CN100465183C - Method of comprehensive utilizing schisandra fruit - Google Patents
Method of comprehensive utilizing schisandra fruit Download PDFInfo
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- CN100465183C CN100465183C CNB2006100415664A CN200610041566A CN100465183C CN 100465183 C CN100465183 C CN 100465183C CN B2006100415664 A CNB2006100415664 A CN B2006100415664A CN 200610041566 A CN200610041566 A CN 200610041566A CN 100465183 C CN100465183 C CN 100465183C
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 235000008422 Schisandra chinensis Nutrition 0.000 title claims abstract description 29
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 17
- 240000006079 Schisandra chinensis Species 0.000 title description 10
- 238000000605 extraction Methods 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000284 extract Substances 0.000 claims abstract description 34
- 150000004676 glycans Chemical class 0.000 claims abstract description 34
- 239000005017 polysaccharide Substances 0.000 claims abstract description 34
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 20
- 241000736075 Schisandra Species 0.000 claims abstract description 19
- 229930013686 lignan Natural products 0.000 claims abstract description 12
- 150000005692 lignans Chemical class 0.000 claims abstract description 12
- 235000009408 lignans Nutrition 0.000 claims abstract description 12
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 238000003809 water extraction Methods 0.000 claims abstract description 5
- 235000021028 berry Nutrition 0.000 claims description 51
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 2
- 241001506371 Kadsura Species 0.000 description 8
- 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 description 5
- 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 5
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 5
- 239000013558 reference substance Substances 0.000 description 5
- 238000002798 spectrophotometry method Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 4
- 208000026487 Triploidy Diseases 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 241000218377 Magnoliaceae Species 0.000 description 1
- 241000736078 Schisandra sphenanthera Species 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 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
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000002443 hepatoprotective effect Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 235000015961 tonic Nutrition 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 229960000716 tonics Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Medicines Containing Plant Substances (AREA)
Abstract
The present invention belongs to the field of schisandra processing technology, and is especially comprehensive schisandra utilizing process. The process capable of utilizing two kinds of active schisandra components, lignan and polysaccharide, includes the following steps: the first supercritical CO2 fluid extraction or alcohol extraction to extract the schisandra lignan from schisandra fruit powder as the material, and the subsequent hot water extraction of schisandra polysaccharide from the residue after lignan extraction. The lignan extract and the polysaccharide extract may be used as food and medicine. The present invention raises the comprehensive utilization value of schisandra obviously.
Description
Technical field
The present invention relates to the shizandra berry processing technique field, refer in particular to a kind of method that fully utilizes shizandra berry, can utilize lignanoid and two kinds of activeconstituentss of polysaccharide in the shizandra berry simultaneously.
Background technology
Shizandra berry is Magnoliaceae shizandra berry (Schisandra chinensis (Turcz.) Baill, be commonly called as Schisandra chinensis) or schisandra chinensis (S.sphenanthera Rehd.et Wils, be commonly called as kadsura longepedunculata) dry mature fruit, the medicinal history in existing more than 2,000 year, its acid of distinguishing the flavor of, sweet, warm in nature, return lung, the heart, kidney channel, it is astringent or styptic treatment for spontaneous sweating to have convergence, the effect of supplementing QI for promoting the production of body fluid and kidney calming, be traditional Chinese medical science strengthening by means of tonics medicine commonly used, its main active ingredient has lignanoid, polysaccharide etc., shizandra berry lignanoid is the main active ingredient of shizandra berry hepatoprotective effect, the shizandra berry polysaccharide has antitumor, the anti-ageing multiple effect of waiting for a long time.But the utilization to shizandra berry mainly is a lignanoid at present, and is few to polysaccharide isoreactivity components utilising; Shizandra berry residue after the extraction lignanoid generally abandons as refuse, causes the waste of medicine resource.Therefore how fully utilizing shizandra berry, improve the comprehensive utilization ratio of resource, is to be one of present problem demanding prompt solution.
The supercritical CO of activeconstituents lignanoid in the relevant shizandra berry
2Fluid extraction method or alcohol extracting method extract existing bibliographical information [Journal of Chromatography B, 2002,770,283-289. both at home and abroad; Northeast China Normal University's journal natural science edition, 2004,36 (2): 50-54.; Plant research, 2005,25 (2): 213-215.], but the utilization of shizandra berry residue research does not appear in the newspapers after extracting.[the Shaanxi traditional Chinese medical science, 2003,24 (3) such as Li Qiaoyun etc. [Food science, 2004,25 (5): 105-109.], Xue Mei; 267-268.] reported the extraction process of shizandra berry polysaccharide, but activeconstituents lignanoid wherein is not used.
Summary of the invention
The objective of the invention is in order to solve the deficiency that the above-mentioned background technology exists, a kind of method of comprehensive utilization that can utilize lignanoid and two kinds of activeconstituentss of polysaccharide in the shizandra berry simultaneously is provided.
At this goal of the invention, the present invention adopts following technical scheme; With the schisandra fruit powder is raw material, at first adopts supercritical CO
2Fluid extraction method or alcohol extracting method extract the activeconstituents lignanoid in the shizandra berry; Extract the shizandra berry polysaccharide the residue of reusable heat water extraction method after extracting lignanoid.The present invention can utilize in the shizandra berry two kinds of activeconstituents lignanoids and polysaccharide simultaneously, significantly improves the comprehensive utilization value of schisandra chinensis medicinal material.Its key step is:
1, extraction shizandra berry lignanoid
(1) supercritical CO
2The fluid extraction method
With the schisandra fruit powder is raw material, under 30～50 ℃ of extracting pressure 20～35MPa, extraction temperature, and static extracting or static immersing 2～10 hours; Then at extracting pressure 20～35MPa, 30～50 ℃ of extraction temperature and CO
2Dynamic extraction is 2～6 hours under flow 1～4L/min, obtains shizandra berry lignanoid extract and residue extract remainder.With the Wuweizi ester A is reference substance, chromotropic acid colour developing, spectrophotometry lignanoid content, and shizandra berry extract total lignans extraction rate reached is more than 90%, and lignanoid's content reaches more than 8% in the extract;
(2) alcohol extracting method extracts shizandra berry lignanoid
With the schisandra fruit powder is raw material, refluxing extraction in ethanolic soln, fruit powder wood is 1:5～1:20 (w/v with the solid-liquid ratio of ethanolic soln, g/mL), alcohol concn is that 60～95% (v/v), extraction time are 1～3 hour, extraction time 1～3 time, filter, filtrate concentrate the shizandra berry lignans extract, collect alcohol extracting shizandra berry residue.Shizandra berry extract total lignans extraction rate reached is more than 56%, and lignanoid's content reaches more than 3% in the extract;
2, the extraction of shizandra berry polysaccharide in the residue
With supercritical CO
2After the extraction shizandra berry lignanoid or the shizandra berry polysaccharide that extracts in the residue after the shizandra berry lignanoid of alcohol extracting method adopt 60～100 ℃ hot water extraction, solid-liquid ratio 1:5～1:30 (w/v of residue and hot water, g/mL), 1～8 hour extraction time, extraction time 1～5 time.United extraction liquid, be concentrated into 1/2～1/3 of original volume, add trichoroacetic acid(TCA) and make that pH value of solution is 1～3, ice bath is the centrifugal precipitation of removing after 2～8 hours, regulator solution pH value is to neutral, concentrate neutral solution to 1/2～1/3 of original volume, add ethanol and make that ethanol content reaches 60～80% (v/v) in the solution, ethanol can be medical ethanol or dehydrated alcohol, standing over night, with dehydrated alcohol, acetone, anhydrous diethyl ether washing, vacuum-drying promptly gets shizandra berry Crude polysaccharides powder successively for suction filtration, precipitation.
The invention has the advantages that provides a kind of method of comprehensive utilization that can utilize lignanoid and two kinds of activeconstituentss of polysaccharide in the shizandra berry simultaneously, for the utilization of shizandra berry residue provides a new way.
Description of drawings
Fig. 1 shizandra berry method of comprehensive utilization flow process
Embodiment:
Comparative Examples 1:
On the south the schisandra fruit powder be raw material, solid-liquid ratio 1:20 (w/v, g/mL), boiling water refluxing extraction 6 hours is extracted 1 time, filter, filtrate decompression concentrates, and concentrated solution adopts trichloroacetic acid method to remove albumen, adds 95% long-pending ethanol sedimentation of triploid in the filtrate, with dehydrated alcohol, acetone, anhydrous diethyl ether washing, vacuum-drying gets shizandra berry Crude polysaccharides powder to precipitation successively.Kadsura longepedunculata Crude polysaccharides yield is 12.8%, and it is 32.2% that the phenolsulfuric acid method records polysaccharide content.
Comparative Examples 2;
To the north of the schisandra fruit powder be raw material, operate with method by Comparative Examples 1.After measured, Schisandra chinensis Crude polysaccharides yield is 20.1%, and it is 29.6% that the phenolsulfuric acid method records polysaccharide content.
Embodiment 1:
On the south the schisandra fruit powder be raw material, take by weighing the 20g supercritical CO of packing into
2Extraction plant is at CO
2Static extracting was 5 hours when pressure was 35 ℃ of 25MPa, extraction temperature; Then at extracting pressure 25MPa, 35 ℃ of extraction temperature, CO
2Under the flow 2L/min condition, dynamic extraction 3 hours, separation temperature is 60 ℃, collects kadsura longepedunculata extract and extract remainder residue.With the Wuweizi ester A is reference substance, the chromotropic acid colour developing, and spectrophotometry lignanoid content, the result is a total lignans extraction yield 95.5% in the kadsura longepedunculata extract, lignanoid's content 9.2%.
With the kadsura longepedunculata supercritical CO
2The extract remainder residue is a raw material, and solid-liquid ratio 1:20 (w/v, g/mL), boiling water refluxing extraction 6 hours, extract 1 time, filter, filtrate decompression is concentrated into 1/3 of original volume, concentrated solution adopts trichloroacetic acid method to remove albumen, add trichoroacetic acid(TCA) and make that pH value of solution is 2, ice bath is the centrifugal sedimentation and filtration of removing after 4 hours, adds the long-pending medical ethanol precipitation of triploid in the filtrate, with dehydrated alcohol, acetone, anhydrous diethyl ether washing, vacuum-drying gets shizandra berry Crude polysaccharides powder to precipitation successively.The Crude polysaccharides yield is 13.5% in the kadsura longepedunculata supercritical CO 2 extract remainder after measured, and it is 33.6% that the phenolsulfuric acid method records polysaccharide content.
Embodiment 2:
To the north of the schisandra fruit powder be raw material, press embodiment 1 and operate with method.With the Wuweizi ester A is reference substance, the chromotropic acid colour developing, and spectrophotometry lignanoid content, the result is a total lignans extraction yield 93.2% in the Schisandra chinensis extract, lignanoid's content 13.0%.The Schisandra chinensis supercritical CO
2The Crude polysaccharides yield is 19.6% in the extract remainder residue, and it is 28.5% that the phenolsulfuric acid method records polysaccharide content.
Embodiment 3:
On the south the schisandra fruit powder be raw material, (w/v, g/mL), the lignanoid in 60% ethanolic soln (v/v) the refluxing extraction shizandra berry extracts each 2 hours 2 times to solid-liquid ratio 1:10.Filter, the filtrate vacuum concentration gets extract medicinal extract, collects the alcohol extracting residue.With the Wuweizi ester A is reference substance, the chromotropic acid colour developing, and spectrophotometry lignanoid content, the result is total lignans extraction yield 70.8% in the Fructus Schisandrae Sphenantherae extract, lignanoid's content 3.6%.
With the residue after the kadsura longepedunculata 60% extraction using alcohol lignanoid is raw material, solid-liquid ratio 1:20 (w/v, g/mL), boiling water refluxing extraction 6 hours, extract 1 time, filter, filtrate decompression contracts to 1/3 of original volume, concentrated solution adopts trichloroacetic acid method to remove albumen, adds trichoroacetic acid(TCA) and makes that pH value of solution is 2, and ice bath is the centrifugal sedimentation and filtration of removing after 4 hours, filter, add 95% long-pending ethanol sedimentation of triploid in the filtrate, with dehydrated alcohol, acetone, anhydrous diethyl ether washing, vacuum-drying gets shizandra berry Crude polysaccharides powder to precipitation successively.The Crude polysaccharides yield is 9.25% in the kadsura longepedunculata alcohol extracting residue after measured, and it is 36.9% that the phenolsulfuric acid method records polysaccharide content.
Embodiment 4:
To the north of the schisandra fruit powder be raw material, press embodiment 3 and operate with method.With the Wuweizi ester A is reference substance, the chromotropic acid colour developing, and spectrophotometry lignanoid content, the result is total lignans extraction yield 57% in the Radix Schisandrae Bicolori extract, lignanoid's content 3.0%.The Crude polysaccharides yield is 13.5% in the Schisandra chinensis 60% alcohol extracting residue, and polysaccharide content is 28.3%.
Method of comprehensive utilization of the present invention all can effectively be utilized activeconstituents lignanoid in the schisandra chinensis medicinal material and polysaccharide, can significantly improve the comprehensive utilization value of shizandra berry.
Claims (5)
1, a kind of method that fully utilizes shizandra berry is characterized in that: with the schisandra fruit powder is raw material, at first adopts supercritical CO
2Fluid extraction method or alcohol extracting method extract the activeconstituents lignanoid in the shizandra berry; Extract the shizandra berry polysaccharide the residue of reusable heat water extraction method after extracting lignanoid.
2, a kind of method that fully utilizes shizandra berry according to claim 1 is characterized in that: supercritical CO
2The concrete steps that the fluid extraction method is extracted activeconstituents lignanoid are: with the schisandra fruit powder is raw material, under 30～50 ℃ of extracting pressure 20～35MPa, extraction temperature, and static extracting or static immersing 2～10 hours; Then at extracting pressure 20～35MPa, 30～50 ℃ of extraction temperature and CO
2Dynamic extraction is 2～6 hours under flow 1～4L/min, obtains shizandra berry lignanoid extract and residue extract remainder.
3, a kind of method that fully utilizes shizandra berry according to claim 1, it is characterized in that: the concrete steps that alcohol extracting method extracts shizandra berry lignanoid are: with the schisandra fruit powder is raw material, refluxing extraction in ethanolic soln, the solid-liquid ratio of fruit powder and ethanolic soln is 1:5～1:20 (w/v, g/mL), alcohol concn is that 60～95% (v/v), extraction time are 1～3 hour, extraction time 1～3 time filters, filtrate concentrate the shizandra berry lignans extract.
4, a kind of method that fully utilizes shizandra berry according to claim 1, it is characterized in that: the concrete steps of the extraction of shizandra berry polysaccharide are in the residue: adopt 60～100 ℃ hot water extraction, solid-liquid ratio 1:5～1:30 (w/v of residue and hot water, g/mL), 1～8 hour extraction time, extraction time 1～5 time, extracting solution is concentrated into 1/2～1/3 of original volume, add trichoroacetic acid(TCA) and make that pH value of solution is 1～3, ice bath is the centrifugal precipitation of removing after 2～8 hours, regulator solution pH value is to neutral, concentrate neutral solution to 1/2～1/3 of original volume, add ethanol and make that ethanol content reaches 60～80% (v/v), standing over night, suction filtration in the solution, precipitation is used dehydrated alcohol successively, acetone, the anhydrous diethyl ether washing, vacuum-drying promptly gets shizandra berry Crude polysaccharides powder.
5, a kind of method that fully utilizes shizandra berry according to claim 3, it is characterized in that: ethanol is medical ethanol.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101766690B (en) * | 2010-02-24 | 2012-10-24 | 哈尔滨仁皇药业股份有限公司 | Multipurpose utilization method for improving the value of schisandra chinensis medicinal material |
| CN102757510A (en) * | 2012-04-28 | 2012-10-31 | 江苏大学 | Low-molecular weight schisandra chinensis polysaccharides and preparation method and application thereof |
| CN102920783B (en) * | 2012-11-14 | 2014-05-07 | 沈阳药科大学 | Process for preparing effective components of schisandrachinensis |
| CN105287729A (en) * | 2014-07-29 | 2016-02-03 | 西安旭煌生物技术有限公司 | Novel method for extracting polysaccharides and total lignans from schisandra chinensis |
| CN107773610A (en) * | 2016-08-25 | 2018-03-09 | 吉林省跨海生化药业制造有限公司 | A kind of Chinese medicine composition and its preparation to chemical damage with auxiliary protection function |
| CN107595695A (en) * | 2017-09-13 | 2018-01-19 | 李德海 | A kind of extracting method of Schisandra chinens P.E and its application |
| CN109021129B (en) * | 2018-07-10 | 2021-01-08 | 广西壮族自治区药用植物园 | Method for extracting black tiger fruit polysaccharide |
| CN112057500A (en) * | 2020-10-16 | 2020-12-11 | 陕西嘉禾药业有限公司 | Method for extracting polysaccharide, volatile oil, flavone and lignan from schisandra chinensis |
| CN112791137B (en) * | 2020-12-30 | 2023-07-04 | 沈嘉 | Three shizandra berry extracts and preparation process and application thereof |
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