CN113827645A - Method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra and application thereof - Google Patents
Method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra and application thereof Download PDFInfo
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- CN113827645A CN113827645A CN202111173349.1A CN202111173349A CN113827645A CN 113827645 A CN113827645 A CN 113827645A CN 202111173349 A CN202111173349 A CN 202111173349A CN 113827645 A CN113827645 A CN 113827645A
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- 235000008422 Schisandra chinensis Nutrition 0.000 title claims abstract description 124
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 66
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 66
- 241000736075 Schisandra Species 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 56
- 229930182490 saponin Natural products 0.000 title claims abstract description 56
- 150000007949 saponins Chemical class 0.000 title claims abstract description 56
- 235000017709 saponins Nutrition 0.000 title claims abstract description 56
- 229930013686 lignan Natural products 0.000 title claims abstract description 46
- 235000009408 lignans Nutrition 0.000 title claims abstract description 46
- 150000005692 lignans Chemical class 0.000 title claims abstract description 46
- 150000004676 glycans Chemical class 0.000 title claims abstract 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 243
- 238000000605 extraction Methods 0.000 claims abstract description 111
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 240000006079 Schisandra chinensis Species 0.000 claims abstract description 65
- 239000000284 extract Substances 0.000 claims abstract description 35
- 238000005406 washing Methods 0.000 claims abstract description 31
- 238000000746 purification Methods 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 238000000502 dialysis Methods 0.000 claims abstract description 13
- 238000003809 water extraction Methods 0.000 claims abstract description 11
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 10
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 10
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 48
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 46
- 239000007864 aqueous solution Substances 0.000 claims description 39
- 239000000706 filtrate Substances 0.000 claims description 34
- 239000003208 petroleum Substances 0.000 claims description 32
- 239000002244 precipitate Substances 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 14
- 238000010828 elution Methods 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000006210 lotion Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000013049 sediment Substances 0.000 claims description 10
- 239000012259 ether extract Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229940046892 lead acetate Drugs 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000004375 Dextrin Substances 0.000 claims description 5
- 229920001353 Dextrin Polymers 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 235000019425 dextrin Nutrition 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000000469 ethanolic extract Substances 0.000 claims description 4
- 239000003480 eluent Substances 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 2
- 238000012958 reprocessing Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 7
- 239000008367 deionised water Substances 0.000 abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 85
- 150000004804 polysaccharides Chemical class 0.000 description 46
- 238000010992 reflux Methods 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- ZWRRJEICIPUPHZ-UHFFFAOYSA-N schisandrol B Natural products COC1=C2C=3C(OC)=C(OC)C(OC)=CC=3CC(C)(O)C(C)CC2=CC2=C1OCO2 ZWRRJEICIPUPHZ-UHFFFAOYSA-N 0.000 description 3
- YEFOAORQXAOVJQ-RZFZLAGVSA-N schisandrol a Chemical compound C1[C@H](C)[C@@](C)(O)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC YEFOAORQXAOVJQ-RZFZLAGVSA-N 0.000 description 3
- XDVOVYYAPHHHBE-YGIMCSHQSA-N schizantherin b Chemical compound C[C@@H]/1[C@](C)(O)[C@@H](OC(=O)C(\C)=C/C)C2=CC(OC)=C(OC)C(OC)=C2[C@H]2C(OC)=C(OCO3)C3=C\C2=C\1 XDVOVYYAPHHHBE-YGIMCSHQSA-N 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- YEFOAORQXAOVJQ-UHFFFAOYSA-N wuweizischun A Natural products C1C(C)C(C)(O)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC YEFOAORQXAOVJQ-UHFFFAOYSA-N 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 241001506304 Kadsura japonica Species 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229920001284 acidic polysaccharide Polymers 0.000 description 2
- 150000004805 acidic polysaccharides Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- GUBGYTABKSRVRQ-WFVLMXAXSA-N DEAE-cellulose Chemical compound OC1C(O)C(O)C(CO)O[C@H]1O[C@@H]1C(CO)OC(O)C(O)C1O GUBGYTABKSRVRQ-WFVLMXAXSA-N 0.000 description 1
- 206010067125 Liver injury Diseases 0.000 description 1
- 241000218377 Magnoliaceae Species 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 241000736078 Schisandra sphenanthera Species 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000000658 coextraction Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- HWJHWSBFPPPIPD-UHFFFAOYSA-N ethoxyethane;propan-2-one Chemical compound CC(C)=O.CCOCC HWJHWSBFPPPIPD-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 231100000753 hepatic injury Toxicity 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/79—Schisandraceae (Schisandra family)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/57—Magnoliaceae (Magnolia family)
-
- 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
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Mycology (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
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- Materials Engineering (AREA)
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Abstract
The invention discloses a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra and application thereof. According to the invention, the ammonium sulfate solution is added into the crude schisandra chinensis polysaccharide obtained by water extraction and alcohol precipitation, so that macromolecular impurities such as protein and the like can be effectively removed, and the centrifuged supernatant is dialyzed in deionized water by using a dialysis bag to remove the micromolecular impurities, so that high-purity schisandra chinensis polysaccharide is obtained; the supernatant obtained by water extraction and alcohol precipitation and the alcohol extract are combined, subjected to alcohol removal and then loaded onto macroporous resin, washed by water and then eluted by low-concentration ethanol, so that non-target components can be effectively removed, the content of the target components obtained by alcohol washing is further improved, and a mixture of lignans and total saponins with higher content can be obtained after macroporous resin purification, thereby facilitating subsequent purification; the method has the advantages of high resource utilization, high extraction efficiency and wide application prospect.
Description
Technical Field
The invention relates to the technical field of extraction of plant effective components, and in particular relates to a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra and application thereof.
Background
Fructus Schisandrae is dried mature fruit of Schisandra chinensis of Magnoliaceae, and is divided into Schisandra chinensis Baill and Schisandra sphenanthera Baill; the main producing areas of the schisandra chinensis are northeast areas, inner Mongolia, Hebei, Shanxi and the like, and the schisandra chinensis is planted in southern provinces of Yangtze river basin.
Fructus Schisandrae chinensis has wide pharmacological action, and has effects of resisting liver injury, inhibiting central nervous system, tonifying heart, enhancing immunity, and resisting bacteria, and its main chemical components include fructus Schisandrae chinensis total lignanoid, polysaccharide, saponins, vitamin C and tannin.
In the prior art, the extraction method of the schisandra total lignans comprises a solvent extraction method, a reflux extraction method, an ultrasonic extraction method and supercritical CO2An extraction method; wherein the solvent extraction method and reflux extraction method are more traditional methods, although the requirement on equipment is not high, the method has the defects of long extraction time, solvent consumption and the like, and the ultrasonic extraction method and the supercritical CO extraction method2The extraction method, as a new extraction technology, can accelerate the dissolution of effective components, has short extraction time and low extraction temperature, can protect the effective components from being damaged, but has expensive equipment and is not suitable for large-scale industrial production.
Chinese patent application with publication number CN107126460A discloses a method for preparing total lignans from fructus Schisandrae, which comprises pulverizing fructus Schisandrae, extracting with ethanol, concentrating, performing macroporous resin column chromatography, washing with ethanol solutions of different concentrations, concentrating to obtain extract, dissolving the extract with methanol, mixing with silica gel, stirring, dispersing, drying, adding into chromatographic column filled with silica gel, washing with petroleum ether-acetone mixture, collecting eluate, and concentrating to obtain total lignans.
Chinese patent application with publication number CN101757111A discloses a method for preparing total lignans from fructus Schisandrae, which comprises pulverizing fructus Schisandrae, extracting with ethanol, adding active carbon into the extractive solution, stirring, decolorizing, loading on silica gel column, eluting with chloroform/methanol mixed solution, crystallizing the eluate with acetone, and drying to obtain the final product.
The Chinese patent application with publication number CN108676176A discloses a preparation method of lignans from Kadsura japonica, which comprises extracting Kadsura japonica with ethanol, concentrating to obtain extract, sequentially extracting with petroleum ether, ethyl acetate and n-butanol, removing large polar substances with macroporous resin, and performing silica gel column chromatography to obtain lignans.
Chinese patent application with publication number CN108083992A discloses a simple method for extracting and separating schizandrol A and schizandrol B, which comprises leaching raw materials to obtain schizandrol A and schizandrol B, mixing with polyamide, and separating with polyamide chromatographic column to obtain schizandrol A and schizandrol B monomeric compounds.
In conclusion, the extraction of the total lignans of the schisandra chinensis is mostly performed by ethanol extraction, the method is simple and easy to implement, but the components in the extracting solution are complex, and the subsequent purification process is complicated; in addition, there is a method of leaching with acetone, ethyl acetate and dichloromethane as solvents, which can reduce the extraction of impurities, but such solvents are highly hazardous and are not suitable for use in large quantities in industrial production.
In the prior art, the extraction of schisandra chinensis polysaccharide mostly uses water as a solvent for extraction, and then different means are used for purification to obtain a target product.
Chinese patent application with publication number CN107163157A discloses a schisandra acidic polysaccharide and its preparation method and application, wherein the raw materials are extracted with water, then concentrated and precipitated with alcohol to obtain total polysaccharide, the total polysaccharide is dissolved and then put on DEAE-cellulose column, and sodium chloride is eluted to obtain acidic polysaccharide; the method is generally used in laboratories, and large-scale production is difficult to carry out.
Chinese patent application with publication number CN109651522A discloses a method for preparing schisandra chinensis polysaccharide, which comprises adding absolute ethyl alcohol into raw materials for degreasing, drying the raw materials, then extracting with water, precipitating the water extract with alcohol to obtain crude schisandra chinensis polysaccharide; the method has no subsequent operation after alcohol precipitation, and the obtained product has no better purity.
The Chinese patent application with publication number CN102492050A discloses a preparation method of active ingredient polysaccharide in schisandra chinensis dregs, and specifically discloses a method for extracting the dregs by water, precipitating by alcohol, dissolving the precipitate by water, freezing and thawing, centrifuging to obtain clear liquid, classifying by ethanol, centrifuging to obtain the precipitate, dissolving the precipitate by water, performing enzymolysis by using chain protease, deproteinizing by a Sevag method, and freeze-drying to obtain polysaccharide; the polysaccharide obtained by the method has high purity, but easily causes harmful solvent residue.
In the prior art, the extraction and purification method of the total saponins of schisandra chinensis is conventionally that water or organic solvent is used for extraction, the extract is purified by weak polar resin, and then water saturated n-butanol is used for further refining to obtain the total saponins with higher purity.
Chinese patent application with publication number CN102028754A discloses a method for rapidly preparing total lignans and total saponins from fructus Schisandrae, which comprises pulverizing fructus Schisandrae (fruit pulp), stem and carpopodium of Chinese medicinal materials, adding methanol or high-alcohol, performing flash extraction at low temperature (room temperature), and subjecting the extract to macroporous resin chromatography and extraction to obtain total saponins with content of above 50%; however, the method for obtaining the schisandra total saponins and the total lignans can not realize better separation and has no higher yield.
So far, no relevant reports about a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins in schisandra are found.
In view of this, the invention is particularly proposed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for comprehensively extracting fructus Schisandrae polysaccharide, fructus Schisandrae total lignanoid and fructus Schisandrae total saponin from fructus Schisandrae comprises,
s1, water extraction
Adding powdered fructus Schisandrae chinensis raw material into water, heating for extraction, performing solid-liquid separation to obtain water extractive solution, and drying the extractive residue at low temperature;
s2, extraction and purification of polysaccharide
Concentrating the water extract to 1.1-1.2 Baume, adding ethanol, controlling ethanol content to 70-80 v%, standing, filtering to obtain a first filtrate containing saponin and a filter cake containing polysaccharide, and post-treating the filter cake to obtain Schisandra chinensis polysaccharide;
s3 flash alcohol extraction
Extracting the extraction residue dried in the step S1 with high-concentration ethanol water solution by adopting a flash extraction method, and filtering to obtain an ethanol extract containing total lignans and total saponins;
s4 extraction and purification of total lignans
Combining the first filtrate obtained in the step S2 with the alcohol extract obtained in the step S3, sequentially carrying out impurity removal treatment, alcohol solution elution and alcohol concentration removal, then extracting with petroleum ether, and reprocessing the petroleum ether extract to obtain the schisandra total lignans;
s5, extraction and purification of total saponins
Purifying the water phase residue obtained after the petroleum ether extraction in the step S4 to obtain total saponins of schisandra chinensis;
wherein the order of step S2 and step S3 may be interchanged.
In the above technical solution, in step S2, the concentration of the ethanol added is 92-98 v%, and the ethanol is added while stirring.
In the above technical solution, in step S2, the standing time is 12-20h, and more preferably at 3-8 ℃ for 12-15 h.
Further, in the above technical solution, in step S2, the post-processing includes,
washing the filter cake with anhydrous ethanol at a temperature lower than 35 deg.C to obtain crude polysaccharide of fructus Schisandrae chinensis, re-dissolving with water, centrifuging to remove insoluble substances, adding ammonium sulfate until saturation, standing, centrifuging to remove protein, collecting supernatant, dialyzing to obtain polysaccharide extractive solution, and concentrating and drying to obtain fructus Schisandrae chinensis polysaccharide.
In a specific embodiment of the present invention, the number of times of adding the ammonium sulfate and centrifuging to remove the protein is 3 to 5 times in step S2.
In the embodiment of the present invention, in step S2, the dialysis is specifically performed by subjecting the supernatant to dialysis with a dialysis bag having a molecular weight cut-off of 5000-.
In a specific embodiment of the present invention, in step S2, the dialysis temperature and time are 2-10 deg.C and 48-120h, respectively.
In the above technical solution, in step S3, the concentration of the ethanol aqueous solution is 75-85 v%.
In a preferred embodiment of the present invention, in step S3, the concentration of the ethanol aqueous solution is 78-82 v%.
In the above technical solution, in step S3, the ethanol aqueous solution is added in an amount that the feed-liquid ratio is controlled to be 1 g: 5-50 ml.
In the above technical solution, in step S3, the temperature and time of the extraction are 20-50 ℃ and 5-10min, respectively.
In the above technical solution, in step S3, the number of times of extraction is 2-3, and after extraction and filtration, the alcohol extract is obtained by combining them.
In the above technical solution, in step S1, the amount of the powdered schisandra raw material added into water is controlled to be 1 g: 5-50 ml.
In the above technical solution, in step S1, the temperature and time of the heating extraction are 80-100 ℃ and 30-120min, respectively.
In the above technical solution, in step S1, the number of times of the heating extraction is 2-3, and after the heating extraction, the heating extraction and the combination are performed to obtain the water extract.
Still further, in the above technical scheme, in step S4, the impurity removal process includes recovering ethanol, diluting with water, purifying with a macroporous resin column, and eluting with water and 10-30 v% ethanol aqueous solution in sequence to remove impurities.
Still further, in the above technical solution, in step S4, the alcohol solution is specifically eluted by 60-95 v% aqueous ethanol solution, and the eluate is collected.
Further, in the above technical solution, in step S4, the petroleum ether extraction specifically includes transferring the concentrated and dealcoholized eluate to a separating funnel, adding an equal volume of petroleum ether, shaking sufficiently, standing for layering, separating an aqueous layer and a petroleum ether layer, and preferably repeating for 3 times to extract sufficiently.
Further, in the above technical solution, in step S4, the petroleum ether extract is further processed by adding white dextrin to the petroleum ether extract, and concentrating and drying under reduced pressure.
In the embodiment of the present invention, in the step S4, the volume multiple of the mixture diluted with water is 2 to 10 times in the impurity removing process.
In a specific embodiment of the present invention, in step S4, the macroporous resin column is one of LX-60 type, LX-T28 type, LX-T81 type and LX-T91 type macroporous resin columns.
In the specific embodiment of the present invention, in the step S4, the loading flow rate of the macroporous resin column is 0.5-2.0 BV/h.
In a specific embodiment of the present invention, in step S4, the elution flow rates of the 10-30 v% ethanol aqueous solution and the 60-95 v% ethanol aqueous solution are both 1.0-3.0 BV/h.
In a specific embodiment of the present invention, in step S4, the elution volumes of the water, the 10-30 v% aqueous ethanol solution, and the 60-95 v% aqueous ethanol solution are all 3-6 BV.
Still further, in the above technical solution, in the step S5, the purification process includes adding a neutral lead acetate solution to the aqueous phase residue until no precipitate is formed, filtering, washing the precipitate with ice water for 2-3 times, completely dissolving the washed precipitate with a 90-98 v% aqueous ethanol solution, and introducing an excess amount of H2Performing double decomposition on S gas to generate PbS sediment, filtering the sediment to obtain a second filtrate, washing the PbS sediment by using 90-98 v% ethanol water solution to obtain PbS lotion, finally combining the second filtrate and the PbS lotion, adding activated carbon to decolor, and sequentially filtering, concentrating and drying to obtain the PbS washing lotion.
In a preferred embodiment of the present invention, in step S5, the lead acetate solution is a 20-30 wt% aqueous solution of lead acetate as it is being prepared.
In another preferred embodiment of the present invention, in step S5, the 90-98 v% ethanol aqueous solution dissolving the precipitate has a mass 30-50 times as large as the mass of the precipitate.
In still another preferred embodiment of the present invention, in step S5, the amount of the activated carbon is 0.01 to 0.05 times the mass of the sum of the second filtrate and the PbS washing solution.
The invention also provides the application of the method in comprehensively extracting schisandra polysaccharide, schisandra total lignanoid and schisandra total saponin in schisandra.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the ammonium sulfate solution is added into the crude schisandra chinensis polysaccharide obtained by water extraction and alcohol precipitation, so that macromolecular impurities such as protein and the like can be effectively removed, and the centrifuged supernatant is dialyzed in deionized water by using a dialysis bag to remove the micromolecular impurities, so that high-purity schisandra chinensis polysaccharide is obtained;
(2) according to the invention, the supernatant obtained by water extraction and alcohol precipitation and the alcohol extract are combined, subjected to alcohol removal and then loaded onto macroporous resin, and washed by water and then eluted by low-concentration ethanol, so that non-target components can be removed to the maximum extent, the content of the target components obtained by alcohol washing is further increased, and a mixture of lignans and total saponins with higher content can be obtained after macroporous resin purification, so that further purification is facilitated;
(3) the method provided by the invention has high resource utilization, can extract and purify various active ingredients in the schisandra chinensis, maximizes the resource utilization and reduces the waste;
(4) the method provided by the invention has high extraction efficiency, can extract effective components in plants within minutes by using a flash extraction technology, has obviously increased extraction efficiency compared with other extraction methods, and has wide practical application prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments.
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the means used are conventional in the art unless otherwise specified.
The terms "comprises," "comprising," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion.
For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The reagents and equipment used in the examples and comparative examples of the present invention were all commercially available products.
Example 1
The embodiment of the invention provides a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra, which specifically comprises the following steps:
s1, water extraction
Weighing 100g of dried and crushed powdered schisandra raw material, performing reflux extraction for 90min at 90 ℃ by using 1000ml of pure water, performing reflux extraction for 60min on filter residues after solid-liquid separation by using 700ml of pure water under the same condition, combining filtrate obtained by two times of reflux extraction to obtain water extract, and drying the extraction residues at 60 ℃ for later use;
s2, extraction and purification of polysaccharide
Concentrating the water extract obtained in the step S1 to 1.2 Baume under reduced pressure, adding 95 v% ethanol, stirring while adding ethanol to enable the ethanol content to reach 75 v%, standing for 12h at 4 ℃, filtering, collecting precipitate and filtrate, respectively obtaining a filter cake containing polysaccharide and a first filtrate containing saponin, washing the filter cake with absolute ethanol at 25 ℃ to obtain crude schisandra chinensis polysaccharide, then redissolving with water, centrifuging to remove insoluble substances, adding ammonium sulfate until the mixture is saturated, standing, centrifuging to remove protein (repeating for 4 times), taking supernatant, putting the supernatant into a dialysis bag with molecular weight cutoff of 5000Da, dialyzing for 60h to obtain polysaccharide extract, concentrating and drying under reduced pressure to obtain 7.58g of schisandra chinensis polysaccharide, and detecting the polysaccharide content to be 85.28 wt% by using an ultraviolet spectrophotometer;
s3 flash alcohol extraction
Extracting the extraction residue dried in the step S1 with high-concentration ethanol aqueous solution by adopting a flash extraction method, wherein the specific conditions are that 80 v% ethanol aqueous solution is used for extracting twice at room temperature, the extraction time is 5min, the dosage of the ethanol aqueous solution is 500ml in the first extraction, the dosage of the ethanol aqueous solution is 300ml in the second extraction, and after the extraction is finished, filtering and combining the filtrate to obtain ethanol extract containing the total lignans and the total saponins;
s4 extraction and purification of total lignans
Combining the first filtrate containing saponin in the step S2 and the alcohol extract in the step S3, recovering ethanol, adding water to dilute to 400ml, loading to an LX-60 type macroporous resin column at a loading flow rate of 1.5BV/h, washing with 5BV water to remove water-soluble impurities, eluting with 4BV ethanol aqueous solution (25 v%) at an elution flow rate of 1.8BV/h to remove other impurities without target components, eluting with 4BV ethanol aqueous solution (93 v%) at an elution flow rate of 2.0BV/h, collecting the eluent, concentrating and recovering ethanol in sequence, transferring to a separating funnel, adding equal volume of petroleum ether, shaking sufficiently, standing for demixing, separating a water layer and a petroleum ether layer, repeatedly adding equal volume of petroleum ether for 3 times for full extraction, then adding 5.00g of white dextrin into the petroleum ether extract, concentrating and drying under reduced pressure to obtain 2.89g of total lignans of schisandra chinensis, detecting total lignanoid content by HPLC method to be 51.97 wt%;
s5, extraction and purification of total saponins
Adding 25 wt% of neutral lead acetate aqueous solution (used as the existing preparation) into the water phase residue after the petroleum ether extraction in the step S4 until no new precipitate is generated, stirring to completely precipitate, filtering, washing the precipitate with ice water for 3 times, discarding filtrate and washing liquid, completely dissolving the washed precipitate with 100ml of 95 v% ethanol aqueous solution, introducing excessive H2Double decomposition of S gas to produce PbSPrecipitating, filtering to remove lead element to obtain a second filtrate, washing PbS precipitate twice with 100ml ethanol water solution (95 v%), collecting PbS lotion, finally combining the second filtrate and PbS lotion, adding 2g powdered activated carbon to decolorize at 55 ℃, filtering, concentrating and drying to obtain 1.98g of total saponins of Schisandra chinensis, and detecting the content of total saponins to 94.28 wt% by using an ultraviolet spectrophotometer.
Example 2
The embodiment of the invention provides a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra, which specifically comprises the following steps:
s1, water extraction
Weighing 1000g of dried and crushed powdered schisandra raw material, performing reflux extraction for 100min at the temperature of 100 ℃ by using 10L of pure water, performing reflux extraction for 60min on filter residues after solid-liquid separation by using 8L of pure water under the same condition, combining filtrate obtained by two times of reflux extraction to obtain water extract, and drying the extraction residues at the temperature of 60 ℃ for later use;
s2, extraction and purification of polysaccharide
Concentrating the water extract obtained in the step S1 under reduced pressure to 1.2 Baume, adding 95 v% ethanol, stirring while adding ethanol to reach 73 v%, standing at 4 ℃ for 12h, filtering, collecting precipitate and filtrate to obtain a filter cake containing polysaccharide and a first filtrate containing saponin, washing the filter cake with 20 ℃ absolute ethanol to obtain crude schisandra chinensis polysaccharide, redissolving with water, centrifuging to remove insoluble substances, adding ammonium sulfate until saturated, standing, centrifuging to remove protein (repeating for 5 times), collecting supernatant, putting into a dialysis bag with cut-off molecular weight of 5000Da, dialyzing for 48h to obtain polysaccharide extract, concentrating under reduced pressure and drying to obtain 75.91g of schisandra chinensis polysaccharide, and detecting the polysaccharide content to be 86.00 wt% by using an ultraviolet spectrophotometer;
s3 flash alcohol extraction
Extracting the extraction residue dried in the step S1 with high-concentration ethanol aqueous solution by adopting a flash extraction method, wherein the specific conditions are that 78 v% ethanol aqueous solution is used for extracting twice at room temperature, the dosage and the extraction time of the ethanol aqueous solution are respectively 4.5L and 6min in the first extraction, the dosage and the extraction time of the ethanol aqueous solution are respectively 3.5L and 4min in the second extraction, filtering after the extraction is finished, and combining the filtrate to obtain ethanol extract containing total lignans and total saponins;
s4 extraction and purification of total lignans
Combining the first filtrate containing saponin in the step S2 with the alcohol extract in the step S3, recovering ethanol, adding water to dilute to 3L, passing through an LX-T28 type macroporous resin column at a sample flow rate of 1.5BV/h, washing with 6BV water to remove water-soluble impurities, eluting with 4BV ethanol aqueous solution (28 v%) at an elution flow rate of 1.8BV/h to remove other impurities without target components, eluting with 4.5BV ethanol aqueous solution (92 v%) at an elution flow rate of 2.0BV/h, collecting the eluate, concentrating and recovering ethanol, transferring to a separating funnel, adding equal volume of petroleum ether, shaking sufficiently, standing for layering, separating a water layer and a petroleum ether layer, repeatedly adding equal volume of petroleum ether for 3 times for sufficient extraction, adding 50.00g of white dextrin into the petroleum ether extract, concentrating and drying under reduced pressure to obtain 29.31g of total lignans of schisandra chinensis, detecting total lignanoid content by HPLC method to be 52.39 wt%;
s5, extraction and purification of total saponins
Adding 25 wt% of neutral lead acetate aqueous solution (used as the existing preparation) into the water phase residue after the petroleum ether extraction in the step S4 until no new precipitate is generated, stirring to completely precipitate, filtering, washing the precipitate with ice water for 3 times, discarding filtrate and washing liquid, completely dissolving the washed precipitate with 1.2L of 95 v% ethanol aqueous solution, introducing excessive H2Performing double decomposition on S gas to generate PbS sediment, filtering to remove lead element to obtain a second filtrate, washing the PbS sediment twice by using 1L of ethanol water solution (95 v%) and collecting PbS lotion, finally combining the second filtrate and the PbS lotion, adding 25.0g of powdered activated carbon to decolor at 60 ℃, filtering, concentrating and drying to obtain 20.05g of schisandra total saponin, and detecting the content of the total saponin to be 94.07 wt% by using an ultraviolet spectrophotometer.
Example 3
The embodiment of the invention provides a method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra, which specifically comprises the following steps:
s1, water extraction
Weighing 10kg of dried and crushed powdered schisandra chinensis raw material, performing reflux extraction for 90min at 90 ℃ by using 120L of pure water, performing reflux extraction for 60min on filter residue after solid-liquid separation by using 75L of pure water under the same condition, combining filtrate obtained by two times of reflux extraction to obtain water extract, and drying the extraction residue at 60 ℃ for later use;
s2, extraction and purification of polysaccharide
Concentrating the water extract obtained in the step S1 to 1.2 Baume under reduced pressure, adding 95 v% ethanol, stirring while adding ethanol to make the ethanol content reach 78 v%, standing at 4 ℃ for 12h, filtering, collecting precipitate and filtrate to obtain a filter cake containing polysaccharide and a first filtrate containing saponin, washing the filter cake with 20 ℃ absolute ethanol to obtain crude schisandra chinensis polysaccharide, redissolving with water, centrifuging to remove insoluble substances, adding ammonium sulfate until saturated, standing, centrifuging to remove protein (repeating for 4 times), collecting supernatant, putting into a dialysis bag with molecular weight cutoff of 6000Da, dialyzing for 72h to obtain polysaccharide extract, concentrating and drying under reduced pressure to obtain 751.94g of schisandra chinensis polysaccharide, and detecting the polysaccharide content to be 86.72 wt% by using an ultraviolet spectrophotometer;
s3 flash alcohol extraction
Extracting the extraction residue dried in the step S1 with high-concentration ethanol aqueous solution by adopting a flash extraction method, wherein the specific conditions are that the extraction is carried out twice by using 82 v% ethanol aqueous solution at room temperature, the dosage and the extraction time of the ethanol aqueous solution in the first extraction are respectively 55L and 5min, the dosage and the extraction time of the ethanol aqueous solution in the second extraction are respectively 40L and 4min, filtering after the extraction is finished, and combining the filtrate to obtain alcohol extract containing total lignans and total saponins;
s4 extraction and purification of total lignans
Combining the first filtrate containing saponin in the step S2 with the alcohol extract in the step S3, recovering ethanol, adding water to dilute to 40L, passing through an LX-T81 type macroporous resin column at a sample flow rate of 1.5BV/h, washing with 5BV water to remove water-soluble impurities, eluting with 3.5BV ethanol aqueous solution (30 v%) at an elution flow rate of 2.0BV/h to remove other impurities without target components, eluting with 5BV ethanol aqueous solution (94 v%) at an elution flow rate of 1.8BV/h, collecting the eluent, concentrating and recovering ethanol in sequence, transferring to a separating funnel, adding equal volume of petroleum ether, shaking sufficiently, standing for layering, separating a water layer and an ether layer, repeatedly adding equal volume of petroleum ether for 3 times for sufficient extraction, then adding 500.00g of white dextrin into the petroleum ether extract, concentrating and drying under reduced pressure to obtain 295.17g of total lignans of schisandra chinensis, detecting the total lignanoid content to be 52.13 wt% by using an HPLC method;
s5, extraction and purification of total saponins
Adding 30 wt% of neutral lead acetate aqueous solution (used as the existing preparation) into the water phase residue after the petroleum ether extraction in the step S4 until no new precipitate is generated, stirring to completely precipitate, filtering, washing the precipitate with ice water for 3 times, discarding filtrate and washing liquid, completely dissolving the washed precipitate with 9.5L of 95 v% ethanol aqueous solution, introducing excessive H2Performing double decomposition on S gas to generate PbS sediment, filtering to remove lead element to obtain a second filtrate, washing the PbS sediment twice by using 90L ethanol water solution (95 v%) and collecting PbS lotion, finally combining the second filtrate and the PbS lotion, adding 200.0g of powdered activated carbon to decolor at 60 ℃, filtering, concentrating and drying to obtain 199.86g of schisandra total saponin, and detecting the content of the total saponin to be 94.42 wt% by using an ultraviolet spectrophotometer.
Analyzing the results of examples 1-3, it can be seen that:
(1) according to the embodiment of the invention, the ammonium sulfate solution is added into the crude schisandra chinensis polysaccharide obtained by water extraction and alcohol precipitation, so that macromolecular impurities such as protein and the like can be effectively removed, and the centrifuged supernatant is dialyzed in deionized water by using a dialysis bag to remove micromolecular impurities, so that high-purity schisandra chinensis polysaccharide is obtained;
(2) according to the embodiment of the invention, the supernatant obtained by water extraction and alcohol precipitation and the alcohol extract are combined, subjected to alcohol removal and then loaded onto macroporous resin, and washed by water and then eluted by low-concentration ethanol, so that non-target components can be removed to the maximum extent, the content of the target components obtained by alcohol washing is further increased, and a mixture of lignans and total saponins with higher content can be obtained after macroporous resin purification, so that the further purification is facilitated;
(3) the method provided by the embodiment of the invention has high resource utilization, can extract and purify various active ingredients in the schisandra chinensis, maximizes the resource utilization and reduces the waste;
(4) the method provided by the embodiment of the invention has high extraction efficiency, can extract the effective components in the plants within a few minutes by using a flash extraction technology, has obviously increased extraction efficiency compared with other extraction methods, and has wide practical application prospect.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention.
It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for comprehensively extracting schisandra polysaccharide, schisandra total lignans and schisandra total saponins from schisandra is characterized in that,
comprises the steps of (a) preparing a mixture of a plurality of raw materials,
s1, water extraction
Adding powdered fructus Schisandrae chinensis raw material into water, heating for extraction, performing solid-liquid separation to obtain water extractive solution, and drying the extractive residue at low temperature;
s2, extraction and purification of polysaccharide
Concentrating the water extract to 1.1-1.2 Baume, adding ethanol, controlling ethanol content to 70-80 v%, standing, filtering to obtain a first filtrate containing saponin and a filter cake containing polysaccharide, and post-treating the filter cake to obtain Schisandra chinensis polysaccharide;
s3 flash alcohol extraction
Extracting the extraction residue dried in the step S1 with high-concentration ethanol water solution by adopting a flash extraction method, and filtering to obtain an ethanol extract containing total lignans and total saponins;
s4 extraction and purification of total lignans
Combining the first filtrate obtained in the step S2 with the alcohol extract obtained in the step S3, sequentially carrying out impurity removal treatment, alcohol solution elution and alcohol concentration removal, then extracting with petroleum ether, and reprocessing the petroleum ether extract to obtain the schisandra total lignans;
s5, extraction and purification of total saponins
Purifying the water phase residue obtained after the petroleum ether extraction in the step S4 to obtain total saponins of schisandra chinensis;
wherein the order of step S2 and step S3 may be interchanged.
2. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 1, wherein,
in the step S2, in the step S,
the concentration of the added ethanol is 92-98 v%, and the ethanol is added and stirred at the same time;
and/or the standing time is 12-20h, and the standing time is more preferably 12-15h at the temperature of 3-8 ℃.
3. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 1 or 2, wherein,
in step S2, the post-processing includes,
washing the filter cake with anhydrous ethanol at a temperature lower than 35 deg.C to obtain crude polysaccharide of fructus Schisandrae chinensis, re-dissolving with water, centrifuging to remove insoluble substances, adding ammonium sulfate until saturation, standing, centrifuging to remove protein, collecting supernatant, dialyzing to obtain polysaccharide extractive solution, and concentrating and drying to obtain fructus Schisandrae chinensis polysaccharide.
4. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 3, wherein,
in the step S2, in the step S,
adding the ammonium sulfate and centrifuging to remove protein for 3-5 times;
and/or, the dialysis is specifically to dialyze the supernatant by a dialysis bag with the molecular weight cut-off of 5000-;
and/or the dialysis temperature and time are 2-10 ℃ and 48-120h respectively.
5. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 1, wherein,
in the step S3, in the step S,
the concentration of the ethanol water solution is 75-85 v%, preferably 78-82 v%;
and/or the adding amount of the ethanol water solution is controlled to be 1 g: 5-50 ml;
and/or, the temperature and time of the extraction are 20-50 ℃ and 5-10min respectively;
and/or the extraction times are 2-3 times, and the alcohol extract is obtained by combining the extraction and the filtration.
6. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 1, wherein,
in the step S1, in the step S,
the amount of the powdery schisandra raw material added into water is controlled to be 1 g: 5-50 ml;
and/or, the temperature and time of the heating extraction are respectively 80-100 ℃ and 30-120 min;
and/or the times of heating extraction are 2-3 times, and the water extract is obtained by combining the heating extraction and the extraction.
7. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to any one of claims 1 to 6, wherein,
in the step S4, in the step S,
the impurity removal treatment comprises recovering ethanol, adding water for dilution, loading onto a macroporous resin column, and sequentially eluting with water and 10-30 v% ethanol water solution for impurity removal;
and/or, the alcohol solution is specifically eluted by 60-95 v% ethanol water solution and the eluate is collected;
and/or, the petroleum ether extraction is specifically that the eluent after concentration and alcohol removal is transferred into a separating funnel, the equal volume of petroleum ether is added, the mixture is sufficiently shaken, and after standing and layering, a water layer and a petroleum ether layer are separated, and preferably repeated for 3 times to sufficiently extract;
and/or, the petroleum ether extract is re-treated by adding white dextrin into the petroleum ether extract, and concentrating and drying under reduced pressure.
8. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to claim 7, wherein,
in the step S4, in the step S,
in the impurity removal treatment, the volume multiple of the impurity removal treatment after being diluted by water is 2-10 times;
and/or the macroporous resin column is one of LX-60 type, LX-T28 type, LX-T81 type and LX-T91 type macroporous resin column;
and/or the sample loading flow rate of the macroporous resin column is 0.5-2.0 BV/h;
and/or the elution flow rates of the 10-30 v% ethanol aqueous solution and the 60-95 v% ethanol aqueous solution are both 1.0-3.0 BV/h;
and/or the elution volumes of the water, the 10-30 v% ethanol aqueous solution and the 60-95 v% ethanol aqueous solution are all 3-6 BV.
9. The method for comprehensively extracting schisandra chinensis polysaccharides, schisandra chinensis total lignans and schisandra chinensis total saponins from schisandra chinensis according to any one of claims 1 to 8,
in the step S5, in the step S,
the purification treatment comprises adding neutral lead acetate solution into the water phase residue until no precipitate is generated, filtering, washing the precipitate with ice water for 2-3 times, and washing the precipitate with 90-98v% of ethanol aqueous solution is completely dissolved and excess H is introduced2Performing double decomposition on S gas to generate PbS sediment, filtering the sediment to obtain a second filtrate, washing the PbS sediment by using 90-98 v% ethanol water solution to obtain PbS lotion, finally combining the second filtrate and the PbS lotion, adding activated carbon to decolor, and sequentially filtering, concentrating and drying to obtain the PbS washing lotion;
preferably, the lead acetate solution is 20-30 wt% of lead acetate aqueous solution which is used in preparation, and/or the 90-98 v% of ethanol aqueous solution for dissolving the precipitate has the mass 30-50 times of the mass of the precipitate, and/or the amount of the activated carbon is 0.01-0.05 times of the sum of the mass of the second filtrate and the PbS washing liquor.
10. Use of the method of any one of claims 1-9 for the integrated extraction of schisandra polysaccharides, schisandra total lignans and schisandra total saponins from schisandra.
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