CN106266168A - A kind of preparation method of Fructus Schisandrae Sphenantherae lignanoid extract - Google Patents
A kind of preparation method of Fructus Schisandrae Sphenantherae lignanoid extract Download PDFInfo
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- 239000000284 extract Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000012567 medical material Substances 0.000 claims abstract description 55
- 239000011347 resin Substances 0.000 claims abstract description 44
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 238000010828 elution Methods 0.000 claims abstract description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 238000010079 rubber tapping Methods 0.000 claims abstract description 16
- 230000006837 decompression Effects 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 11
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000000469 ethanolic extract Substances 0.000 claims description 14
- 235000019640 taste Nutrition 0.000 claims description 12
- UFCGDBKFOKKVAC-DSASHONVSA-N Schisantherin A Chemical compound O([C@H]1C=2C=C(C(=C(OC)C=2C2=C(OC)C=3OCOC=3C=C2C[C@H](C)[C@@]1(O)C)OC)OC)C(=O)C1=CC=CC=C1 UFCGDBKFOKKVAC-DSASHONVSA-N 0.000 claims description 9
- UFCGDBKFOKKVAC-CEFZEKJPSA-N Schisantherin A Natural products O=C(O[C@@H]1[C@](O)(C)[C@H](C)Cc2c(c(OC)c3OCOc3c2)-c2c(OC)c(OC)c(OC)cc12)c1ccccc1 UFCGDBKFOKKVAC-CEFZEKJPSA-N 0.000 claims description 9
- ZEMSHIOAFVYIFX-UHFFFAOYSA-N benzoylgomisin Q Natural products C12=CC(OC)=C(OC)C(OC)=C2C=2C(OC)=C(OC)C(OC)=CC=2CC(C)C(C)(O)C1OC(=O)C1=CC=CC=C1 ZEMSHIOAFVYIFX-UHFFFAOYSA-N 0.000 claims description 9
- 229930013686 lignan Natural products 0.000 claims description 6
- 150000005692 lignans Chemical class 0.000 claims description 6
- 235000009408 lignans Nutrition 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 229920005610 lignin Polymers 0.000 abstract description 6
- 241000561709 Kadsura longipedunculata Species 0.000 abstract description 4
- 229940126678 chinese medicines Drugs 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 238000000034 method Methods 0.000 description 23
- JEJFTTRHGBKKEI-OKILXGFUSA-N deoxyschizandrin Chemical compound C1[C@H](C)[C@H](C)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC JEJFTTRHGBKKEI-OKILXGFUSA-N 0.000 description 11
- JEJFTTRHGBKKEI-UHFFFAOYSA-N deoxyschizandrin Natural products C1C(C)C(C)CC2=CC(OC)=C(OC)C(OC)=C2C2=C1C=C(OC)C(OC)=C2OC JEJFTTRHGBKKEI-UHFFFAOYSA-N 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 235000013399 edible fruits Nutrition 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000002481 ethanol extraction Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 240000006079 Schisandra chinensis Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 208000008967 Enuresis Diseases 0.000 description 1
- 235000008422 Schisandra chinensis Nutrition 0.000 description 1
- 241000736078 Schisandra sphenanthera Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- HLVXFWDLRHCZEI-UHFFFAOYSA-N chromotropic acid Chemical compound OS(=O)(=O)C1=CC(O)=C2C(O)=CC(S(O)(=O)=O)=CC2=C1 HLVXFWDLRHCZEI-UHFFFAOYSA-N 0.000 description 1
- 208000013116 chronic cough Diseases 0.000 description 1
- 208000019902 chronic diarrheal disease Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000027939 micturition Effects 0.000 description 1
- 230000000324 neuroprotective effect Effects 0.000 description 1
- 230000036565 night sweats Effects 0.000 description 1
- 206010029410 night sweats Diseases 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- BSCHIACBONPEOB-UHFFFAOYSA-N oxolane;hydrate Chemical compound O.C1CCOC1 BSCHIACBONPEOB-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 239000002023 wood 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)
-
- 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
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
This belongs to technical field of Chinese medicines, is specifically related to the preparation method of a kind of Kadsura longipedunculata lignin.The Kadsura longipedunculata lignin preparation method of the present invention is to use ethanol water reflux, extract, Fructus Schisandrae Sphenantherae medical material, prepare load solution again, load solution is crossed low pole macroporous resin adsorption post, first carry out eluting remove impurity with the ethanol of 10 30%, then with 70 90% ethanol elution, and collect ethanol elution, ethanol elution is crossed the alumina adsorption post of 0.5 2 times of medical material weight, collect effluent decompression or normal pressure reclaims solvent to the greatest extent, in 60 100 DEG C of decompressions or constant pressure and dry, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract.The extraction efficiency of the present invention improves, and tapping is smooth and easy, and the big compliance that produces is greatly improved, and the production time significantly shortens, and saves production cost.
Description
Technical field
This belongs to technical field of Chinese medicines, is specifically related to a kind of Fructus Schisandrae Sphenantherae lignanoid extract and preparation method thereof.
Background technology
Fructus Schisandrae Sphenantherae is Magnoliacea plant schisandra chinensis (Schisandra sphenanthera Rehd.et Wils.)
Dry mature fruit, be important conventional Chinese medicine.There is convergence astringent or styptic treatment for spontaneous sweating, supplementing QI for promoting the production of body fluid, effect of kidney calming, for chronic cough
Dyspnea due to deficiency, emission, enuresis frequent micturition, incessant chronic diarrhea, spontaneous perspiration, night sweat, Tianjin wound are thirsty, deficient pulse of losing heart, interior-heat are quenched one's thirst, cardiopalmus is lost
Sleep.
Lignanoid is the main active of Fructus Schisandrae Sphenantherae, document report its have anticancer, antiviral, antioxidation, protect the liver,
The pharmacologically active such as Adjust-blood lipid, neuroprotective, Fructus Schisandrae Sphenantherae lignanoid extract can be widely used for the field such as medicine, health food,
There is good market prospect.
The method for preparing extractive (CN200510023873.5) of existing Kadsura longipedunculata lignin is: with the 6-15 times of south five tastes
The water distillation medical material of sub-medical material weight 1-6 hour；Filter, remain medicinal residues；Decoct medicinal residues 10-60 minute, filter；Volume is medical material
The ethanol water measuring more than 75% weight of 5-15 times extracts medicinal residues, each 0.5-3 hour, filters and obtains filtrate；By gained
Filtrate crosses 1-3 times of medical material amount resin absorbing column, it is thus achieved that effluent, and described resin is selected from polar macroporous adsorption resin；With volume it is
Ethanol elution more than 75% weight of amount of resin 1-5 times, it is thus achieved that eluent；Merge effluent and eluent, it is thus achieved that liquid south
Fructus Schisandrae Chinensis lignans extract.The method implementation process finds be not suitable for big production operation, owing to Fructus Schisandrae Sphenantherae is fruit
Class medical material, after water distillation and soak by water medical material, the easy gelatinizing of medical material, tapping difficulty, hinder production to carry out, and owing to medicinal residues contain
Large quantity of moisture, when adding ethanol extraction, actual concentration of alcohol declines, and causes effective ingredient lignanoid extraction ratio low；Macroporous absorption tree
Fat is that polar resin, sample solution and eluent are all collected, and does not has remove impurity elution step, and purification effect is limited, final extraction ratio and
Effective site content is the most relatively low, it is desirable to have preferably method is to meet being smoothed out of big production, and it is effective to improve extract
Component content and yield.
Summary of the invention
The problem existed for prior art, the present invention provides a kind of preparation side preparing Fructus Schisandrae Sphenantherae lignanoid extract
Method, it is therefore an objective to improve the extraction ratio of lignanoid, meet big industrial requirement.
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present invention follows the steps below:
(1) the ethanol water reflux, extract, south of the weight fraction 70-90% of 8-12 times of Fructus Schisandrae Sphenantherae medical material weight is used
Schisandra chinensis medicinal material 1-3 time, each 0.5-2 hour, each tapping time was 30 minutes, is filtrated to get ethanol extraction after extraction
Liquid；
(2) ethanol extract is evaporated to 1-2 times of medical material bulking value, adds water and be diluted to 3-10 times of medical material weight
Volume, obtains load solution；
(3) gained load solution is crossed the low pole macroporous resin adsorption post of 0.5-3 times of medical material weight, first sets with 1-4 times
The ethanol of the weight fraction 10-30% of fat weight carries out eluting remove impurity, then with the weight fraction 70-of 2-5 times of weight resin
The ethanol elution of 90%, and collect ethanol elution；
(4) ethanol elution is crossed the alumina adsorption post of 0.5-2 times of medical material weight, collects effluent decompression or normal pressure returns
Receive solvent to the greatest extent, in 60-100 DEG C of decompression or constant pressure and dry, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract.
Wherein, in described step (1), the consumption of ethanol water is preferably 10 times of Fructus Schisandrae Sphenantherae medical material weight, ethanol
Aqueous solution preferred concentration is weight percentage 80%.
Described step (1) reflux, extract, Fructus Schisandrae Sphenantherae medical material number of times preferably 2 times, the most each 1 hour.
The described low pole macroporous adsorbent resin in step (3) is optimized for AB-8 type.
Gained load solution is crossed the low pole macroporous resin adsorption post of 0.5-3 times of medical material weight by described step (3), first
Eluting remove impurity is carried out, then with the weight fraction 80% of 3 times of weight resins with the ethanol of the weight fraction 20% of 2 times of weight resins
Ethanol elution, and collect ethanol elution.
Aluminium oxide in described step (4) selects neutral alumina.
Described Fructus Schisandrae Sphenantherae lignanoid extract, according to percentage by weight, containing lignanoid 60%-90%, wherein
Schisantherin A 8%-30%, deoxyschizandrin 8%-30%.
Compared with prior art, the feature of the present invention and providing the benefit that:
(1) present invention directly uses ethanol extraction medical material, compared to the distillation of former method water and soak by water step, extraction efficiency
Improving, tapping is smooth and easy, and the big compliance that produces is greatly improved, and the production time significantly shortens, and saves production cost.
(2) although the present invention and former technics comparing all use macroporous adsorbent resin to be purified, but both operating procedures are complete
Complete different, the macroporous adsorbent resin polarity of use is different, and remove impurity principle is the most different, and the effect of purification is the most different.Fructus Schisandrae Sphenantherae
Lignanoid's effective site is liposoluble constituent, and former technique uses polar macroporous adsorption resin, the direct loading of alcohol extract, utilizes liposoluble
Property composition do not adsorb, water-solubility impurity is adsorbed on resin and reaches remove impurity purpose, collects effluent and eluent, obtains the south five tastes
Sub-lignanoid effective site；And the inventive method changes employing low pole macroporous adsorbent resin, extracting solution reclaims organic solvent and adds water
Dilution, aqueous solution loading, need the fat-soluble effective ingredient obtained to be adsorbed on resin column, water-solubility impurity does not adsorbs, and flows out
Liquid discards, and uses low solubility ethanol elution, it is possible to remove middle polarity material such as organic acid etc., more weak with high concentration ethanol desorbing
The fat-soluble lignanoids effective ingredient of alkalescence, obtains Kadsura longipedunculata lignin effective site, and purification effect is more preferable.
(3) present invention increases aluminium oxide decolouring removal step, removes the pigment compositions such as chlorophyll, further increases south five
The content of taste lignans extract effective ingredient.
Detailed description of the invention
The Fructus Schisandrae Sphenantherae extracting method of the present invention uses high concentration ethanol as extracting reagent, then uses macroporous resin and oxygen
Change aluminum and carry out adsorption and purification, to extract lignanoid, schisantherin A and deoxyschizandrin as quality control standard, use the present invention's
Preparation method, can obtain the Fructus Schisandrae Sphenantherae lignanoid extract containing high-load lignanoid.
In the present embodiment, the detection to total lignans in Fructus Schisandrae Sphenantherae lignanoid extract and schisantherin A content uses
Shimadzu UV-2550 spectrophotometer and Agilent HPLC-1260, concrete grammar is:
Total lignans: accurate absorption schisantherin A reference substance solution, need testing solution and each 0.4ml of methanol, puts respectively
In 10mL measuring bottle, 80 DEG C of water-baths volatilize, and are separately added into 0.5mL10% chromotropic acid solution, 3mL concentrated sulphuric acid, 1.5mL distilled water,
Put in boiling water bath and heat 30 minutes, cool down rapidly, with methanol pipe as blank, measure absorbance at spectrophotometric 570nm, calculate wood
Fat cellulose content.
Schisantherin A and deoxyschizandrin: HPLC method, flow phase oxolane-water (38:62), detects wavelength 258nm,
Flow velocity 1ml/min, column temperature 25 DEG C.
Embodiment 1～5 and the testing result of comparative example as shown in table 1.
Embodiment 1:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment follows the steps below:
(1) take 20kg Fructus Schisandrae Sphenantherae dry fruit, use the second of the weight fraction 80% of 10 times of Fructus Schisandrae Sphenantherae medical material weight
Alcohol-water solution reflux, extract, Fructus Schisandrae Sphenantherae medical material 2 times, each 1 hour, each tapping time all at 30 minutes, merged twice ethanol
Extracting solution, is filtrated to get 360L ethanol extract；
(2) ethanol extract is evaporated to 40L, adds water and be diluted to 100L, obtain load solution；
(3) gained load solution is crossed the AB-8 resin absorbing column of 1 times of medical material weight, first with the weight of 2 times of weight resins
The ethanol of mark 20% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 80% of 3 times of weight resins, and collects second
Alcohol eluen；
(4) ethanol elution is crossed the alumina adsorption post of 1 times of medical material weight, collects effluent decompression recycling ethanol, in
80 DEG C of vacuum drying, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract, extract yield is 3.65%.
The Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment, according to percentage by weight, containing lignanoid 80%, the wherein five tastes
Sub-ester first 13.2%, deoxyschizandrin 13.5%.
Embodiment 2:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment follows the steps below:
(1) take 20kg Fructus Schisandrae Sphenantherae dry fruit, use the ethanol of the weight fraction 90% of 8 times of Fructus Schisandrae Sphenantherae medical material weight
Aqueous solution reflux, extract, Fructus Schisandrae Sphenantherae medical material 2 times, each 0.5 hour, each tapping time all at 30 minutes, merged twice ethanol
Extracting solution, is filtrated to get 280L ethanol extract；
(2) ethanol extract is evaporated to 20L, adds water and be diluted to 60L, obtain load solution；
(3) gained load solution is crossed the AB-8 resin absorbing column of 0.5 times of medical material weight, first with the weight of 4 times of weight resins
The ethanol of amount mark 20% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 80% of 5 times of weight resins, and collects
Ethanol elution；
(4) ethanol elution is crossed the alumina adsorption post of 0.5 times of medical material weight, collects effluent decompression recycling ethanol,
In 60 DEG C of drying under reduced pressure, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract, extract yield is 3.26%.
The Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment, according to percentage by weight, containing lignanoid 69%, the wherein five tastes
Sub-ester first 9.5%, deoxyschizandrin 10.2%.
Embodiment 3:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment follows the steps below:
(1) take 20kg Fructus Schisandrae Sphenantherae dry fruit, use the second of the weight fraction 70% of 12 times of Fructus Schisandrae Sphenantherae medical material weight
Alcohol-water solution reflux, extract, Fructus Schisandrae Sphenantherae medical material 2 times, each 1.5 hours, each tapping time all at 30 minutes, merged twice second
Alcohol extract, is filtrated to get 440L ethanol extract；
(2) ethanol extract is evaporated to 40L, adds water and be diluted to 200L, obtain load solution；
(3) gained load solution is crossed the AB-8 resin absorbing column of 1 times of medical material weight, first with the weight of 2 times of weight resins
The ethanol of mark 20% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 70% of 3 times of weight resins, and collects second
Alcohol eluen；
(4) ethanol elution is crossed the alumina adsorption post of 1 times of medical material weight, collects effluent decompression recycling ethanol, in
100 DEG C of constant pressure and dries, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract, extract yield is 3.45%.
The Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment, according to percentage by weight, containing lignanoid 75%, the wherein five tastes
Sub-ester first 11.3%, deoxyschizandrin 12.5%.
Embodiment 4:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment follows the steps below:
(1) take 20kg Fructus Schisandrae Sphenantherae dry fruit, use the second of the weight fraction 70% of 10 times of Fructus Schisandrae Sphenantherae medical material weight
Alcohol-water solution reflux, extract, Fructus Schisandrae Sphenantherae medical material 3 times, each 1 hour, each tapping time, all at 30 minutes, merged three ethanol
Extracting solution, is filtrated to get 720L ethanol extract；
(2) ethanol extract is evaporated to 40L, adds water and be diluted to 200L, obtain load solution；
(3) gained load solution is crossed the AB-8 resin absorbing column of 1 times of medical material weight, first with the weight of 2 times of weight resins
The ethanol of mark 20% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 80% of 3 times of weight resins, and collects second
Alcohol eluen；
(4) ethanol elution is crossed the alumina adsorption post of 1 times of medical material weight, collects effluent decompression recycling ethanol, in
80 DEG C of vacuum drying, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract, extract yield is 3.36%.
The Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment, according to percentage by weight, containing lignanoid 78%, the wherein five tastes
Sub-ester first 12.1%, deoxyschizandrin 13.1%.
Embodiment 5:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment follows the steps below:
(1) take 20kg Fructus Schisandrae Sphenantherae dry fruit, use the second of the weight fraction 80% of 10 times of Fructus Schisandrae Sphenantherae medical material weight
Alcohol-water solution reflux, extract, Fructus Schisandrae Sphenantherae medical material 2 times, each 1 hour, each tapping time all at 30 minutes, merged twice ethanol
Extracting solution, is filtrated to get 440L ethanol extract；
(2) ethanol extract is evaporated to 40L, adds water and be diluted to 100L, obtain load solution；
(3) gained load solution is crossed the AB-8 resin absorbing column of 2 times of medical material weight, first with the weight of 3 times of weight resins
The ethanol of mark 30% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 90% of 4 times of weight resins, and collects second
Alcohol eluen；
(4) ethanol elution is crossed the alumina adsorption post of 1 times of medical material weight, collects effluent decompression recycling ethanol, in
80 DEG C of vacuum drying, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract, extract yield is 3.56%.
Resin demand is 2 times of medical material amount, and medicinal liquid first enters with the ethanol of 3 times of resinite accumulated amount 30% concentration after having crossed post bed
Row eluting remove impurity, after with 4 times of resinite accumulated amount 90% concentration ethanol eluting, collect 90% ethanol elution, cross 2 times of medical material amount oxygen
Change aluminum adsorption column, effluent decompression recycling ethanol, 80 DEG C of vacuum drying, obtain Fructus Schisandrae Sphenantherae lignanoid extract.
The Fructus Schisandrae Sphenantherae lignanoid extract of the present embodiment, according to percentage by weight, containing lignanoid 73%, the wherein five tastes
Sub-ester first 11.5%, deoxyschizandrin 12.6%.
Comparative example:
The method preparing Fructus Schisandrae Sphenantherae lignanoid extract of comparative example follows the steps below:
Take 20kg Fructus Schisandrae Sphenantherae dry fruit, carry out vapor distillation 4 hours with the water of 10 times of medical material amounts, filter, tapping
7 hours time, obtain medicinal residues；
The medicinal residues water boiling and extraction 30 minutes of 6 times of medical material amounts, 10 hours tapping time, filters, discards filtrate；
With 80% alcohol reflux of 10 times of medical material amounts, extracting altogether twice, each 1 hour, each tapping time is all 3
About hour, merging twice ethanol extract, filter, obtain 380L medicinal liquid, gained medicinal liquid crosses resin absorbing column LSA-7, resin
Consumption is 1 times of medical material amount, and 85% ethanol elution used by medicinal liquid after having crossed post bed, collects ethanol and (includes flowing through liquid and eluting
Liquid), filter, reclaim ethanol, water bath method, 60 DEG C of drying, obtain Fructus Schisandrae Sphenantherae lignanoid extract.
After testing, Fructus Schisandrae Sphenantherae lignanoid extract prepared by comparative example contains lignin 56%, wherein schisantherin A
7.2%, deoxyschizandrin 7.5%.
Table 1 embodiment 1～5 and the lignin extraction result table of comparative example
As it can be seen from table 1 the Fructus Schisandrae Sphenantherae medical material of five crowdes of 20kg is after the new method extraction purification of the present invention, the south five tastes
Sub-lignans extract yield relative to medical material input amount all more than 3%, lignanoid's content (total lignans in extract after testing
Percentage by weight shared in extract) more than 60%, schisantherin A and deoxyschizandrin content are all more than 9%.
And comparative example Fructus Schisandrae Sphenantherae lignanoid extract yield is about 2.5%, after testing in extract the content of lignanoid 56%,
Schisantherin A and deoxyschizandrin content are all below 9%.
Production process tapping situation, new method 5 batches extraction each tapping time is all at about 30 minutes, and former method tapping
Time is respectively 7 hours, 10 hours, 3 hours, 3 hours, and overlong time seriously restricts production process.
As it has been described above, the method for the present invention can extract Fructus Schisandrae Sphenantherae lignanoid extract efficiently, technique is suitable for big raw
Producing operation, active constituent content is high, and extract yield is the highest, has more preferable productivity effect.
Claims (7)
1. the preparation method of a Fructus Schisandrae Sphenantherae lignanoid extract, it is characterised in that follow the steps below:
(1) the ethanol water reflux, extract, south five tastes of the weight fraction 70-90% of 8-12 times of Fructus Schisandrae Sphenantherae medical material weight are used
Sub-medical material 1-3 time, each 0.5-2 hour, each tapping time was 30 minutes, is filtrated to get ethanol extract after extraction；
(2) ethanol extract is evaporated to 1-2 times of medical material bulking value, adds water and be diluted to 3-10 times of medical material weighing body
Long-pending, obtain load solution；
(3) gained load solution is crossed the low pole macroporous resin adsorption post of 0.5-3 times of medical material weight, first with 1-4 times of resin weight
The ethanol of the weight fraction 10-30% of amount carries out eluting remove impurity, then with the weight fraction 70-90%'s of 2-5 times of weight resin
Ethanol elution, and collect ethanol elution；
(4) ethanol elution is crossed the alumina adsorption post of 0.5-2 times of medical material weight, collects effluent decompression or normal pressure reclaims to the greatest extent
Solvent, in 60-100 DEG C of decompression or constant pressure and dry, it is thus achieved that Fructus Schisandrae Sphenantherae lignanoid extract.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described step
(1) in, the consumption of ethanol water is preferably 10 times of Fructus Schisandrae Sphenantherae medical material weight, and ethanol water preferred concentration is weight hundred
Proportion by subtraction is 80%.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described step
(1) reflux, extract, Fructus Schisandrae Sphenantherae medical material number of times preferably 2 times, the most each 1 hour.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described step
(3) the low pole macroporous adsorbent resin in is optimized for AB-8 type.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described step
(3) gained load solution is crossed the low pole macroporous resin adsorption post of 0.5-3 times of medical material weight, first with the weight of 2 times of weight resins
The ethanol of amount mark 20% carries out eluting remove impurity, then with the ethanol elution of the weight fraction 80% of 3 times of weight resins, and collects
Ethanol elution.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described step
(4) aluminium oxide in selects neutral alumina.
The preparation method of Fructus Schisandrae Sphenantherae lignanoid extract the most according to claim 1, it is characterised in that described south five
Taste lignans extract by weight percentage, containing lignanoid 60%-90%, wherein schisantherin A 8%-30%, five
Taste A prime 8%-30%.
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| CN107468803A (en) * | 2017-07-27 | 2017-12-15 | 磐安县派普特生物科技有限公司 | The preparation method of shizandra active extract |
| CN107663188A (en) * | 2017-10-27 | 2018-02-06 | 河南中医药大学 | A kind of root bark of Chinese wolf-berry total lignan amide alkaloid extract and its production and use |
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| CN1813900A (en) * | 2005-02-05 | 2006-08-09 | 苏州市思源医药科技有限公司 | Kadsura longipedunculata lignin extract and its preparing method and use |
| CN101214278A (en) * | 2007-12-26 | 2008-07-09 | 沈阳药科大学 | New raw material for extracting fructus schizandrae total lignans and preparation technique and use |
| CN101757111A (en) * | 2009-12-23 | 2010-06-30 | 南京泽朗医药科技有限公司 | Preparation method of Chinese magnoliavine fruit total lignan |
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| CN1813900A (en) * | 2005-02-05 | 2006-08-09 | 苏州市思源医药科技有限公司 | Kadsura longipedunculata lignin extract and its preparing method and use |
| CN101214278A (en) * | 2007-12-26 | 2008-07-09 | 沈阳药科大学 | New raw material for extracting fructus schizandrae total lignans and preparation technique and use |
| CN101757111A (en) * | 2009-12-23 | 2010-06-30 | 南京泽朗医药科技有限公司 | Preparation method of Chinese magnoliavine fruit total lignan |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107468803A (en) * | 2017-07-27 | 2017-12-15 | 磐安县派普特生物科技有限公司 | The preparation method of shizandra active extract |
| CN107663188A (en) * | 2017-10-27 | 2018-02-06 | 河南中医药大学 | A kind of root bark of Chinese wolf-berry total lignan amide alkaloid extract and its production and use |
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