CN101337000A - Solanum nigrum extract, preparation method and use thereof - Google Patents

Solanum nigrum extract, preparation method and use thereof Download PDF

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CN101337000A
CN101337000A CNA2008100336197A CN200810033619A CN101337000A CN 101337000 A CN101337000 A CN 101337000A CN A2008100336197 A CNA2008100336197 A CN A2008100336197A CN 200810033619 A CN200810033619 A CN 200810033619A CN 101337000 A CN101337000 A CN 101337000A
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herba solani
solani nigri
ethanol
resin
mentioned steps
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CN101337000B (en
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王妍
秦继红
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Shanghai Shuofang Pharmaceutical Technology Co ltd
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HAITIAN MEDICINE SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd SHANGHAI
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Abstract

The invention relates to a solanum nigrum extractive, the preparation method and the medicament application thereof, wherein, the total content of solancarpine, solamargine and solasurine is 80wt% to 99wt%; the content of solancarpine is 30wt% to 50wt%; the content of solamargine is 10wt% to 30wt%; and the content of solasurine is 30wt% to 50wt%. The invention further relates to the preparation method of the solanum nigrum extractive and the application with the solanum nigrum extractive being the active components in the medicaments for preventing and curing diseases, such as tumor, diabetes, asthma, coronary heart disease, etc.

Description

Herba Solani Nigri extract, its preparation method and medicinal usage thereof
Technical field
The present invention relates to the plant black nightshade extract, its preparation method and as the application of the medicine of diseases such as active component preparation prevention and treatment tumor, diabetes, asthma, coronary heart disease.
Background technology
Herba Solani Nigri Solalum Nigrum L. is annual Solanum herbaceous plant, and all there is growth most of at home provinces and regions.The herb hyoscine, cold in nature, bitter in the mouth is hot little sweet, slightly poisonous, returns lung, urinary bladder channel.The energy dissipating blood stasis for subsidence of swelling, heat-clearing and toxic substances removing.Gold-coloured staphylococci, Bacillus typhi, dysentery bacterium, Bacillus proteus, escherichia coli, pseudomonas aeruginosa, hog cholera bacillus all there is stronger bacteriostasis, effects such as anticancer and urinary system infection and leucorrhea are arranged, treatment carbuncle commonly used, tumor, dysentery etc., among the people to be used for the treatment of diabetes curative effect remarkable.Herba Solani Nigri also has certain dietary function in addition, therefore has good medical value.Be rich in steroid alkaloid in the plant, ((δ-solanigrine), Herba Solani Nigri are decided alkali (solanigridine), solasurine solasurine etc. for ε-solanigrine), δ-solanine as: solasonine (solasonine), solamargine (solamargine), the bright alkali of Australian eggplant (solasodamine), ε-solanine, these steroid alkaloids all are present in Solanum nigrum stem, leaf, root, really with the form of glycosides, and aglycon is solasodine (solasodine).
Figure A20081003361900051
Solasonine solasonine solamargine solamargine
Figure A20081003361900052
The Glu glucose, Gal galactose, Rha rhamnose, Man mannose, Gui quinovose
Solasurine solasurine
Solasonine and solamargine are two main in Herba Solani Nigri alkaloid components, in in vitro tests, two chemical compounds all show the destructiveness of cell membrane fat, both show cooperative effect, the destructiveness of solamargine is stronger, and rhamnose wherein may play important function in the combining of guiding glycoalkaloid and cell; Some studies show that solamargine, thus solamargine can regulate the expression of Tumor Necrosis Factor Receptors and cause cancer cell-apoptosis, 2 rhamnose may play a decisive role in triggering apoptosis.Other glycoalkaloid also shows proximate physiologically active.Therefore, find out suitable technology, from Herba Solani Nigri, extract glucosides total alkaloids position, carry out drug efficacy study, can be used as a direction of anti-cancer agent research.To the research of prophylactic treatment diabetes, asthma and the coronary heart disease isoreactivity of Herba Solani Nigri crude extract also is external focus at present, but at present also not research show it is which chemical constituent is in action in the crude extract definitely.
Water-soluble extract, its preparation method and the pharmaceutical compositions thereof of the disclosed nightshade of Chinese patent Granted publication CN1329038C, wherein water-soluble extract is to be that solasonine and solamargine by 60%-90% constituted basically.
The Herba Solani Nigri extracting method cost that uses is higher at present, and active constituent content is lower, and impurity is more, and the pollution that produces in the preparation process is bigger.The product content of effective that obtains after extracting has limited its use in pharmaceutical compositions, still can not satisfy the needs of efficient pharmaceutical compositions.
Summary of the invention
Purpose first aspect of the present invention has provided a kind of Herba Solani Nigri extract.
Purpose second aspect of the present invention provides the preparation method of above-mentioned Herba Solani Nigri extract.
The purpose third aspect of the present invention provides the application of above-mentioned Herba Solani Nigri extract in medicine.
As the Herba Solani Nigri extract of first aspect present invention, comprise solasonine and solamargine, also comprise solasurine, wherein solasonine, solamargine and solasurine three's total content is 80wt%~99wt%.
Solasonine content is 30wt%~50wt%, and solamargine content is 10wt%~30wt%, and solasurine content is 30wt%~50wt%.
Preparation method as the Herba Solani Nigri extract of second aspect present invention may further comprise the steps:
(1) herb of Herba Solani Nigri and fruit add ethanol extraction, collect extracting solution A;
(2) ethanol in the recovery extracting solution gets concentrated solution B to there not being the alcohol flavor;
(3) concentrated solution B cationic exchange resin adsorption, water, ethanol and contain alkali ethanol and carry out eluting are successively collected and are contained alkali ethanol elution portion C;
(4) contain alkali ethanol elution portion C, reclaim ethanol and get concentrated solution D;
(5) supernatant is abandoned in concentrated solution D centrifugalize, gets precipitate E;
(6) precipitate E is washed with water to near-white and supernatant pH value less than 9, promptly gets Herba Solani Nigri extract after the precipitation drying.
In above-mentioned steps (1), at every turn make a living 2~8 times of volumes of dose of consumption of ethanol; Alcoholic acid weight percent concentration is 50%~95%.Be preferably at every turn make a living 5 times of volumes of dose of consumption of ethanol; Alcoholic acid weight percent concentration is 90%.
In above-mentioned steps (1), adopt and reflux or the ultrasonic power extraction, extraction time is 2~5 times, each 1~3 hour.Be preferably and adopt reflux type to extract, extraction time is 3 times, each 1.5 hours.
When raw medicinal herbs is a herb of Herba Solani Nigri, in above-mentioned steps (2), increase by one to the step of concentrated solution B with the petroleum ether extraction defat.Be preferably 3 defats of equal-volume petroleum ether extraction to concentrated solution B.
In above-mentioned steps (3), make a living 0.5~5 times of volume of dose of the consumption of cation exchange resin.Be preferably 1 times of volume of crude drug amount.
The functional group of described cation exchange resin is a kind of among sulfonic group, pyrovinic acid base, phosphate, carboxyl and the phenolic hydroxyl group.Be preferably sulfonic group.
In above-mentioned steps (3), preferred elution process is closely colourless to effluent for washing resin successively with water, and the weight percent concentration of 1~10 times of resin volume is 30%~90% ethanol elution, 0.5~10 times of resin volume contain the alkali ethanol elution.Preferred elution process is closely colourless to effluent for washing resin successively with water, the weight percent concentration of 1~2 times of resin volume is 30%~60% ethanol elution, the weight percent concentration of 1~5 times of resin volume is 90% ethanol elution, 1~5 times of resin volume contain the alkali ethanol elution.Most preferred type of elution is closely colourless to effluent for washing resin successively with water, the weight percent concentration of 1 times of resin volume is 40% ethanol elution, the weight percent concentration of 2 times of resin volumes is 90% ethanol elution, 3 times of resin volumes contain the alkali ethanol elution.
In above-mentioned steps (3), the described alkali ethanol that contains is that weight percent concentration is the mixed solution of 50~95% ethanol and alkali, and wherein alkali is a kind of among ammonia, sodium hydroxide, sodium carbonate, sodium bicarbonate and other commercial production alkali commonly used.Preferably containing alkali ethanol is that weight percent concentration is that 90% ethanol and weight percent concentration are 10: 1 by volume blended solution of 25% ammonia.
In above-mentioned steps (6),, increase by a usefulness washing with acetone and be precipitated to subalbous step if precipitate E color is darker.
In above-mentioned steps (3), described cation exchange resin can be regenerated, and its regenerated method is: add the heat soaking resin with 2% sodium hydrate aqueous solution; The dress post, the sodium hydrate aqueous solution 800ml eluting with 2%; Wash with water to effluent and be neutral; With 1N salt pickling resin to effluent pH value is 2; Washing resin to effluent pH value with deionized water is 6, can drop into repeated use.
Solasonine, solamargine and solasurine three's total content is 80wt%~99wt% in the Herba Solani Nigri extract that method produced according to the present invention obtains, solasonine content is 30wt%~50wt%, solamargine content is 10wt%~30wt%, and solasurine content is 30wt%~50wt%.
As the medicinal usage of the above-mentioned Herba Solani Nigri extract of third aspect present invention be with the solasonine in the described Herba Solani Nigri extract, solamargine and solasurine as active component, add acceptable accessories, the medicine of any dosage form of making.Preferred dosage form is an injection.
The application of Herba Solani Nigri extract in the medicine that is preparing diseases such as prevention and treatment tumor, diabetes, asthma, heart disease as active component as third aspect present invention.
Above-mentioned Herba Solani Nigri extract is as follows as the concrete medicinal usage of active component, but is not limited to following medicinal usage:
1, can in preparation prevention and medicine for treating tumor thing, use as active component with Herba Solani Nigri extract.
2, can in preparation prevention and treatment diabetes medicament, use as active component with Herba Solani Nigri extract.
3, can in preparation prevention and treatment asthma medicine, use as active component with Herba Solani Nigri extract.
4, can in preparation prevention and treatment medicaments for coronary disease, use as active component with Herba Solani Nigri extract.
Herba Solani Nigri extract of the present invention contains active component solasonine, solamargine and solasurine, and it has certain curative effect aspect diseases such as tumor, diabetes, asthma, coronary heart disease in prevention with treating.Preparation method of the present invention compared with prior art, this method technology advanced person produces practically greatly, cost is relatively low.Organic solvent is mainly ethanol, and the soda acid after the use is discharging after treatment all, and environmental pollution is little.Extract obtained impurity is few, the active constituent content height.
The specific embodiment
The present invention is described further below in conjunction with specific embodiment, but do not limit the present invention in any way.
Embodiment 1
The preparation of Herba Solani Nigri extract:
(1) herb of Herba Solani Nigri 400g adds 90% ethanol 2000ml, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution recovery ethanol gets the about 300ml of concentrated solution to there not being the alcohol flavor, petroleum ether extraction 3 times, and each consumption is 300ml;
(3) concentrated solution is processed into HD-8 strongly acidic cation-exchange (Shanghai Huazhen Science and Technology Co., Ltd.) the dress post absorption of H+ type with 400ml, to be eluted to effluent closely colourless for water successively, 40% ethanol 400ml eluting, 90% ethanol 800ml eluting contains ammonia ethanol (90% ethanol: 25% ammonia is 10: 1) 1200ml eluting;
(4) collection contains ammonia ethanol elution part, reclaims ethanol;
(5) concentrated solution 5000rpm is centrifugal 10 minutes, abandons supernatant;
(6) low amounts of water washing precipitation, centrifugal 10 minutes of 5000rpm so washes with water 2 times, and the reuse small amount of acetone is washed once, promptly gets Herba Solani Nigri extract 0.17g, yield 0.04% behind the precipitation drying under reduced pressure.
Wherein resin regeneration process is as follows: add the heat soaking resin with 2% sodium hydrate aqueous solution 800ml; The dress post, the sodium hydrate aqueous solution 800ml eluting with 2%; Wash with water to effluent and be neutral; With 1N salt pickling resin to effluent pH value is 2; Washing resin to effluent pH value with deionized water is 6, can drop into repeated use.
Embodiment 2
The preparation of Herba Solani Nigri extract:
(1) Solanum nigrum fruit 1000g adds 90% ethanol 5000ml, reflux, extract, 3 times, each 1.5 hours;
(2) extracting solution recovery ethanol gets the about 800ml of concentrated solution to there not being the alcohol flavor;
(3) concentrated solution is processed into HD-8 strongly acidic cation-exchange (Shanghai Huazhen Science and Technology Co., Ltd.) the dress post absorption of H+ type with 1000ml, to be eluted to effluent closely colourless for water successively, 40% ethanol 1000ml eluting, 90% ethanol 2000ml eluting contains ammonia ethanol (90% ethanol: 25% ammonia is 10:1) 3000ml eluting;
(4) collection contains ammonia ethanol elution part, reclaims ethanol;
(5) concentrated solution 5000rpm is centrifugal 10 minutes, abandons supernatant;
(6) low amounts of water washing precipitation, centrifugal 10 minutes of 5000rpm so washes with water 2 times, and the reuse small amount of acetone is washed once, promptly gets Herba Solani Nigri extract 1.5g, yield 0.15% behind the precipitation drying under reduced pressure.
Wherein resin regeneration process is as follows: add the heat soaking resin with 2% sodium hydrate aqueous solution 2000ml; The dress post, the sodium hydrate aqueous solution 2000ml eluting with 2%; Wash with water to effluent and be neutral; With 1N salt pickling resin to effluent pH value is 2; Washing resin to effluent pH value with deionized water is 6, can drop into repeated use.
Embodiment 3
The preparation of Herba Solani Nigri extract:
(1) herb of Herba Solani Nigri 400g adds 90% ethanol 2000ml, supersound extraction 3 times, each 1.5 hours;
(2) extracting solution recovery ethanol gets the about 300ml of concentrated solution to there not being the alcohol flavor, petroleum ether extraction 3 times, and each consumption is 300ml;
(3) concentrated solution is processed into HD-8 strongly acidic cation-exchange (Shanghai Huazhen Science and Technology Co., Ltd.) the dress post absorption of H+ type with 400ml, to be eluted to effluent closely colourless for water successively, 40% ethanol 400ml eluting, 90% ethanol 800ml eluting contains 80% ethanol 1200ml eluting of 0.1% sodium hydroxide;
(4) collection contains sodium hydroxide ethanol elution part, reclaims ethanol;
(5) concentrated solution 5000rpm is centrifugal 10 minutes, abandons supernatant;
(6) low amounts of water washing precipitation, centrifugal 10 minutes of 5000rpm.After so washing 4 times with water, the supernatant pH value is about 8.Promptly get Herba Solani Nigri extract 0.13g, yield 0.03% after the precipitation drying.
Wherein resin regeneration process is as follows: add the heat soaking resin with 2% sodium hydrate aqueous solution 800ml; The dress post, the sodium hydrate aqueous solution 800ml eluting with 2%; Wash with water to effluent and be neutral; With 1N salt pickling resin to effluent pH value is 2; Washing resin to effluent pH value with deionized water is 6, can drop into repeated use.
Embodiment 4
(LC-MS method) measured in alkaloidal discriminating in the Herba Solani Nigri extract
Experimental apparatus:
The LC-MS instrument, Agilent 1200LC/MSD/VL
Evaporative light scattering detector, SoftA 300A
Enlightening horse C18 jewel post, 250 * 4.6mm
The HPLC condition:
Methanol: 0.2% acetic acid, gradient 0min, 5: 95; 10min, 5: 95; 15min, 90: 10; 25min, 100: 0.Flow velocity 0.8ml/min, 35 ℃ of column temperatures.
The evaporative light scattering detector testing conditions:
DT=70℃,SC=35℃,GAS=50psi
Experimental technique and result:
Get Herba Solani Nigri extract 10mg, the accurate title, decide, put in the 25ml measuring bottle, and the small amount of methanol dissolving, methanol is diluted to scale, 0.45 μ m filtering with microporous membrane, 10 μ l sample introductions.The one group peak of retention time between 16~20 minutes is glycoalkaloid, and the peak area sum accounts for 85% of total peak area.HPLC-MS detects molecular ion peak 17.5min, 884 (solasonine, M+1); 17.8,868 (solamargine, M+1); 18.2,722 (solasurine, M+1).
Embodiment 5
The mensuration of alkaloid (thin layer chromatography scanning) in the Herba Solani Nigri extract
Experimental apparatus:
Tianjin, island CS-9310 type dual-wavelength lamellar scanning instrument
The TLC condition:
High-efficient silica gel G plate 10cm * 20cm; Developing solvent is a n-butyl alcohol: ammonia (4: 1) upper strata liquid; The bismuth potassium iodide colour developing; λ S=468nm scanning.
Experimental technique and result:
Get Herba Solani Nigri extract 10.05mg, the accurate title, decide, and puts in the 5ml measuring bottle small amount of methanol dissolving, methanol is diluted to scale, shakes up, and gets 5 μ l point samples, launches, colour developing, scanning, the area percentage of solasonine, solamargine and three points of solasurine is 40.5%, 25.4% and 34.1%.
Embodiment 6
The preparation of Herba Solani Nigri extract injection
Get Herba Solani Nigri extract 2000mg, add injection water 900ml, 1,2-propylene glycol 50ml, sodium chloride 9g with the hydrochloric acid adjust pH to 4.0 of 0.1N, adds the injection water to 1000ml, with 0.2 μ m filtering with microporous membrane, embedding, moist heat sterilization, gets the Herba Solani Nigri extract injection.
Embodiment 7
The Herba Solani Nigri extract gastric infusion is to the experimentation of rat liver cancer H22 influence
Choose the female C57BL/6 mice of 18~20g, get well-grown rat liver cancer H22 ascites, be diluted to 1~2 * 10 with normal saline 7The cell suspension of individual/ml concentration, every the right axil subcutaneous vaccination of mice 0.2ml, random packet, several 10 of every treated animal, 15 of matched groups, establish:
Blank group (coordinative solvent, 25ml/kg, ig * 7)
Cyclophosphamide for injection (30mg/kg, ip * 7)
Herba Solani Nigri extract (50mg/kg, ig * 7)
Herba Solani Nigri extract (100mg/kg, ig * 7)
Herba Solani Nigri extract (200mg/kg, ig * 7)
Herba Solani Nigri extract is made into suspension with 0.5%CMC after with several tween 80 hydrotropies, and Cyclophosphamide for injection is mixed with desired concn with normal saline.
Administration is played next day in the inoculation back, and the administration volume is the 0.5ml/20g body weight, and per os was irritated stomach 7 days continuously.Inoculate back 10 days and take off neck execution animal, dissect and get the tumor piece, claim tumor heavy, calculate tumour inhibiting rate.
Result of the test sees Table 1, and Herba Solani Nigri extract can obviously reduce rat liver cancer H22 50,100, on the level of 200mg/kg during the per os gastric infusion and organize level.After the administration 7 days, each administration group is compared with matched group, and tumor is heavy, and there were significant differences (P<0.01).
Table 1. Herba Solani Nigri extract gastric infusion is to the tumor-inhibiting action of rat liver cancer H22
Figure A20081003361900111
Compare with matched group: *P<0.05, *P<0.01.
Embodiment 8
The Herba Solani Nigri extract gastric infusion is to the experimentation of Mice Bearing Lewis Lung Cancer influence
Choose the female C57BL/6 mice of 18~20g, get well-grown Mice Bearing Lewis Lung Cancer tumor piece, be prepared into 1~2 * 10 with normal saline homogenate method 7The cell suspension of individual/ml concentration, every the right axil subcutaneous vaccination of mice 0.2ml, random packet, several 6 of each treated animal, 12 of matched groups, establish:
The blank group (coordinative solvent, 25ml/kg)
Cyclophosphamide for injection (30mg/kg, ip * 7)
Herba Solani Nigri extract (50mg/kg, ig * 10)
Herba Solani Nigri extract (100mg/kg, ig * 10)
Herba Solani Nigri extract (200mg/kg, ig * 10)
Herba Solani Nigri extract is made into suspension with 0.5%CMC after with several tween 80 hydrotropies, and Cyclophosphamide for injection is mixed with desired concn with normal saline.
Inoculation plays administration next day, and the administration volume is the 0.5ml/20g body weight, and per os was irritated stomach 10 days continuously.Inoculate back 14 days and take off neck execution animal, dissect and get the tumor piece, claim tumor heavy, calculate tumour inhibiting rate.
Result of the test sees Table 2, and Herba Solani Nigri extract can obviously reduce Mice Bearing Lewis Lung Cancer 50,100, on the level of 200mg/kg during the per os gastric infusion and organize level.After the administration 10 days, each administration group is compared with matched group, and tumor is heavy, and there were significant differences (P<0.01).
Table 2. Herba Solani Nigri extract gastric infusion is to the tumor-inhibiting action of Mice Bearing Lewis Lung Cancer
Figure A20081003361900121
Compare with matched group: *P<0.05, *P<0.01.
Embodiment 9
The experimentation that Herba Solani Nigri extract is subcutaneous, intraperitoneal administration influences rat liver cancer H22
Choose the female C57BL/6 mice of 18~20g, get well-grown rat liver cancer H22 ascites, be prepared into 1~2 * 10 with normal saline homogenate method 7The cell suspension of individual/ml concentration, every the right axil subcutaneous vaccination of mice 0.2ml, random packet, several 10 of each treated animal, 15 of matched groups, establish:
The blank group (coordinative solvent, 25ml/kg)
Cyclophosphamide for injection (30mg/kg, ip * 7)
Herba Solani Nigri extract (40mg/kg, sc * 10)
Herba Solani Nigri extract (40mg/kg, ip * 10)
Herba Solani Nigri extract is made into suspension with 0.5%CMC after with several tween 80 hydrotropies, and Cyclophosphamide for injection is mixed with desired concn with normal saline.
Inoculation plays administration next day, and the administration volume is the 0.5ml/20g body weight, subcutaneous continuously, intraperitoneal administration 7 days.Inoculate back 10 days and take off neck execution animal, dissect and get the tumor piece, claim tumor heavy, calculate tumour inhibiting rate.
Result of the test sees Table 3, and Herba Solani Nigri extract can obviously reduce rat liver cancer H22 during subcutaneous and intraperitoneal administration and organize level on the level of 40mg/kg.After the administration 7 days, Herba Solani Nigri extract 40mg/kg subcutaneous administration group, intraperitoneal injection group are compared with matched group, and tumor is heavy, and there were significant differences (P<0.01).
Table 3. Herba Solani Nigri extract is subcutaneous, intraperitoneal administration is to the tumor-inhibiting action of rat liver cancer H22
Figure A20081003361900131
Compare with matched group: *P<0.05, *P<0.01.
Embodiment 10
The experimentation that Herba Solani Nigri extract is subcutaneous, intraperitoneal administration influences Mice Bearing Lewis Lung Cancer
Choose the male C57BL/6 mice of 18~20g, get well-grown mouse lung carcinoma piece, be prepared into 1~2 * 10 with normal saline homogenate method 7The cell suspension of individual/ml concentration, every the right axil subcutaneous vaccination of mice 0.2ml, random packet, several 10 of each treated animal, 15 of matched groups, establish:
The blank group (coordinative solvent, 25ml/kg)
Cyclophosphamide for injection (30mg/kg, ip * 7)
Herba Solani Nigri extract (40mg/kg, sc * 10)
Herba Solani Nigri extract (40mg/kg, ip * 10)
Herba Solani Nigri extract is made into suspension with 0.5%CMC after with several tween 80 hydrotropies, and Cyclophosphamide for injection is mixed with desired concn with normal saline.
Inoculation plays administration next day, and the administration volume is the 0.5ml/20g body weight, subcutaneous continuously, intraperitoneal administration 10 days.Inoculate back 14 days and take off neck execution animal, dissect and get the tumor piece, claim tumor heavy, calculate tumour inhibiting rate.
Result of the test sees Table 4, and Herba Solani Nigri extract can obviously reduce Mice Bearing Lewis Lung Cancer during subcutaneous and intraperitoneal administration and organize level on the level of 40mg/kg.After the administration 10 days, Herba Solani Nigri extract 40mg/kg intraperitoneal injection group is compared with matched group, and tumor is heavy, and there were significant differences (P<0.01).
Table 4. Herba Solani Nigri extract is subcutaneous, intraperitoneal administration is to the tumor-inhibiting action of Mice Bearing Lewis Lung Cancer
Figure A20081003361900141
Compare with matched group: *P<0.05, *P<0.01.
Embodiment 11
Herba Solani Nigri extract is to the influence of normal mouse post-prandial glycemia
Choose 18~20g male mice in kunming, be divided into blank group (normal saline), positive matched group (glibenclamide 2.5mg/kg), administration group I (Herba Solani Nigri extract 10mg/kg) and administration group II (Herba Solani Nigri extract 20mg/kg) at random by body weight, every group each 6, water is can't help in the 18h fasting before the test, behind the gastric infusion 1,2,4,8, the 10h tail vein blood, behind the centrifugal separation plasma, measure glucose level with glucose oxidase-peroxidase (GOD-POD) method.
Result of the test sees Table 5, and Herba Solani Nigri extract can obviously reduce the normal mouse level of postprandial blood sugar 10, on the level of 20mg/kg.Behind administration 8h, the 10h, 20mg/kg dosage group is compared with matched group, and there were significant differences for blood glucose value (P<0.01).
Table 5. Herba Solani Nigri extract is to the influence of normal mouse post-prandial glycemia
Figure A20081003361900151
Compare with matched group: *P<0.05, *P<0.01 (n=6).
Embodiment 12
Herba Solani Nigri extract is to the influence of tissue of experimental diabetic mice post-prandial glycemia
Choose 18~20g male mice in kunming, water is can't help in the 24h fasting, presses 120mg/kg lumbar injection alloxan physiological salt liquid, feeding behind the 1h, tail vein blood is measured blood sugar level behind the 48h, and the mice that reaches more than the 200mg/100ml when blood glucose value is decided to be the diabetes model Mus.It is divided into blank group (normal saline), positive matched group (glibenclamide 2.5mg/kg), administration group I (Herba Solani Nigri extract 10mg/kg) and administration group II (Herba Solani Nigri extract 20mg/kg) at random by body weight, every group each 6, behind the gastric infusion 1,2,4,8, the 10h tail vein blood, behind the centrifugal separation plasma, measure glucose level with glucose oxidase-peroxidase (GOD-POD) method.
Result of the test sees Table 6, and Herba Solani Nigri extract can obviously reduce the tissue of experimental diabetic mice level of postprandial blood sugar 10, on the level of 20mg/kg.Behind administration 4h, 8h and the 10h, each dosage group is compared with matched group, and there were significant differences for blood glucose value (P<0.01).
Table 6. Herba Solani Nigri extract is to the influence of tissue of experimental diabetic mice post-prandial glycemia
Figure A20081003361900152
Compare with matched group: *P<0.05, *P<0.01 (n=6).
Embodiment 13
Herba Solani Nigri extract is to the influence of Cavia porcellus experimental asthma
Choose 200~250g healthy guinea pig and be divided into normal control group, asthmatic model group, administration group I (Herba Solani Nigri extract 10mg/kg) and administration group II (Herba Solani Nigri extract 20mg/kg) at random, every group each 6.Set up the asthmatic guinea pigs model with ovalbumin (OVA) lumbar injection sensitization with atomizing to suck to excite.Detect serum NO level, T-NOS, iNOS level.
Result of the test sees Table 7, and Herba Solani Nigri extract can obviously reduce serum NO level, T-NOS and iNOS level 10, on the level of 20mg/kg, and relatively there were significant differences (P<0.05) with model group.
Table 7. Herba Solani Nigri extract is to the influence of Cavia porcellus experimental asthma
Figure A20081003361900161
Compare with model group: *P<0.05 (n=6).
Embodiment 14
Herba Solani Nigri extract is to the protective effect of myocardial ischemia reperfusion injury
Adopt isolated rat perfusion heart (Langendorff heart) ischemia-reperfusion injury model, with the K-HShi buffer perfused hearts that contains Herba Solani Nigri extract, detect in the cardiac muscular tissue MDA content and irritate LDH activity in the 15min perfusate again, this two indexes can reflect and the closely-related oxygen-derived free radicals level variation of myocardial damage indirectly.Chamber incidence rate of quivering of each group of record.The result that causes of perfusion is shown in table 8,9,10 again.
Table 8. Herba Solani Nigri extract is to the quiver influence of incidence rate of isolated rat perfusion heart chamber
Figure A20081003361900162
Annotate: compare with negative control group, *P<0.05, *P<0.01 (n=12).
Table 9. Herba Solani Nigri extract is organized the influence of MDA content to isolated myocardium
Figure A20081003361900171
Annotate: compare with negative control group, *P<0.05, *P<0.01 (n=12).
Table 10. Herba Solani Nigri extract extract is to irritating the active influence of LDH in the perfusate again
Figure A20081003361900172
Annotate: compare with negative control group, *P<0.05, *P<0.01 (n=12).
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in the foregoing description and the description just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (27)

1, Herba Solani Nigri extract comprises solasonine and solamargine, also comprises solasurine, and wherein solasonine, solamargine and solasurine three's total content is 80wt%~99wt%.
2, Herba Solani Nigri extract as claimed in claim 1 is characterized in that, solasonine content is 30wt%~50wt%, and solamargine content is 10wt%~30wt%, and solasurine content is 30wt%~50wt%.
3, a kind of method for preparing the described Herba Solani Nigri extract of claim 1 is characterized in that, may further comprise the steps:
(1) herb of Herba Solani Nigri and fruit add ethanol extraction, collect extracting solution A;
(2) ethanol in the recovery extracting solution gets concentrated solution B to there not being the alcohol flavor;
(3) concentrated solution B cationic exchange resin adsorption, water, ethanol and contain alkali ethanol and carry out eluting are successively collected and are contained alkali ethanol elution portion C;
(4) contain alkali ethanol elution portion C, reclaim ethanol and get concentrated solution D;
(5) supernatant is abandoned in concentrated solution D centrifugalize, gets precipitate E;
(6) precipitate E is washed with water to near-white and supernatant pH value less than 9, promptly gets Herba Solani Nigri extract after the precipitation drying.
4, method as claimed in claim 3 is characterized in that, in above-mentioned steps (1), and at every turn make a living 2~8 times of volumes of dose of consumption of ethanol; Alcoholic acid weight percent concentration is 50%~95%.
5, method as claimed in claim 3 is characterized in that, in above-mentioned steps (1), and at every turn make a living 5 times of volumes of dose of consumption of ethanol; Alcoholic acid weight percent concentration is 90%.
6, method as claimed in claim 3 is characterized in that, in above-mentioned steps (1), adopts and refluxes or the ultrasonic power extraction, and extraction time is 2~5 times, each 1~3 hour.
7, method as claimed in claim 3 is characterized in that, in above-mentioned steps (1), adopts reflux type to extract, and extraction time is 3 times, each 1.5 hours.
8, method as claimed in claim 3 is characterized in that, when raw medicinal herbs is a herb of Herba Solani Nigri, in above-mentioned steps (2), increases by one to the step of concentrated solution B with the petroleum ether extraction defat.
9, method as claimed in claim 3 is characterized in that, when raw medicinal herbs is a herb of Herba Solani Nigri, in above-mentioned steps (2), increases by one to the step of concentrated solution B with 3 defats of equal-volume petroleum ether extraction.
10, method as claimed in claim 3 is characterized in that, in above-mentioned steps (3), and make a living 0.5~5 times of volume of dose of the consumption of described cation exchange resin.
11, method as claimed in claim 3 is characterized in that, in above-mentioned steps (3), and make a living 1 times of volume of dose of the consumption of described cation exchange resin.
12, method as claimed in claim 3 is characterized in that, in above-mentioned steps (3), the functional group of described cation exchange resin is a kind of among sulfonic group, pyrovinic acid base, phosphate, carboxyl and the phenolic hydroxyl group.
13, method as claimed in claim 3 is characterized in that, in above-mentioned steps (3), the functional group of described cation exchange resin is a sulfonic group.
14, method as claimed in claim 3, it is characterized in that, in above-mentioned steps (3), the elution process that adopts is closely colourless to effluent for washing resin successively with water, the weight percent concentration of 1~10 times of resin volume is 30%~90% ethanol elution, 0.5~10 times of resin volume contain the alkali ethanol elution.
15, method as claimed in claim 3, it is characterized in that, in above-mentioned steps (3), the elution process that adopts is closely colourless to effluent for washing resin successively with water, the weight percent concentration of 1~2 times of resin volume is 30%~60% ethanol elution, 90% ethanol elution of 1~5 times of resin volume, 1~5 times of resin volume contain the alkali ethanol elution.
16, method as claimed in claim 3, it is characterized in that, in above-mentioned steps (3), the type of elution that adopts is closely colourless to effluent for washing resin successively with water, the weight percent concentration of 1 times of resin volume is 40% ethanol elution, 90% ethanol elution of 2 times of resin volumes, 3 times of resin volumes contain the alkali ethanol elution.
17, as claim 3 or 12 or 13 or 14 described methods, it is characterized in that, the described alkali ethanol that contains is that weight percent concentration is the mixed solution of 50~95% ethanol and alkali, and wherein alkali is a kind of among ammonia, sodium hydroxide, sodium carbonate, sodium bicarbonate and other commercial production alkali commonly used.
As claim 3 or 12 or 13 or 14 described methods, it is characterized in that 18, the described alkali ethanol that contains is that weight percent concentration is that 90% ethanol and weight percent concentration are 10: 1 by volume blended solution of 25% ammonia.
19, method as claimed in claim 3 is characterized in that, in above-mentioned steps (6), if precipitate E color is darker, increases by a usefulness washing with acetone and is precipitated to subalbous step.
20, method as claimed in claim 3 is characterized in that, described cation exchange resin can be regenerated, and its regenerated method is: add the heat soaking resin with 2% sodium hydrate aqueous solution; The dress post, the sodium hydrate aqueous solution 800ml eluting with 2%; Wash with water to effluent and be neutral; With 1N salt pickling resin to effluent pH value is 2; Washing resin to effluent pH value with deionized water is 6, can drop into repeated use.
21, method as claimed in claim 3, it is characterized in that, solasonine content is 30wt%~50wt% in the Herba Solani Nigri extract that described step (6) obtains, solamargine content is 10wt%~30wt%, solasurine content is 30wt%~50wt%, and solasonine, solamargine and solasurine three's total content is 80wt%~99wt%.
22, the medicinal usage of the described Herba Solani Nigri extract of a kind of claim 1~2 be with the solasonine in the described Herba Solani Nigri extract, solamargine and solasurine as active component, add acceptable accessories, the medicine of any dosage form of making.
23, purposes as claimed in claim 22 is characterized in that, described dosage form is an injection.
24, the described Herba Solani Nigri extract of a kind of claim 1~2 is used in preparation prevention and medicine for treating tumor thing as active component.
25, the described Herba Solani Nigri extract of a kind of claim 1~2 is used in preparation prevention and treatment diabetes medicament as active component.
26, the described Herba Solani Nigri extract of a kind of claim 1~2 is used in preparation prevention and treatment asthma medicine as active component.
27, the described Herba Solani Nigri extract of a kind of claim 1~2 is used in preparation prevention and treatment medicaments for coronary disease as active component.
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CN102872260A (en) * 2011-06-10 2013-01-16 德英生物科技股份有限公司 Method for treating and/or preventing inflammation and cutaneous photodamage by using water soluble extract from plant of Solanum genus and having photoprotective effect
AU2012200389B2 (en) * 2011-05-04 2013-10-31 G & E Herbal Biotechnology Co., Ltd. Anti-wart pharmaceutical composition and method for treating wart
US8614196B2 (en) 2011-05-12 2013-12-24 G & E Herbal Biotechnology Co., Ltd. Treatment and/or prevention of inflammation and cutaneous photodamage and photoprotection of the skin with a water-soluble extract from plant of Solanum genus
CN106509579A (en) * 2016-11-24 2017-03-22 张锦超 Preparation method for nigrum fruit products
CN106577844A (en) * 2016-11-15 2017-04-26 中国农业科学院麻类研究所 Preparation for prevention and cure of pepper phytophthora blight, and production and application thereof
CN107260685A (en) * 2017-06-02 2017-10-20 神威药业集团有限公司 A kind of preparation method of Solanum nigrum granule
CN108324798A (en) * 2018-05-10 2018-07-27 李明慧 A kind of converted products and purposes of S. photeinocarpum
CN109620885A (en) * 2019-02-02 2019-04-16 李明慧 A kind of black nightshade converted products and application thereof
CN109674884A (en) * 2019-02-01 2019-04-26 李明慧 Black nightshade product and processing method and purposes
CN110501200A (en) * 2019-09-23 2019-11-26 吉林师范大学 A kind of black nightshade effective ingredient that can be recycled is extracted and separation method
CN111214581A (en) * 2018-11-26 2020-06-02 天津中新药业集团股份有限公司研究院分公司 Preparation method and application of solanum nigrum fruit total alkaloids
CN111493255A (en) * 2020-04-15 2020-08-07 吉林创岐生态农业技术开发有限公司 Solanum torvum solid beverage and application thereof
CN114767766A (en) * 2022-04-13 2022-07-22 陕西海斯夫生物工程有限公司 Extraction method of black nightshade fruit extract

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* Cited by examiner, † Cited by third party
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AU2012200389B2 (en) * 2011-05-04 2013-10-31 G & E Herbal Biotechnology Co., Ltd. Anti-wart pharmaceutical composition and method for treating wart
US8614196B2 (en) 2011-05-12 2013-12-24 G & E Herbal Biotechnology Co., Ltd. Treatment and/or prevention of inflammation and cutaneous photodamage and photoprotection of the skin with a water-soluble extract from plant of Solanum genus
CN102872260A (en) * 2011-06-10 2013-01-16 德英生物科技股份有限公司 Method for treating and/or preventing inflammation and cutaneous photodamage by using water soluble extract from plant of Solanum genus and having photoprotective effect
CN106577844B (en) * 2016-11-15 2019-08-30 中国农业科学院麻类研究所 Prevent and treat capsicum epidemic disease preparation, its preparation and application
CN106577844A (en) * 2016-11-15 2017-04-26 中国农业科学院麻类研究所 Preparation for prevention and cure of pepper phytophthora blight, and production and application thereof
CN106509579A (en) * 2016-11-24 2017-03-22 张锦超 Preparation method for nigrum fruit products
CN106509579B (en) * 2016-11-24 2017-06-30 张锦超 A kind of preparation method of black nightshade fruit product
CN107260685A (en) * 2017-06-02 2017-10-20 神威药业集团有限公司 A kind of preparation method of Solanum nigrum granule
CN107260685B (en) * 2017-06-02 2020-11-24 神威药业集团有限公司 Preparation method of solanum nigrum fruit formula granules
CN108324798A (en) * 2018-05-10 2018-07-27 李明慧 A kind of converted products and purposes of S. photeinocarpum
CN111214581A (en) * 2018-11-26 2020-06-02 天津中新药业集团股份有限公司研究院分公司 Preparation method and application of solanum nigrum fruit total alkaloids
CN109674884A (en) * 2019-02-01 2019-04-26 李明慧 Black nightshade product and processing method and purposes
CN109620885A (en) * 2019-02-02 2019-04-16 李明慧 A kind of black nightshade converted products and application thereof
CN110501200A (en) * 2019-09-23 2019-11-26 吉林师范大学 A kind of black nightshade effective ingredient that can be recycled is extracted and separation method
CN110501200B (en) * 2019-09-23 2022-05-03 吉林师范大学 Method for extracting and separating effective components of recyclable black nightshade
CN111493255A (en) * 2020-04-15 2020-08-07 吉林创岐生态农业技术开发有限公司 Solanum torvum solid beverage and application thereof
CN114767766A (en) * 2022-04-13 2022-07-22 陕西海斯夫生物工程有限公司 Extraction method of black nightshade fruit extract

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