polysaccharide.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for extracting atractylis ovata polysaccharide comprises the following steps:
(1) taking powder of dry rhizoma atractylodis macrocephalae roots or/and stems, adding distilled water with the temperature of more than 85 ℃ for extraction to obtain an extract, and then adjusting the temperature of the extract to 30-80 ℃;
(2) adding distilled water into the leaching liquor obtained in the step (1), adding a sulfate solution, adjusting the pH value to 3-8, reacting for 0.5-3.0h, and filtering to obtain a first extracting solution and filter residues;
(3) and (3) repeatedly extracting the obtained filter residue at least once according to the steps (1) and (2) to obtain multiple extracting solutions, combining the multiple extracting solutions, evaporating and concentrating, adding absolute ethyl alcohol, standing overnight, filtering to obtain a precipitate, washing and drying the precipitate to obtain a crude product of the atractylenovata polysaccharide chelated with metal ions. Among them, in the step (1), distilled water at 90 ℃ or higher is preferable for extraction.
Preferably, in the step (2), the mass ratio of the added distilled water volume to the white atractylodes rhizome powder is 5-30 ml: 1g of the total weight of the composition.
Preferably, in the step (2), the mass ratio of the added distilled water volume to the white atractylodes rhizome powder is 10 ml: 1g of the total weight of the composition. Through a plurality of experiments, the inventor of the application finds that the mass ratio of the distilled water volume to the white atractylodes rhizome powder is 10 ml: the dissolution rate of the atractylodes macrocephala polysaccharide is the best when 1g is used. It should be noted that the dissolution rate in the present application refers to the yield of the water-soluble polysaccharide.
Preferably, the sulfate in the step (2) is at least one of zinc sulfate, copper sulfate and ferrous sulfate. More preferably, the sulfate in step (2) is ferrous sulfate, and the inventors of the present application found through many experiments that the dissolution rate of the atractylodes macrocephala polysaccharide is higher when the sulfate in step (2) is ferrous sulfate.
Preferably, the amount of the absolute ethyl alcohol added in the step (3) is 4 times of the volume of the evaporation concentrated solution of the two extracting solutions.
Preferably, the powder in the step (1) is filtered through a 60-mesh 250-micron molecular sieve, and then distilled water is added.
Preferably, the pH value in the step (2) is 4-5. Through multiple experiments, the inventor of the present application finds that the dissolution rate of the atractylodes macrocephala polysaccharide is better when the PH value is 4 or 5 in the step (2).
Preferably, the temperature in the step (1) is adjusted to 60-70 ℃. Through a plurality of experiments, the inventor of the present application finds that the dissolution rate of the atractylodes macrocephala polysaccharide is better when the temperature in the step (1) is adjusted to 60 ℃ or 70 ℃.
Preferably, the reaction time in the step (2) is 1 h. Through multiple experiments, the inventor of the present application finds that the dissolution rate of the atractylodes macrocephala polysaccharide is better when the reaction time in the step (2) is 1 h.
Preferably, in the step (2), the pH value is 4.5, and the mass ratio of the added distilled water volume to the white atractylodes rhizome powder is 8 ml: 1g, the sulfate is copper sulfate. Through a plurality of experiments, the inventor of the application finds that when the pH value in the step (2) is 4.5, the mass ratio of the added distilled water volume to the white atractylodes rhizome powder is 8 ml: 1g, when the sulfate is copper sulfate, the dissolution rate of the atractylodes macrocephala polysaccharide is optimal.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention applies the chelation extraction technology in the mining technology to the extraction of polysaccharide in plants, which is different from the traditional technology that: in the traditional process, a chelating agent is used for assisting in extracting metal ions in ores, and the metal ions are used for chelating polysaccharide to promote the extraction efficiency of the polysaccharide in plants;
2. the process can directly obtain the polysaccharide microelement chelate by only one step, avoids energy and water waste in the processes of heating, extracting, separating, purifying, drying and heating for chelation from the process, and also reduces the environmental pollution; the product competitiveness is improved;
3. the prepared white atractylodes rhizome polysaccharide microelement chelate not only can efficiently supplement microelements, but also can supplement biological immune active substance polysaccharide.
Detailed Description
The trace element complex has the characteristics of high biological value, safety and the like, and the product obtained by the process is used as a feed additive, so that on one hand, the product can supplement necessary immune bioactive substances for animals, and simultaneously can efficiently supplement trace elements, thereby greatly reducing the addition of trace elements (Fe, Cu, Zn and the like) in the feed, reducing the material-weight ratio, reducing the feed cost, reducing the consumption of mineral resources, simultaneously reducing the residue of the trace elements in meat food, reducing the content of the trace elements in animal excrement, and further reducing the pollution of the breeding industry to the environment. Therefore, the invention develops a new process, relates to an extraction method of the bighead atractylodes rhizome polysaccharide metal complex, can be used for ensuring the safety of meat products, protecting the environment and saving resources, and simultaneously reduces the feed cost, increases the income of farmers and promotes the richness of farmers.
The chelation extraction process disclosed by the invention utilizes the fact that microelements (copper, iron and zinc) and polysaccharide can be complexed to form a stable chelate, and can form a synergistic effect on the extraction of the polysaccharide in plant raw materials, so that the difficulty of the polysaccharide extraction process is reduced, the extraction conditions are milder, the yield is higher, the intermediate links of the preparation of the polysaccharide metal complex are reduced, the polysaccharide extraction process of hot water extraction for a long time is not needed, and the biological activity of the atractylodes macrocephala polysaccharide can be greatly maintained.
The extraction method of the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry rhizoma atractylodis macrocephalae powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at the temperature of more than 85 ℃ for 1h, adjusting the temperature to reaction temperature (30-80 ℃), adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the rhizoma atractylodis macrocephalae sample to the volume of the distilled water: 1/5-1/30), immediately adding a certain volume (0-40ml) of 0.5mol/L sulfate (zinc sulfate, copper sulfate or ferrous sulfate) solution, adjusting the pH value (3-8) for a certain period of time (0.5-3.0h), filtering, and preserving the extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution after rotary evaporation and concentration, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain the crude product of the atractylis ovata polysaccharide metal complex.
In the process of leaching the atractylodes macrocephala polysaccharide by hot water, factors such as the amount of added metal ions, reaction temperature, reaction time, material-liquid ratio, pH value and the like are controlled, the polysaccharide dissolution rate is calculated by using a phenol-sulfuric acid method through single-factor and orthogonal test optimization, and the metal content in the obtained metal complex is measured by an ETDA titration method, so that the optimal test condition for synthesizing the atractylodes macrocephala polysaccharide chelate in one step is determined.
The invention also relates to the determination of a glucose standard curve, the determination of a calculation formula of the polysaccharide dissolution rate, the determination of the metal content in the complex, a single-factor optimization test and an orthogonal optimization test, which are respectively introduced as follows:
(1) determination of the glucose Standard Curve
And (3) determining the polysaccharide content by adopting a phenol-sulfuric acid method. Precisely weighing 0.200g of glucose standard product dried to constant weight at 105 ℃, dissolving and dissolving in a 100ml volumetric flask to prepare 2mg/ml glucose mother liquor for later use. Then 0, 0.25ml, 0.5ml, 0.75ml, 1.0ml, 1.25ml, 1.5ml, 1.75ml and 2.0ml are respectively sucked and put into a 50ml volumetric flask for constant volume. Adding 1ml of 6% phenol solution into 1ml of each, rapidly adding 5ml of concentrated sulfuric acid, mixing, standing for 5min, heating in 85 deg.C water bath for 20min, taking out, cooling to room temperature, and measuring absorbance at 490 nm. And determining a glucose standard curve regression equation of each test group by taking the glucose mass concentration c (mg/ml) as an abscissa X and the absorbance A (abs) as an ordinate Y.
(2) Measuring the absorbance of the sample to calculate the polysaccharide dissolution rate
Taking 0.100g of sample and fixing the volume in a 100ml volumetric flask to obtain 1mg/ml sample mother solution. 2ml of sample mother liquor is taken to be put into a 50ml volumetric flask for constant volume, and 0.04mg/ml of sample solution is obtained. 1ml of sample solution is taken, 1ml of 6% phenol is added, 5ml of concentrated sulfuric acid is rapidly added, and the mixture is uniformly mixed. And standing for 5 minutes. And heating in 85 deg.C water bath for 20min, cooling to room temperature, and measuring absorbance at 490nm to calculate polysaccharide dissolution rate of each test group.
2.1 regression equation for each test set:
test zinc group: y is 10.21x +0.011, R2 is 0.997;
test copper group: y is 10.53x +0.006, R2 is 0.999;
test iron group: y is 10.63x-0.011, and R2 is 0.999;
note: test zinc group: adding a zinc sulfate solution into the white atractylodes rhizome polysaccharide extraction process for a co-heating reaction group;
test copper group: adding a copper sulfate solution in the process of extracting the atractylodes macrocephala polysaccharide to carry out a co-heating reaction group;
test iron group: adding ferrous sulfate solution in the process of extracting the atractylodes macrocephala polysaccharide to carry out a co-heating reaction group.
2.2 the polysaccharide dissolution rate calculation formula of each test group is as follows:
test zinc group polysaccharide dissolution rate [ crude polysaccharide × (a-0.011) × 2500]/(10.21 × 101 × 10);
test copper group polysaccharide dissolution rate [ crude polysaccharide × (a-0.006) × 2500]/(10.53 × 101 × 10);
test iron group polysaccharide dissolution rate [ crude polysaccharide × (a +0.011) × 2500]/(10.63 × 101 × 10);
note: in the formula, A refers to absorbance, 2500 is a dilution multiple, 10 refers to grams of rhizoma atractylodis macrocephalae raw material extracted, and 101 refers to milligrams of crude polysaccharide complex extracted when the absorbance is measured.
(3) Determination of the Metal content in the Complex
3.1 iodometry determination of copper ion content
Weighing 0.4g of sample (weighed to 0.0002g), placing the sample in a 250ml iodine measuring flask, adding 50ml of water for dissolving, adding 4ml of glacial acetic acid and 2g of potassium iodide for shaking up, placing the sample in a dark place for 10min, titrating the mixture to be light yellow by using a sodium thiosulfate standard solution (0.1mol/L), adding 2ml of starch solution, and continuously titrating until blue just disappears to obtain the end point.
The percentage of copper, X1, is calculated according to formula (a):
X1＝0.06355×C1×V1/M1 (a)
in the formula: c1 is the mol/L of the molar concentration of the sodium thiosulfate standard solution;
v1 is the volume ml of sodium thiosulfate standard solution consumed in titration;
0.06355 is the mass in grams per millimole of copper;
m1 is sample mass g.
3.2EDTA titration method for determining the content of Zinc ions
Weighing 0.100g of sample, adding 30ml of deionized water to dissolve the sample, adding 5% NaOH until precipitation just occurs, adding 20ml of acetic acid-sodium acetate buffer solution with pH5.5, adding 2 drops of xylenol orange, and titrating the solution by using EDTA standard solution (0.013mol/L) from wine red to bright yellow as an end point.
The percentage of zinc, X2, is calculated according to formula (b):
X2＝0.065×C2×V2/M2 (b)
in the formula: c2 is the molar concentration mol/L of the EDTA standard solution;
v2 is the volume ml of EDTA standard solution consumed in titration;
0.065 is mass grams per millimole of zinc;
m2 is sample mass g.
3.3EDTA titration method for determining the content of iron ions and ferrous ions
Weighing 0.100g of sample, placing the sample in a 250ml volumetric flask, adding 40ml of deionized water for dissolution, adjusting the pH to 1.8-2.5, adding 10 drops of sulfosalicylic acid (100g/L) as an indicator, titrating ferric ions by using EDTA (0.0109mol/L) until the bright yellow with stable purple red color is the titration end point, and recording the consumption volume of the EDTA.
Adding concentrated nitric acid 5ml, heating for 5min, cooling to convert ferrous iron ion into ferric iron ion, adjusting pH to 1.8-2.5 to make the solution turn to mauve, titrating ferric iron ion with EDTA until the color changes from mauve to bright yellow, and recording the volume consumed by EDTA.
The percentage of iron, X3, is calculated according to formula (c):
X3＝0.065×C3×V3/M3 (c)
(4) one factor optimization
4.1 determination of the optimum sulfate volumetric addition
Adding 0.5mol/L sulfate with different volumes (0-40ml) into the extract according to the ratio of material to liquid (the ratio of the mass of the rhizoma atractylodis macrocephalae sample to the volume of distilled water) of 1g/10ml, reacting for 1h at the temperature of 60 ℃ and the pH value of the extract, measuring the absorbance of polysaccharide by a phenol-sulfuric acid method at 490nm, and calculating the dissolution rate of the polysaccharide. Test results show that when the addition amount of sulfate in the zinc group, the copper group and the iron group is respectively 16ml, 4ml and 12ml, the dissolution rates of polysaccharide are optimal and respectively 31.51%, 33.30% and 35.62%.
4.2 determination of optimum reaction pH
After the adding amount of the zinc, copper and ferrous ion solution is determined, the pH value is adjusted to 3-8, the material-liquid ratio is 1/10, and the extraction is carried out for 1h at 60 ℃. Tests show that the dissolution rates of polysaccharide are respectively 33.24%, 28.56% and 40.70% when the pH values of the zinc group, the copper group and the iron group are respectively 5, 4 and 5.
4.3 determination of optimum reaction temperature
After the adding amount and the pH value of the ionic solution of the test groups of zinc, copper and iron are determined, the extraction temperature is adjusted to be between 30 and 80 ℃, and the extraction is carried out for 1 hour under the condition of the reference solution ratio of 1/10. The test shows that the dissolution rates of the polysaccharide are respectively 32.61%, 35.33% and 35.20% when the temperature of the zinc group, the copper group and the iron group is respectively 60 ℃, 70 ℃ and 60 ℃.
4.4 determination of optimum reaction time
After the adding amount, the pH value and the reaction temperature of ionic solutions of test groups of zinc, copper and iron are determined, the ionic solutions are extracted for a period of time (0.5-3.0h) under the condition of a feed-liquid ratio of 1/10, and when the extraction time of the test groups of zinc, copper and iron is 1h, the polysaccharide dissolution rates are the best and are respectively 30.45%, 33.27% and 35.20%.
4.5 determination of optimum feed-to-liquid ratio
After the adding amount, the pH value, the reaction temperature and the reaction time of ionic solutions of a zinc test group, a copper test group and an iron test group are determined, extracting for 1h under a certain material-liquid ratio (1/5-1/30), wherein when the material-liquid ratio of the zinc test group, the copper test group and the iron test group is 1/10, the polysaccharide dissolution rates are the best, and are respectively 32.04%, 29.49% and 35.20%.
5. Quadrature optimization
According to the result of the single-factor test, the ZnSO is selected from the zinc test group4Volume (10-30ml), pH (4-6) and feed-liquid ratio (1/5-1/15), CuSO is selected from copper test group4Volume (10-30ml), pH (4-6) and feed-liquid ratio (1/5-1/15), and FeSO is selected from iron test group4Orthogonal tests are carried out by three factors of volume (10-30ml), temperature (45-65 ℃) and time (0.5-2.5 h).
Testing of zinc group in ZnSO4The volume addition amount is 16ml, the pH value is 5.0, the polysaccharide dissolution rate is the best when the material-liquid ratio is 1/12, the polysaccharide dissolution rate is 30.55%, and the percentage content of zinc ions is 9.49% when 0.101g of product is taken.
Test copper group in CuSO4The volume addition amount is 5ml, the pH is 4.5, and the polysaccharide dissolution rate is 41.26% when the material-liquid ratio is 1/8. The percentage of copper ions was found to be 2.44% with 0.401g of product.
Test of iron group in FeSO4The volume addition amount is 10ml, the temperature is 55 ℃, and the polysaccharide dissolution rate is 36.02% when the time is 0.75 h. Taking 0.102g of the product, the percentage content of iron ions was found to be 6.11%.
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 85 ℃ for 1h, adjusting the temperature to 30 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the bighead atractylodes rhizome sample to the volume of the distilled water: 1g:5ml), immediately adding 4ml of 0.5mol/L zinc sulfate solution, adjusting the pH value to 3, carrying out co-reaction for 0.5h, filtering, and storing an extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume being 3.5 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 17.42%.
Example 2
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 87 ℃ for 1h, adjusting the temperature to 50 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the bighead atractylodes rhizome sample to the volume of the distilled water: 1g:15ml), immediately adding 16ml of 0.5mol/L copper sulfate solution, adjusting the pH value to 4, reacting for 1.5h, filtering, and storing an extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 24.35%.
Example 3
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 90 ℃ for 1h, adjusting the temperature to 70 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the bighead atractylodes rhizome sample to the volume of the distilled water: 1g:10ml), immediately adding 12ml of 0.5mol/L ferrous sulfate solution, adjusting the pH value to 5, reacting for 1h, filtering, and storing an extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 29.57%.
Example 4
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 92 ℃ for 1h, adjusting the temperature to 60 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the bighead atractylodes rhizome sample to the volume of the distilled water: 1g:25ml), immediately adding 25ml of 0.5mol/L copper sulfate solution, adjusting the pH value to 6, reacting for 2.5h, filtering, and storing an extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume 4.5 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 18.21%.
Example 5
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 95 ℃ for 1h, adjusting the temperature to 80 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the bighead atractylodes rhizome sample to the volume of the distilled water: 1g:30ml), immediately adding 40ml of 0.5mol/L zinc sulfate solution, adjusting the pH value to 8, reacting for 3.0h, filtering, and storing an extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 22.32%.
Example 6
One embodiment of the method for extracting the atractylodes macrocephala polysaccharide comprises the following steps:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use; weighing 10g of dry rhizoma atractylodis macrocephalae powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 90 ℃ for 1h, adjusting the temperature to 50 ℃, adding distilled water according to a certain material-liquid ratio (the ratio of the mass of the rhizoma atractylodis macrocephalae sample to the volume of the distilled water: 1g:8ml), immediately adding 5ml of 0.5mol/L copper sulfate solution, adjusting the pH value to 4.5, jointly reacting for 1.5h, filtering, and preserving the extracting solution. And then, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained twice, performing rotary evaporation and concentration, adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution, standing overnight in a refrigerator at 4 ℃, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude product of the white atractylodes rhizome polysaccharide metal complex, wherein the dissolution rate of the white atractylodes rhizome polysaccharide is 39.28%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (1)
1. The method for extracting the atractylodes macrocephala polysaccharide is characterized by comprising the following steps of:
crushing a bighead atractylodes rhizome sample by using a universal crusher, sieving the powder by using a 60-mesh 250-micron molecular sieve, and drying the powder for 24 hours at 60 ℃ for later use;
weighing 10g of dry bighead atractylodes rhizome powder, quickly adding 100.0ml of distilled water, carrying out magnetic stirring leaching in hot water at 90 ℃ for 1h, adjusting the temperature to 50 ℃, adding distilled water according to a certain material-liquid ratio, immediately adding 5ml of 0.5mol/L copper sulfate solution, adjusting the pH value to 4.5, carrying out co-reaction for 1.5h, filtering, storing an extracting solution, repeatedly extracting the obtained filter residue once according to the operation, combining the extracting solutions obtained in two times, carrying out rotary evaporation concentration, adding absolute ethyl alcohol with 4 times volume of the concentrated solution, standing in a refrigerator at 4 ℃ for overnight, filtering, washing the collected precipitate with absolute ethyl alcohol and acetone, and drying at 60 ℃ to obtain a crude bighead atractylodes rhizome polysaccharide metal complex product;
wherein the feed-liquid ratio is the ratio of the mass of the rhizoma atractylodis macrocephalae sample to the volume of distilled water of 1g to 8 ml.
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