CN101744886A - Method for extracting high-purity schisandra total lignan - Google Patents
Method for extracting high-purity schisandra total lignan Download PDFInfo
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- CN101744886A CN101744886A CN201010119871A CN201010119871A CN101744886A CN 101744886 A CN101744886 A CN 101744886A CN 201010119871 A CN201010119871 A CN 201010119871A CN 201010119871 A CN201010119871 A CN 201010119871A CN 101744886 A CN101744886 A CN 101744886A
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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 extracting method 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 listed in top gradely, has the effect of astringent or styptic treatment for spontaneous sweating, the supplementing QI for promoting the production of body fluid of convergence, 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 that contains the Fructus Schisandrae Chinensis lignin has folk prescription and compound recipe at present, 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 main extracting method 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 by 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
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of extracting method of high-purity schisandra total lignan is provided, and it is simple that this extracting method has extraction process, the total lignans purity height of extraction, advantage such as Impurity removal is thorough.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of extracting method 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 standby; (2) the filtering residue supercritical CO after will pulverizing
2Method extract, the extract that obtains with steam distillation after concentrating under reduced pressure, concentrate is standby; (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 filtrate, 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 the following conditions: 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, time weak point, processing ease, effective component extraction rate height, impure characteristics such as few.
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 a large amount of fatty oils, 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.
It is simple that extracting method of the present invention has extraction process, the total lignans purity height of extraction, and advantage such as 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 extracting method 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 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 solution of the present invention and form.
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 standby; (2) the filtering residue supercritical CO after will pulverizing
2Extraction, described supercritical CO
2Extraction carries out under the following conditions: extracting pressure is that 30MPa, extraction temperature are 40 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1.5 hours; With the extract that the obtains steam distillation 6h with 110 ℃, concentrating under reduced pressure obtains concentrate, and is standby; (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 again for eluent; After testing, the total lignans that contains 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 standby; (2) the filtering residue supercritical CO after will pulverizing
2Extraction, described supercritical CO
2Extraction carries out under the following conditions: extracting pressure is that 35MPa, extraction temperature are 50 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 2 hours; With the extract that the obtains steam distillation 1h with 120 ℃, concentrating under reduced pressure obtains concentrate, and is standby; (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 again for eluent; After testing, the total lignans that contains 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 standby; (2) the filtering residue supercritical CO after will pulverizing
2Extraction, described supercritical CO
2Extraction carries out under the following conditions: extracting pressure is that 25MPa, extraction temperature are 30 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1 hour; With the extract that the obtains steam distillation 8h with 100 ℃, concentrating under reduced pressure obtains concentrate, and is standby; (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 again for eluent; After testing, the total lignans that contains 63.8wt% in the extract of the present invention.
Claims (8)
1. the extracting method of a 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 standby; (2) filtering residue after will pulverizing adopts supercritical CO
2Method extract, the extract that obtains with steam distillation after concentrating under reduced pressure, concentrate is standby; (3) with the concentrate purification, promptly.
2. it is characterized in that in accordance with the method for claim 1: in the step (1) with static immersing in the tangible water of Schisandra fruit 18～24 hours.
3. according to claim 1 or 2 described methods, it is characterized in that: by g/mL, the solid-liquid ratio of fruit and water is 1: 6～1: 10.
4. it is characterized in that in accordance with the method for claim 1: the supercritical CO described in the step (2)
2Extraction carries out under the following conditions: extracting pressure is that 25～35MPa, extraction temperature are 30～50 ℃, CO
2Flow velocity is 12Kg/h, dynamic extraction 1～2 hour.
5. it is characterized in that in accordance with the method for claim 1: the steam distillation described in the step (2) is meant under steam temperature is 100～120 ℃ temperature and distilled 1～8 hour.
6. in accordance with the method for claim 1, it is characterized in that 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.
7. in accordance with the method for claim 6, it is characterized in that: 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.
8. according to claim 6 or 7 described methods, it is characterized in that: described ethanol is medical alcohol or dehydrated alcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101198717A CN101744886B (en) | 2010-02-24 | 2010-02-24 | Method for extracting high-purity schisandra total lignan |
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| CN2010101198717A CN101744886B (en) | 2010-02-24 | 2010-02-24 | Method for extracting high-purity schisandra total lignan |
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Cited By (10)
| 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 | Method for CO2 supercritical fluid extraction 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 |
| CN103467438A (en) * | 2013-09-18 | 2013-12-25 | 浙江工业大学 | Method for extracting, separating and preparing lignin monomers from schisandra chinensis |
| CN103694213A (en) * | 2013-09-18 | 2014-04-02 | 浙江工业大学 | Extraction separation preparation method of lignin monomers in schisandra chinensis |
| 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 |
| CN105477153A (en) * | 2014-08-01 | 2016-04-13 | 卢比肯股份有限公司 | Adaptogenic compositions and method for production 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 |
| CN111875483A (en) * | 2020-08-25 | 2020-11-03 | 长春工业大学 | Method for extracting lignans 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 |
-
2010
- 2010-02-24 CN CN2010101198717A patent/CN101744886B/en not_active Expired - Fee Related
Cited By (13)
| 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 | Method for CO2 supercritical fluid extraction 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 |
| CN103467438A (en) * | 2013-09-18 | 2013-12-25 | 浙江工业大学 | Method for extracting, separating and preparing lignin monomers from schisandra chinensis |
| CN103694213A (en) * | 2013-09-18 | 2014-04-02 | 浙江工业大学 | Extraction separation preparation method of lignin monomers in 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 |
| CN105477153B (en) * | 2014-08-01 | 2019-11-29 | 卢比肯股份有限公司 | Adapt to former composition and its production method |
| CN105477153A (en) * | 2014-08-01 | 2016-04-13 | 卢比肯股份有限公司 | Adaptogenic compositions and method for production 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 |
| 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 |
| CN107595695A (en) * | 2017-09-13 | 2018-01-19 | 李德海 | A kind of extracting method of Schisandra chinens P.E and its application |
| CN111875483A (en) * | 2020-08-25 | 2020-11-03 | 长春工业大学 | Method for extracting lignans compounds from schisandra chinensis |
| 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 |
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| CN101744886B (en) | 2012-07-04 |
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