CN1733131A - Schisandra fruit extractive, its preparation process and purposes - Google Patents
Schisandra fruit extractive, its preparation process and purposes Download PDFInfo
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- CN1733131A CN1733131A CN 200410058311 CN200410058311A CN1733131A CN 1733131 A CN1733131 A CN 1733131A CN 200410058311 CN200410058311 CN 200410058311 CN 200410058311 A CN200410058311 A CN 200410058311A CN 1733131 A CN1733131 A CN 1733131A
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- fructus schisandrae
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Abstract
The invention relates to a Schisandra fruit extractive containing at least 50% lignans, its preparing process and the use of the extract in preparing medicaments for treating hepatitis, nervous prostration and antisenescence.
Description
Technical field:
The present invention relates to a kind of Fructus Schisandrae Chinensis extrat that contains at least 50% total lignans, its preparation method, and this extract is in preparation treatment hepatitis, neurasthenia, the application in the anti-ageing medicine of waiting for a long time.
Background technology
Fructus Schisandrae Chinensis is the fruit of Schisandraceae Schizandra Radix Schisandrae Bicoloris (Schisandra chinensis Baill) and schisandra chinensis (Schisandra sphenanthera Rehd.Et Wils), is called Radix Schisandrae Bicoloris and Fructus Schisandrae Sphenantherae.Effects such as China's successive dynasties medical information has all been put down in writing Fructus Schisandrae Chinensis the kidney invigorating, and QI invigorating is promoted the production of body fluid, and is astringent or styptic treatment for spontaneous sweating are one of conventional Chinese medicines.Last century, early seventies China clinical discovery Fructus Schisandrae Chinensis honeyed pill and Fructus Schisandrae Chinensis powder had all kinds of reduction hepatitis (to comprise acute infectious hepatitis, chronic and chronic persistent hepatitis and toxic hepatitis) patients serum's glutamate pyruvate transaminase effect and can improve patient's symptom (Lanzhou institute of traditional Chinese medicine of army contagious department, new medicine magazine 1973,9,16; P.L.A. 309 Hospital's internal medicine, new medicine magazine 1973,1,19; 9,18).The ethanol extraction of pharmacological tests explanation seed of Fructus Schisandrae Chinensis can obviously reduce the high serum transaminase that causes with carbon tetrachloride etc. and nervus centralis is had inhibitory action.From then on institute of Materia Medica,Chinese Academy of Medical Sciences plant chamber is separated in the ethanol extraction and is obtained deoxyschizandrin, second element, third element, pure first, pure second, seven lignanoids of ester first, ester the second grade, all has effects such as the serum glutamic pyruvic transminase of reduction, antioxidation, inhibition nervus centralis.Wherein schisandrin B and the schisantherin B activity is the most remarkable and content is the highest (Chinese herbal medicine modern study, the first volume, institute of Materia Medica,Chinese Academy of Medical Sciences is write, combined publication society of China Concord Medical Science University of Beijing Medical University, 349-377). developed transaminase lowering medicine schizandrol sheet and capsule of schisandra fruit on this basis in 1976.Selling the Chinese patent medicine that contains Fructus Schisandrae Chinensis at present on the market has folk prescription and compound recipe, various in style, is crude preparation by using, and active constituent content is low, and dose is bigger.As the content for preparing total lignans in the schizandrol extractum of schizandrol sheet and capsule of schisandra fruit only is 10%, and the existence of a large amount of inert matters causes the generation of some untoward reaction, as phenomenons such as gastrointestinal upset.
Summary of the invention
The defective and the deficiency that the objective of the invention is to exist at above-mentioned prior art provide a kind of Fructus Schisandrae Chinensis extrat that is rich in schisandra active component and preparation method thereof.
Another object of the present invention provides above-mentioned Fructus Schisandrae Chinensis extrat and the application of preparation in pharmaceutical field thereof, particularly the application in preparation treatment hepatitis, neurasthenia, the anti-ageing medicine of waiting for a long time.
Therefore, first aspect present invention relates to a kind of Fructus Schisandrae Chinensis extrat, and it contains at least 50% total lignans.
Further aspect of the present invention relates to the preparation method of the Fructus Schisandrae Chinensis extrat that contains at least 50% total lignans, and it comprises:
(1) with the Fructus Schisandrae Chinensis decocting in water, remove peel, drying is pulverized, and removes volatile oil through steam distillation then;
(2) be selected from a kind of pure room temperature or the heating and refluxing extraction in methanol, ethanol, isopropyl alcohol or n-butyl alcohol of 50-95%, place spend the night after treatment by extracting solution for Fructus Schisandrae Chinensis, and upper strata liquid obtains equivalent extract through normal pressure or concentrating under reduced pressure;
(3) this extractum is with twice of 90% alcohol reflux, reclaim ethanol, residue distributes in organic solvent and aqueous alkali or alkaline dilute alcohol solution (determining alcohol is below 50%), organic layer through washing, dry, obtain total lignans content at the extract more than 50% after concentrating.
The invention still further relates to a kind of product, it comprises Fructus Schisandrae Chinensis extrat and excipient or the carrier that contains at least 50% total lignans.
The invention further relates to the Fructus Schisandrae Chinensis extrat that contains at least 50% total lignans prevents and/or treats or alleviates purposes in the product of disease or symptom in preparation.
According to the present invention, " % " in the extract of the present invention is percentage by weight.
According to the present invention, described disease or symptom have been said for example: hepatitis, neurasthenia, aging.
According to the present invention, alleged excipient of the present invention or carrier are said for example and are excipient or carrier commonly used in food or the pharmaceutical production.
According to the present invention, product can be functional food or medicine among the present invention.
According to the present invention, Fructus Schisandrae Chinensis is said for example and be can be Radix Schisandrae Bicoloris or Fructus Schisandrae Sphenantherae among the present invention.
According to the present invention, Fructus Schisandrae Chinensis extrat of the present invention also can with Chinese medicine couplings such as Radix Salviae Miltiorrhizae, Radix Ginseng, the Radix Astragali.
Further, the preparation method of Fructus Schisandrae Chinensis extrat of the present invention comprises:
Fructus Schisandrae Chinensis is removed sarcocarp through decocting in water, isolates seed, dries, and pulverizes, and steam distillation is removed volatile oil; Doubly measure the methanol of 50-95% with 3-10, ethanol, a kind of room temperature in isopropyl alcohol or the n-butyl alcohol or heating and refluxing extraction 2-3 time, filter, a filtrate 20-50 ℃ placement is spent the night, upper strata liquid through normal pressure or concentrating under reduced pressure to finite concentration, this extractum is with twice of 90% alcohol reflux, reclaim ethanol, residue is at aqueous alkali or alkaline dilute alcohol solution (alkaline solution available hydrogen sodium oxide, the aqueous solution of potassium hydroxide or sodium carbonate is formulated) the middle back organic solvent (dichloromethane that distributes, chloroform, carbon tetrachloride, ethyl acetate, a kind of or several mixed solvents in toluene or the petroleum ether) extraction, organic layer is through washing, dry, concentrate and obtain total lignans content at the Fructus Schisandrae Chinensis extrat more than 50%, this Fructus Schisandrae Chinensis extrat is through recrystallization, gel filtration chromatography, silica gel column chromatography, macroporous adsorption resin chromatography, mixing purification process such as silica gel or kieselguhr backflow can bring up to the content of total lignans more than 70%.The content of lignanoid can be measured with ultraviolet spectrophotometry or high-efficient liquid phase technique.
The contained chemical constituent of Fructus Schisandrae Chinensis also contains a large amount of fatty oil (about about 34%), organic acid (about about 20%), volatile oil (about about 3%), resin inert matters such as (about about 8%) except bioactive lignanoid is arranged.The present invention adopts vapor distillation to remove volatile oil, and alcohol extract is at the 20-50 ℃ of placement fatty oil that can settle out that spends the night, and distributes with aqueous alkali and organic solvent and can remove organic acid and part fatty oil, thereby improve the content of total lignans.
The Fructus Schisandrae Chinensis extrat that utilizes the inventive method to obtain contains total lignans at least 50%, and preferably at least 70%, more preferably at least 75%.
The Fructus Schisandrae Chinensis extrat that utilizes the inventive method to obtain can be used for preparing said preparation on the pharmaceutics, for example: tablet, capsule, drop pill etc.
When the Fructus Schisandrae Chinensis extrat that utilizes the present invention to obtain prepares the various dosage form of required medicine, can be according to the conventional production method preparation of pharmaceutical field.
The specific embodiment
The following examples can further specify the present invention, but do not limit the present invention in any way.
Embodiment 1:
Radix Schisandrae Bicoloris 3kg adds water, and heating kept slight boiling condition 2 hours, rubs with the hands and removes sarcocarp, tells seed, dries, and gets the 1kg seed.Pulverize, steam distillation, residue dries, and adds 4L 85% ethanol, reflux 2 times, each 1.5 hours.Filter, 35 ℃ of insulations of filtrate standing over night, upper strata liquid concentrate thick paste 125g.This thick paste reclaims ethanol with 90% alcohol reflux twice, gets thick paste 120g.Thick paste adds 50% ethanol and disperses, and 1% sodium hydroxide solution transfers to pH=10, chloroform extraction, and the extract anhydrous sodium sulfate drying reclaims chloroform, gets the brown extract of 95 grams, total lignans content 60%.This extract is mixed kieselguhr, and ethyl acetate backflow 5h gets the 80g total lignans, content 70%.
Embodiment 2:
Radix Schisandrae Bicoloris 3kg adds water, and heating kept slight boiling condition 2 hours, rubs with the hands and removes sarcocarp, tells seed, dries, and gets the 1kg seed.Pulverize, steam distillation, residue dries, and adds 4L 75% ethanol, reflux 2 times, each 1.5 hours.Filter, 35 ℃ of insulations of filtrate standing over night, upper strata liquid concentrate thick paste 115g.This thick paste reclaims ethanol with 90% alcohol reflux twice, gets thick paste 110g.Thick paste adds 50% ethanol and disperses, and 1% sodium hydroxide solution transfers to pH=10, petroleum ether: the washing of ethyl acetate (7: 3) extract, reclaim solvent, and get the brown extract of 90 grams, total lignans content 60%.This extract gets the 75g total lignans, content 75% through gel filtration chromatography.
Pharmacological evaluation
Fruit of Chinese magnoliavine effective part causes the protective effect of chmice acute hepatic injury to carbon tetrachloride
[experiment material]
1. laboratory animal: Kunming mouse, male, body weight 18-22 gram is provided by Institute of Experimental Animals, Chinese Academy of Medical Sciences's breeding field, and two grades, the quality certification number: SCXK (capital)-11-00-0006.
2. be subjected to reagent thing: embodiment 1 Fructus Schisandrae Chinensis extrat (total lignans content 60%), the time spent is with the 0.5%CMC-Na suspendible.
3. positive control drug: bifendate drop pill (DDB), purity＞99%, the time spent is with the 0.5%CMC-Na suspendible.
[experimental technique]
Animal is divided into 4 groups at random, is respectively normal control group, carbon tetrachloride model group, bifendate drop pill positive drug control group, is subjected to the reagent group.Positive drug control group and be subjected to reagent group 24,8 and 1 hours oral bifendate drop pill and be subjected to reagent (200 milligrams/kilogram) respectively before giving carbon tetrachloride, normal control group and carbon tetrachloride model group give with the volume excipient.Except that the normal control group, all the other respectively organize equal lumbar injection 0.14% carbon tetrachloride Semen Maydis oil solution, and volume 10ml/kg puts to death the preceding overnight fasting of animal.With the animal sacrificed by decapitation, get blood and separation of serum after 16 hours, measure Serum ALT and AST content.
[experimental result]
After the intact animal gave 0.14% carbon tetrachloride, Serum ALT and AST obviously raise.The positive control drug bifendate drop pill has tangible reduction ALT and AST effect, and it is suitable with contrast medicine bifendate that the ALT effect falls in Fructus Schisandrae Chinensis extrat, falls the AST effect and slightly be better than bifendate (the results are shown in Table 1)
Table 1: fruit of Chinese magnoliavine effective part causes the protective effect of chmice acute hepatic injury to carbon tetrachloride
| Group | Dosage (mg/kg) | ALT | AST | ||
| Toll bar formula unit | Suppression ratio (%) | Toll bar formula unit | Suppression ratio (%) | ||
| The normal control group | 79.4±15.8 | 125.6±19.0 | |||
| Model group | 359.3±256.5 ## | 352.43↑ | 274.4±109.2 ### | 118.40↑ | |
| The DDB drop pill | 200 | 235.5±123.6 | 34.46 | 209.9±104.6 | 23.51 |
| Embodiment 1 extract | 200 | 247.8±154.7 | 31.02 | 191.3±71.8 | 30.27 |
Annotate: every group number of animals is 10
Claims (10)
1. Fructus Schisandrae Chinensis extrat, it contains at least 50 weight % total lignans.
2. the Fructus Schisandrae Chinensis extrat of claim 1, it contains at least 70 weight % total lignans.
3. claim 1 or 2 extract, wherein Fructus Schisandrae Chinensis is Fructus Schisandrae Sphenantherae or Radix Schisandrae Bicoloris.
4. product, it comprises Fructus Schisandrae Chinensis extrat and excipient or carrier that claim 1-3 is arbitrary.
5. a method for preparing Fructus Schisandrae Chinensis extrat is characterized in that this method comprises the following steps: successively
(1) with the Fructus Schisandrae Chinensis decocting in water, remove peel, drying is pulverized, and removes volatile oil through steam distillation then;
(2) be selected from a kind of pure room temperature or the heating and refluxing extraction in methanol, ethanol, isopropyl alcohol or n-butyl alcohol of 50-95%, place spend the night after treatment by extracting solution for Fructus Schisandrae Chinensis, and upper strata liquid obtains equivalent extract through normal pressure or concentrating under reduced pressure;
(3) this extractum is with twice of 90% alcohol reflux, reclaim ethanol, residue distributes in organic solvent and aqueous alkali or alkaline dilute alcohol solution (determining alcohol is below 50%), organic layer through washing, dry, obtain total lignans content at the extract more than 50% after concentrating.
6. preparation method according to claim 1, it is characterized in that it is 20-50 ℃ that extracting solution is placed the temperature of spending the night, used organic solvent is a kind of or several mixed solvents in dichloromethane, chloroform, carbon tetrachloride, ethyl acetate, toluene or the petroleum ether, and used aqueous alkali is the aqueous solution that sodium hydroxide, potassium hydroxide or sodium carbonate are mixed with.
7. preparation method according to claim 5, it comprises and is further purified step, described purification is selected from recrystallization, gel filtration chromatography, silica gel column chromatography or macroporous adsorption resin chromatography, perhaps their combination, perhaps extractum is mixed in silica gel or kieselguhr, dried the back with the organic solvent eluting that refluxes.
8. purification process according to claim 5 is characterized in that the used solvent of eluting is a kind of or several mixed solvents in petroleum ether, ether, dichloromethane, chloroform, ethyl acetate, benzene, toluene, acetone, methanol, ethanol, isopropyl alcohol, the n-butyl alcohol.
9. product according to claim 4, it is tablet, capsule or drop pill.
10. according to the purposes of the arbitrary described Fructus Schisandrae Chinensis extrat of claim 1-3 in preparation prevention or treatment hepatitis, neurasthenia or anti-aging product.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200410058311XA CN1327859C (en) | 2004-08-11 | 2004-08-11 | Schisandra fruit extractive, its preparation process and purposes |
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| CNB200410058311XA CN1327859C (en) | 2004-08-11 | 2004-08-11 | Schisandra fruit extractive, its preparation process and purposes |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101978990A (en) * | 2010-09-30 | 2011-02-23 | 曹云峰 | Schisandra extract and preparation method and application thereof |
| CN101433587B (en) * | 2007-11-12 | 2011-09-21 | 天津天士力制药股份有限公司 | Effective component of Schisandra chinensis and preparation method thereof |
| CN102492049A (en) * | 2011-11-30 | 2012-06-13 | 天津大学 | Method of extracting polysaccharide, volatile oil and lignans from Schisandra chinensis |
| CN103141833A (en) * | 2013-02-04 | 2013-06-12 | 北华大学 | Health food with anti-aging effect and preparation method thereof |
| CN104297363A (en) * | 2014-09-05 | 2015-01-21 | 浙江工业大学 | Method for discriminating Schisandra chinensis and Kadsura longepedunculata through combination of flash evaporation gas chromatography-mass spectrometry and fingerprint |
| CN105853567A (en) * | 2016-03-22 | 2016-08-17 | 中国中医科学院中医临床基础医学研究所 | Traditional Chinese medicine composition for treating hyperthyroidism and preparation method thereof |
| CN108034492A (en) * | 2018-02-01 | 2018-05-15 | 无限极（中国）有限公司 | A kind of extracting method of magnolia vine fruit oil |
| CN108339023A (en) * | 2017-01-22 | 2018-07-31 | 中国中医科学院中医基础理论研究所 | The method for extracting fructus schizandrae total lignans |
| CN109984974A (en) * | 2019-05-13 | 2019-07-09 | 无限极（中国）有限公司 | Schisandra chinens P.E, preparation method and its application in cosmetics |
| CN115844970A (en) * | 2023-02-28 | 2023-03-28 | 广东青云山药业有限公司 | A Chinese medicinal composition containing fructus Schisandrae extract and its preparation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1476881A (en) * | 2003-07-10 | 2004-02-25 | 张玉贵 | Compound Chinese medicine for curing hepatic disease |
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2004
- 2004-08-11 CN CNB200410058311XA patent/CN1327859C/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101433587B (en) * | 2007-11-12 | 2011-09-21 | 天津天士力制药股份有限公司 | Effective component of Schisandra chinensis and preparation method thereof |
| CN101978990A (en) * | 2010-09-30 | 2011-02-23 | 曹云峰 | Schisandra extract and preparation method and application thereof |
| CN101978990B (en) * | 2010-09-30 | 2013-06-05 | 曹云峰 | Schisandra extract and preparation method and application thereof |
| CN102492049A (en) * | 2011-11-30 | 2012-06-13 | 天津大学 | Method of extracting polysaccharide, volatile oil and lignans from Schisandra chinensis |
| CN103141833A (en) * | 2013-02-04 | 2013-06-12 | 北华大学 | Health food with anti-aging effect and preparation method thereof |
| CN104297363A (en) * | 2014-09-05 | 2015-01-21 | 浙江工业大学 | Method for discriminating Schisandra chinensis and Kadsura longepedunculata through combination of flash evaporation gas chromatography-mass spectrometry and fingerprint |
| CN105853567A (en) * | 2016-03-22 | 2016-08-17 | 中国中医科学院中医临床基础医学研究所 | Traditional Chinese medicine composition for treating hyperthyroidism and preparation method thereof |
| CN108339023A (en) * | 2017-01-22 | 2018-07-31 | 中国中医科学院中医基础理论研究所 | The method for extracting fructus schizandrae total lignans |
| CN108034492A (en) * | 2018-02-01 | 2018-05-15 | 无限极（中国）有限公司 | A kind of extracting method of magnolia vine fruit oil |
| CN109984974A (en) * | 2019-05-13 | 2019-07-09 | 无限极（中国）有限公司 | Schisandra chinens P.E, preparation method and its application in cosmetics |
| CN115844970A (en) * | 2023-02-28 | 2023-03-28 | 广东青云山药业有限公司 | A Chinese medicinal composition containing fructus Schisandrae extract and its preparation method |
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| Publication number | Publication date |
|---|---|
| CN1327859C (en) | 2007-07-25 |
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Address after: 102600 building 7, 37 Yongwang Road, Daxing biomedical industrial base, Zhongguancun Science and Technology Park, Daxing District, Beijing Patentee after: Beijing Xiehe Pharmaceutical Co.,Ltd. Address before: 102600 Xingye Road, Daxing District, Beijing Patentee before: Beijing Union Pharmaceutical Factory |
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