CN101214278A - New raw material for extracting fructus schizandrae total lignans and preparation technique and use - Google Patents
New raw material for extracting fructus schizandrae total lignans and preparation technique and use Download PDFInfo
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- CN101214278A CN101214278A CNA2007101591969A CN200710159196A CN101214278A CN 101214278 A CN101214278 A CN 101214278A CN A2007101591969 A CNA2007101591969 A CN A2007101591969A CN 200710159196 A CN200710159196 A CN 200710159196A CN 101214278 A CN101214278 A CN 101214278A
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Abstract
The present invention pertains to the art of medical technology and discloses a novel raw material for Schisandraceae lignans extracted substance and a preparation method thereof. The process takes Chinese medicine Schisandraceae stem (fruit stalk) and Schisandraceae leave as the raw material and adopts one or a plurality of solvent extraction method, resin absorption method, positive-phase column chromatography, reverse-phase column chromatography, etc. after grinding, so as to prepare the extracted substance with 30 to 95 percent of total lignans content. The preparation method has simple process, stable content and good repeatability. The extracted substance can be used as medicine or health food instead of Schisandraceae lignans extracted substance, which makes full use of Schisandraceae resource and releases the short supply of Schisandraceae fruit.
Description
Technical field
The invention belongs to medical technical field, relate to the new raw material and the preparation technology thereof of Fructus Schisandrae Chinensis total lignanoid extract.According to the extract of this preparation technology's gained, the total content of its Lignanoids compounds is at 30-95%.Be used for prevention and treatment hepatitis.
Background technology
The fat-soluble active ingredient of Fructus Schisandrae Chinensis is mainly lignanoid.Its pharmacological action relates to digestive system, cardiovascular system, central nervous system, reproductive system and antioxidation, the anti-ageing various aspects of waiting for a long time (Chinese crude drug the 28th the 2nd phase of volume of February in 2005).
Folium Schisandrae Chinensis and Fructus Schisandrae Chinensis carpopodium (fruit stem) are the dried leaves and the carpopodiums (fruit stem) of Magnoliaceae schisandra plant Radix Schisandrae Bicoloris Schisandra chinensis (Turcz.) Baill., schisandra chinensis Schisandrasphenanthera Rehd.et Wils. and Schizandra other plant.
The foreign scholar uses the CO of high performance liquid chromatograph to Folium Schisandrae Chinensis
2Supercritical extract is analyzed, and finds that it contains the lignanoid identical with fruit of Fructus Schisandrae Chinensis, as (Journal of Chromatography B, 770 (2002) 283289) such as schisandrin, pure second, first element, second element, third element and gomisin N.Contain the lignanoid identical in the Fructus Schisandrae Chinensis carpopodium (fruit stem), as schisandrin, ester first, first element, second element etc. (Yanbian University's medical journal the 28th the 1st phase of volume of March in 2005) with fruit of Fructus Schisandrae Chinensis.
At present, the Fructus Schisandrae Chinensis market demand is very big, do not satisfy the requirement of domestic and international market far away, extinctive cutting having occurred wild resource climingly gathers and destroys, the area that has generally occurs plunderring blue or green phenomenon, makes the Fructus Schisandrae Chinensis resource be subjected in various degree destruction, causes a resource shrinkage of available Fructus Schisandrae Chinensis, downgrade, price are constantly soaring.Fruit was plucked from Cortex et Radix Schisandrae Chinensis with carpopodium (fruit stem) when fruit of Fructus Schisandrae Chinensis was ripe, and carpopodium (fruit stem) is disallowable as impurity, and the Folium Schisandrae Chinensis resource is very abundant especially, if can be with Folium Schisandrae Chinensis and carpopodium (fruit stem) replenishing as Fructus Schisandrae Chinensis lignanoid source, can make full use of resource, turn waste into wealth.
Summary of the invention
The objective of the invention is to provide two kinds of new sources of Fructus Schisandrae Chinensis total lignanoid at above-mentioned schisandra chinensis medicinal material situation in short supply, the preparation technology of two kinds of Fructus Schisandrae Chinensis carpopodiums (fruit stem) and leaf total lignans extract, and the extract and the relevant dosage form thereof that get according to this prepared.As replenishing of Fructus Schisandrae Chinensis resource, substitute fruit of Fructus Schisandrae Chinensis total lignans extract and be used as medicine or health food.
The present invention finishes by following technical solution:
(1), pulverizes decocting in water with Folium Schisandrae Chinensis, carpopodium (fruit stem) drying; With residue drying behind the water extraction, a kind of heating and refluxing extraction of the methanol with 50~95%, ethanol, isopropyl alcohol or n-butyl alcohol, the extracting solution concentrating under reduced pressure is the concentrated solution of density 0.80-1.20; Adopt the macroporous adsorptive resins enrichment, water, 40%~75% ethanol, 95% ethanol elution is collected 95% ethanol elution, the extract that obtains after concentrating, its total lignans weight content is 30%-95%.
(2), pulverize decocting in water with Folium Schisandrae Chinensis, carpopodium (fruit stem) drying; With residue drying behind the water extraction, a kind of heating and refluxing extraction of the methanol with 70~95%, ethanol, isopropyl alcohol or n-butyl alcohol, extracting solution is evaporated to dried, organic solvent room temperature or heating and refluxing extraction, extract adopts the chromatographic column eluting, the extract that obtains behind the eluting, its total lignans weight content is 30%-95%.
According to above prepared and the total lignans extract contain chemical compound: schisandrin, pure second, first element, second element, third element and gomisin G, gomisinL
1, gomisinM
1, gomisinN etc.This extract can mix with acceptable carrier pharmaceutically, makes various useful clinically dosage forms.
Beneficial effect of the present invention
The present invention is directed to and substitute fruit of Fructus Schisandrae Chinensis total lignans extract and be used as medicine or go into health food, make full use of the Fructus Schisandrae Chinensis resource, alleviate the fruit of Fructus Schisandrae Chinensis situation that supply falls short of demand.
The specific embodiment
The following examples can further specify the present invention, but do not limit the present invention in any way.
Embodiment 1:
Chinese cotyledon 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 14L80% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and concentrating under reduced pressure, density is 0.93 concentrated solution 610g.Use the macroporous adsorptive resins enrichment, the difference water, 60% ethanol, 90% ethanol gradient elution, collect 90% ethanol elution, decompression recycling ethanol is used the macroporous adsorptive resins enrichment once more, respectively water, 75% ethanol, 90% ethanol elution is collected 90% ethanol elution, and decompression recycling ethanol obtains the 15g extract.Total lignans content 60%.
Embodiment 2:
Chinese cotyledon 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 14L80% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and decompression recycling ethanol obtain dry extract 130g.With petroleum ether reflux, extract, 3 times, merge extractive liquid,, be evaporated to small size 10ml, by the silica gel column chromatography enrichment, use petroleum ether: behind ethyl acetate (20: the 1) eluting, the reuse petroleum ether: ethyl acetate (2: 1) eluting, collect petroleum ether: ethyl acetate (2: 1) eluent, concentrating under reduced pressure obtains the 10g extract.Total lignans content 65%.
Embodiment 3:
Radix Schisandrae Bicoloris carpopodium (fruit stem) 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 12L90% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and concentrating under reduced pressure, density is 0.91 concentrated solution 650g.Use the macroporous adsorptive resins enrichment, the difference water, 70% ethanol, 90% ethanol gradient elution is collected 90% ethanol elution, and decompression recycling ethanol obtains the 20g extract.Total lignans content 63%.
Embodiment 4:
Radix Schisandrae Bicoloris carpopodium (fruit stem) 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 12L90% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and decompression recycling ethanol obtain dry extract 150g.With petroleum ether reflux, extract, 3 times, merge extractive liquid,, be evaporated to small size 10ml, by the silica gel column chromatography enrichment, use petroleum ether: behind ethyl acetate (20: the 1) eluting, the reuse petroleum ether: ethyl acetate (2: 1) eluting, collect petroleum ether: ethyl acetate (2: 1) eluent, concentrating under reduced pressure obtains the 15g extract.Total lignans content 70%.
Embodiment 5:
Radix Schisandrae Bicoloris carpopodium (fruit stem) 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 12L90% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and decompression recycling ethanol obtain dry extract 150g.With petroleum ether reflux, extract, 3 times, merge extractive liquid,, be evaporated to small size 10ml, silica gel column chromatography, use petroleum ether: behind ethyl acetate (100: 1~1: the 100) gradient elution, merge the same composition eluate, through method purification such as ODS post, high performance liquid chromatogram (HPLC), recrystallization, obtained schisandrin, pure second, first element, second element, third element, gomisin G, gomisinL again
1, gomisinM
1, 25 chemical compounds such as gomisinN.And use nuclear magnetic resonance, NMR (NMR), mass spectrum (MS), infrared spectrum means such as (IR) to determine their structure.
Embodiment 6:
Embodiment 1,2 resulting Folium Schisandrae Chinensis total lignans extracts resulting chemical compound in thin layer chromatography, high performance liquid chromatogram (HPLC) and embodiment 5 is compared, show that it contains schisandrin, pure second, first element, second element, third element, gomisinL
1, gomisinM
1, 14 kinds of lignanoids such as gomisinN.
Embodiment 7:
Radix Schisandrae Bicoloris carpopodium (fruit stem) 2Kg pulverizes, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 12L90% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter, merging filtrate and concentrating under reduced pressure, density is 0.91 concentrated solution 650g.Use the macroporous adsorptive resins enrichment, the difference water, 70% ethanol, 90% ethanol gradient elution is collected 90% ethanol elution, and decompression recycling ethanol obtains the 20g extract.Total lignans content 63%.Add 4g starch, mixing, 80% alcohol granulation, drying adds magnesium stearate 0.3g, mixing, the capsule of packing into No. 1 promptly gets 70 of the hard capsules that the present invention makes.Every contains content 0.3g.
Embodiment 8: the Fructus Schisandrae Chinensis total lignanoid extract is to the therapeutical effect of carbon tetrachloride hepatic injury mice
Get 50 of mices, be divided into 5 groups at random, be respectively normal control group, carbon tetrachloride (CCl
4) model group, fruit of Fructus Schisandrae Chinensis total lignans extract group, embodiment 1 extract group and embodiment 3 extract groups.
Wherein fruit of Fructus Schisandrae Chinensis total lignans preparation method of extract is as follows: the Radix Schisandrae Bicoloris fruit is pulverized, and adds water reflux, extract, twice, keeps slight boiling condition 1.5 hours at every turn, filters, and discards the filtrate of merging.After residue dries, add 90% ethanol, heating and refluxing extraction 3 times, each 2 hours, filter the macroporous adsorptive resins enrichment of merging filtrate and concentrating under reduced pressure, concentrated solution, the difference water, 40% ethanol, 90% ethanol gradient elution is collected 90% ethanol elution, decompression recycling ethanol, decompression recycling ethanol obtain the extract of total lignans content 70%.
Animal experiment method is as follows: except that the normal control group, and every group of first day lumbar injection 0.1%CCl
4Paraffin oil solution (10ml/kg), simultaneously continuous gastric infusion 7 days, 16 hours eye sockets are got blood after the last administration, survey serum glutamic pyruvic transminase (SGPT).
Experimental result sees the following form:
Group (n=10) | Dosage (mg/kg) | SGPT content (U/ml) |
The normal control group | 168.1±27.34 | |
CCl 4Model group | 443.2±47.61 | |
Fruit of Fructus Schisandrae Chinensis total lignans extract group | 200 | 271.3±35.53 |
Embodiment 1 extract group | 200 | 281.4±34.79 |
Embodiment 3 extract groups | 200 | 287.7±36.88 |
Conclusion: CCl4 group mice SGPT is significantly higher than normal control group (P<0.01); Compare with the CCl4 group, fruit of Fructus Schisandrae Chinensis total lignans extract group, embodiment 1 extract group, embodiment 3 extract group SGPT all significantly reduce (P<0.01); Difference there are no significant meaning (P>0.05) between fruit of Fructus Schisandrae Chinensis total lignans extract group, embodiment 1 extract group, the embodiment 3 extract groups.Illustrate that Fructus Schisandrae Chinensis carpopodium (fruit stem) and leaf total lignans extract are suitable to the therapeutical effect of carbon tetrachloride hepatic injury mice with fruit of Fructus Schisandrae Chinensis total lignans extract, all the SGPT that the carbon tetrachloride hepatic injury mice is caused raises significant inhibitory effect is arranged.
Claims (10)
1. extract the new raw material of Fructus Schisandrae Chinensis total lignanoid, it is characterized in that: the extract that the sub-carpopodium of five tastes of medicinal herb and Folium Schisandrae Chinensis are obtained through PROCESS FOR TREATMENT, its total lignans weight content is 30-95%, can substitute fruit of Fructus Schisandrae Chinensis total lignans extract and be used as medicine or go into health food.
2. the new raw material of Fructus Schisandrae Chinensis total lignanoid according to claim 1, it is characterized in that: Folium Schisandrae Chinensis and its plant origin of Fructus Schisandrae Chinensis carpopodium are one or both in the following plants: the plant of magnoliaceae schisandra Schisandra chinensis Bill. and schisandra chinensis Schisandrasphenanthera Rehd.et Wils. and other Schizandras.
3. the new raw material of extraction Fructus Schisandrae Chinensis total lignanoid according to claim 1 and 2 is characterized in that: described lignanoid is one or more in the following compounds, 1: schisandrin; 2: schisantherin B; 3: deoxyschizandrin; 4: schisandrin B; 5: schisandrin C; 6: pseudo-; 7: neoschisandrin; 8: isoschizandrin; 9: SALLRSIPA SAL ADNF-9 schizronol schisanhenol; 10: schisanhenol B; 11: schisanhenol acetate; 12: schizantherin A; 13: schizantherin B; 14: schizantherin C; 15: schizantherin D; 16: schizantherin E; 17: rubschisantherin; 18: Gomisin D.; 19: Gomisin E.; 20: Gomisin F.; 21: Gomisin G.; 22: Gomisin H.; 23: gomisin K
124: gomisin K
225: gomisin K
326: gomisin L
127: gomisin L
228: gomisin M
129: gomisin M
230: Ge Mixin N; 31: Ge Mixin 0; 32: Ge Mixin R; 33: Radix Angelicae Sinensis acyl Gomisin H.; 34: Radix Angelicae Sinensis acyl Ge Mixin 0; 35: Radix Angelicae Sinensis acyl Gomisin P.; 36: Radix Angelicae Sinensis acyl Ge Mixin Q; 37: along root of Dahurian angelica acyl Gomisin H.; 38: along root of Dahurian angelica acyl Gomisin P.; 39: the benzoyl Gomisin H..
4. the preparation technology of a Fructus Schisandrae Chinensis total lignanoid extract as claimed in claim 1 is characterized in that: (1) pulverizes decocting in water with Folium Schisandrae Chinensis, carpopodium drying; With residue drying behind the water extraction, a kind of heating and refluxing extraction of the methanol with 50~95%, ethanol, isopropyl alcohol or n-butyl alcohol, the extracting solution concentrating under reduced pressure is the concentrated solution of density 0.80-1.20 or the extractum that concentrated solution obtains behind organic solvent extraction, adopt the macroporous adsorptive resins enrichment, water, 40%~75% ethanol, 95% ethanol elution, collect 95% ethanol elution, the extract that obtains after concentrating, its total lignans weight content is 30%-95%;
(2), pulverize decocting in water with Folium Schisandrae Chinensis, carpopodium (fruit stem) drying; With residue drying behind the water extraction, a kind of heating and refluxing extraction of the methanol with 70~95%, ethanol, isopropyl alcohol or n-butyl alcohol, extracting solution is evaporated to dried, organic solvent room temperature or heating and refluxing extraction, extract adopts the chromatographic column eluting, the extract that obtains behind the eluting, its total lignans weight content is 30%-95%.
5. the preparation technology of Fructus Schisandrae Chinensis total lignanoid extract according to claim 4 is characterized in that: organic solvent is ether, alcohol, ester, the ketone of polarity less than n-butyl alcohol; The solvent elution mode comprises the positive of single or mixed solvent, anti-phase or gradient elution.
6. put forward the preparation technology of thing according to the described Fructus Schisandrae Chinensis total lignanoid of claim 4, it is characterized in that: described adsorbent resin is one or more in phenylethylene, phenylpropionic acid, third rare amide-type or the nitrogen oxide type macroporous resin.
7. the preparation technology of Fructus Schisandrae Chinensis total lignanoid extract according to claim 4 is characterized in that: chromatographic column filler is one or more in silica gel, aluminium oxide, polyamide, adsorbent resin, glucose gel, ODS, the kieselguhr.
8. the new raw material of extraction Fructus Schisandrae Chinensis total lignanoid according to claim 1 is characterized in that: the extract that is obtained by this raw material can be mixed and made into acceptable drug and food dosage form clinically with pharmaceutically acceptable excipient or carrier
9. the new raw material of extraction Fructus Schisandrae Chinensis total lignanoid according to claim 8 is characterized in that: described dosage form is tablet, capsule, powder, tincture, oral liquid, drop pill and injection or beverage, bread, cookies, confection, wine, tea and cosmetics etc.
10. extract the purposes of the new raw material of Fructus Schisandrae Chinensis total lignanoid, it is characterized in that: the extract that is obtained by this raw material is used for the preparation prevention or treatment hepatitis product is used.
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