CN101744886B - Method for extracting high-purity schisandra total lignan - Google Patents
Method for extracting high-purity schisandra total lignan Download PDFInfo
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- CN101744886B CN101744886B CN2010101198717A CN201010119871A CN101744886B CN 101744886 B CN101744886 B CN 101744886B CN 2010101198717 A CN2010101198717 A CN 2010101198717A CN 201010119871 A CN201010119871 A CN 201010119871A CN 101744886 B CN101744886 B CN 101744886B
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- 238000000605 extraction Methods 0.000 claims abstract description 33
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 235000008422 Schisandra chinensis Nutrition 0.000 claims abstract description 16
- 229930013686 lignan Natural products 0.000 claims abstract description 16
- 150000005692 lignans Chemical class 0.000 claims abstract description 16
- 235000009408 lignans Nutrition 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000284 extract Substances 0.000 claims abstract description 15
- 239000012141 concentrate Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000003480 eluent Substances 0.000 claims description 11
- 238000010828 elution Methods 0.000 claims description 11
- 238000001256 steam distillation Methods 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 6
- 239000010685 fatty oil Substances 0.000 claims description 6
- 239000000049 pigment Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 3
- 240000006079 Schisandra chinensis Species 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 241000736075 Schisandra Species 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 12
- 230000000694 effects Effects 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000000874 microwave-assisted extraction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000713772 Human immunodeficiency virus 1 Species 0.000 description 1
- 241000218377 Magnoliaceae Species 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003064 anti-oxidating 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000029865 regulation of blood pressure Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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Abstract
The invention discloses a method for extracting high-purity schisandra total lignan. The method comprises the following steps: (1) soaking schisandra fruits in water, filtering the soaked schisandra fruits, drying and grinding filter residue for later use; (2) extracting the ground filter residue by a supercritical CO2 method, distilling the obtained extract with steam, concentrating the obtained product under reduced pressure and obtaining concentrate for later use; and (3) purifying the concentrate. The extraction method has the advantages of simple extraction process, high purity of extracted total lignan, thorough impurity removal and the like, and can extract the extract with the total lignan content of over 50 percent from the schisandra fruits.
Description
Technical field
The present invention relates to extraction of effective components in a kind of fruit, relate in particular to a kind of method for distilling of high-purity schisandra total lignan, belong to the extraction field of Fructus Schisandrae Chinensis effective ingredient.
Background technology
(Schisandra chinensis (Turcz.) Ball. is the dry mature fruit of the perennial fallen leaves of Magnoliaceae bejuco to Radix Schisandrae Bicoloris; Its medication is with a long history; Beginning is stated from Shennong's Herbal, is classified as top gradely, has that convergence is astringent or styptic treatment for spontaneous sweating, an effect of supplementing QI for promoting the production of body fluid, kidney calming.Recent studies proves, lignanoid also has central nerve inhibition, anti HIV-1 virus, antioxidation, anticancer, blood pressure regulation and multiple effect such as stable in the Fructus Schisandrae Chinensis except that having function for protecting liver and reducing enzyme activity, is a kind of northern rare Chinese medicine of tunnel.The Chinese patent medicine of selling on the market at present that contains the Fructus Schisandrae Chinensis lignin has folk prescription and compound recipe, and is various in style, but is crude preparation by using, and active constituent content is low, and dose is bigger, and because the existence of a large amount of inert matters causes the generation of some untoward reaction.
The method of at present common extraction schisandra active component lignanoid has several kinds of main method for distilling such as solvent extraction method, microwave extraction method and supercritical fluid extraction.
Solvent extraction method mainly is to adopt water, ethanol, acetone, petroleum ether and chloroform etc. as extracting solvent, extracts through methods such as backflow, dipping, percolation.This method extraction time is long, energy resource consumption is big, and technology is comparatively loaded down with trivial details.Though ask advantages such as short, that solvent load is few, extraction cost is low when ultrasonic extraction has extraction, but still have organic solvent residual.
Summary of the invention
Advantages such as technical problem to be solved by this invention is the deficiency that overcomes prior art, and a kind of method for distilling of high-purity schisandra total lignan is provided, and it is simple that this method for distilling has extraction process, and the total lignans purity of extraction is high, and Impurity removal is thorough.
Technical problem to be solved by this invention realizes by the following technical programs:
A kind of method for distilling of high-purity schisandra total lignan may further comprise the steps:
(1) fruit of Fructus Schisandrae Chinensis is soaked in water; Fruit of Fructus Schisandrae Chinensis after the immersion filters, and the filtering residue oven dry is pulverized, and is subsequent use; (2) filtering residue after will pulverizing is used supercritical CO
2Method extract, the extract that obtains with steam distillation after concentrating under reduced pressure, concentrate is subsequent use; (3), promptly get highly purified Fructus Schisandrae Chinensis total lignanoid with the concentrate purification.
In order to reach better extraction effect, preferred, in the step (1) with static immersing in the tangible water of Schisandra fruit 18～24 hours, the solid-liquid ratio of fruit and water be 1: 6～1: 10 (w/v, g/mL); The present invention is soaked in water fruit of Fructus Schisandrae Chinensis, refilters, and contains water soluble ingredients such as pigment, vitamin and organic acid in the filtrating, so just can remove the water-solubility impurity in the fruit of Fructus Schisandrae Chinensis.
Supercritical CO described in the step (2)
2Extraction preferably carries out under following condition: extracting pressure is that 25～35MPa, extraction temperature are 30～50 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1～2 hour; Steam distillation described in the step (2) is preferably under steam temperature is 100～120 ℃ temperature and distilled 1～8 hour;
Supercritical fluid extraction is compared with microwave extraction method with solvent extraction method, is to adopt nontoxic, nonflammable explosive, inexpensive CO
2As extractant; It is residual to have organic solvent-free; Simplified technology greatly, the loss of avoiding factor such as long period heating that effective ingredient is caused has simultaneously that extraction equipment is simple, high, impure characteristics such as few of time weak point, processing ease, effective component extraction rate.
Preferably, purification comprises described in the step (3): concentrate through absorption with macroporous adsorbent resin, is used ethanol elution, and through the decolorizing resin decolouring, eluent is concentrated, dry again for eluent; Preferred, when using macroporous adsorption resin chromatography, adopt concentration to be lower than 35% ethanol elution removal part fatty oil earlier, adopt concentration to be higher than 85% ethanol elution afterwards, the gained eluent is removed the residue pigment again through the decolorizing resin decolouring.Wherein, described ethanol can be medical alcohol or dehydrated alcohol.
The contained chemical constituent of Fructus Schisandrae Chinensis also contains inert matters such as great amount of fat oil, organic acid, volatile oil and pigment except the lignanoid of biologically active.The present invention adopts water seaoning to remove water-solubility impurity and most of pigments such as organic acid; Adopt steam distillation to remove volatile oil; Adopt low-concentration ethanol eluting macroporous adsorbent resin to remove the part fatty oil, remove the residue pigment, thereby improve the content of total lignans with decolorizing resin.
Advantages such as it is simple that method for distilling of the present invention has extraction process, and the total lignans purity of extraction is high, and Impurity removal is thorough can be extracted from fruit of Fructus Schisandrae Chinensis and obtain total lignans content at the extract more than 50%.
Description of drawings
The flow chart of the method for distilling of Fig. 1 high-purity schisandra total lignan of the present invention.
The specific embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment with form or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall within the scope of protection of the present invention the details of technical scheme of the present invention.
Embodiment 1
With static immersing in the tangible water of Schisandra fruit 22 hours, the solid-liquid ratio of fruit and water be 1: 8 (w/v, g/mL); Fruit of Fructus Schisandrae Chinensis after soaking is filtered, and the filtering residue oven dry is pulverized, and is subsequent use; (2) filtering residue after will pulverizing is used supercritical CO
2Extraction, described supercritical CO
2Extraction carries out under following condition: extracting pressure is that 30MPa, extraction temperature are 40 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1.5 hours; With the steam distillation 6h of the extract that obtains with 110 ℃, concentrating under reduced pressure obtains concentrate, and is subsequent use; (3) with concentrate
Through absorption with macroporous adsorbent resin, adopt 30% ethanol elution to remove the part fatty oil earlier, adopt 85% ethanol elution afterwards, through the decolorizing resin decolouring, eluent is concentrated, dry, promptly gets again for eluent; Through detecting, contain the total lignans of 73.5wt% in the extract of the present invention.
Embodiment 2
With static immersing in the tangible water of Schisandra fruit 24 hours, the solid-liquid ratio of fruit and water be 1: 6 (w/v, g/mL); Fruit of Fructus Schisandrae Chinensis after soaking is filtered, and the filtering residue oven dry is pulverized, and is subsequent use; (2) filtering residue after will pulverizing is used supercritical CO
2Extraction, described supercritical CO
2Extraction carries out under following condition: extracting pressure is that 35MPa, extraction temperature are 50 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 2 hours; With the steam distillation 1h of the extract that obtains with 120 ℃, concentrating under reduced pressure obtains concentrate, and is subsequent use; (3) with concentrate
Through absorption with macroporous adsorbent resin, adopt 20% ethanol elution to remove the part fatty oil earlier, adopt 95% ethanol elution afterwards, through the decolorizing resin decolouring, eluent is concentrated, dry, promptly gets again for eluent; Through detecting, contain the total lignans of 87.2wt% in the extract of the present invention.
Embodiment 3
With static immersing in the tangible water of Schisandra fruit 18 hours, the solid-liquid ratio of fruit and water be 1: 10 (w/v, g/mL); Fruit of Fructus Schisandrae Chinensis after soaking is filtered, and the filtering residue oven dry is pulverized, and is subsequent use; (2) filtering residue after will pulverizing is used supercritical CO
2Extraction, described supercritical CO
2Extraction carries out under following condition: extracting pressure is that 25MPa, extraction temperature are 30 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1 hour; With the steam distillation 8h of the extract that obtains with 100 ℃, concentrating under reduced pressure obtains concentrate, and is subsequent use; (3) with concentrate
Through absorption with macroporous adsorbent resin, adopt 15% ethanol elution to remove the part fatty oil earlier, adopt 85% ethanol elution afterwards, through the decolorizing resin decolouring, eluent is concentrated, dry, promptly gets again for eluent; Through detecting, contain the total lignans of 63.8wt% in the extract of the present invention.
Claims (1)
1. the method for distilling of a high-purity schisandra total lignan may further comprise the steps:
(1) fruit of Fructus Schisandrae Chinensis was soaked in water 24 hours, by g/mL, the solid-liquid ratio of fruit and water is 1: 6; Fruit of Fructus Schisandrae Chinensis after the immersion filters, and the filtering residue oven dry is pulverized, and is subsequent use; (2) filtering residue after will pulverizing adopts supercritical CO
2Method extract supercritical CO
2Extraction carries out under following condition: extracting pressure is that 35MPa, extraction temperature are 50 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 2 hours; The extract that obtains is with 120 ℃ of steam distillations 1 hour, concentrating under reduced pressure behind the steam distillation, and concentrate is subsequent use; (3) with the concentrate purification, through absorption with macroporous adsorbent resin, employing concentration is 20% ethanol elution removal part fatty oil earlier with concentrate; Adopt the ethanol elution of concentration 95% afterwards, the gained eluent is removed the residue pigment again through the decolorizing resin decolouring; Eluent is concentrated, dry, promptly gets.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101198717A CN101744886B (en) | 2010-02-24 | 2010-02-24 | Method for extracting high-purity schisandra total lignan |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101198717A CN101744886B (en) | 2010-02-24 | 2010-02-24 | Method for extracting high-purity schisandra total lignan |
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| Publication Number | Publication Date |
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| CN101744886A CN101744886A (en) | 2010-06-23 |
| CN101744886B true CN101744886B (en) | 2012-07-04 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408947A (en) * | 2011-10-08 | 2012-04-11 | 伊通满族自治县吉云鹿业发展有限公司 | CO (carbon monoxide)2Supercritical extraction method of schisandra kernel essential oil |
| CN102872197A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Chinese magnoliavine fruit extract and preparation method thereof |
| CN103467438B (en) * | 2013-09-18 | 2015-04-22 | 浙江工业大学 | Method for extracting, separating and preparing lignin monomers from schisandra chinensis |
| CN103694213B (en) * | 2013-09-18 | 2015-10-28 | 浙江工业大学 | A kind of extraction and isolation preparation method of Lignans in Schisandra chinensis monomer |
| US9662367B2 (en) * | 2014-08-01 | 2017-05-30 | Rubikon Ltd. | Adaptogenic compositions and method for production thereof |
| CN105232774A (en) * | 2015-10-28 | 2016-01-13 | 青海尤尼克生物技术有限公司 | Lycium barbarum pigment extract and preparation method thereof |
| CN105327001A (en) * | 2015-10-28 | 2016-02-17 | 青海尤尼克生物技术有限公司 | Lycium ruthenicum Murr. pigment extract and preparation method thereof |
| CN107595695A (en) * | 2017-09-13 | 2018-01-19 | 李德海 | A kind of extracting method of Schisandra chinens P.E and its application |
| CN111875483B (en) * | 2020-08-25 | 2022-11-29 | 长春工业大学 | Method for extracting lignanoid compounds from schisandra chinensis |
| 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 |
| CN117224584B (en) * | 2023-08-31 | 2025-05-30 | 汉济生物科技（武汉）有限公司 | Preparation method of total lignans from Herba Lycopodiellae and application thereof in preparation of antithrombotic drugs |
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