CN1709416A - Sambucus Chinensis extract and its preparing method - Google Patents
Sambucus Chinensis extract and its preparing method Download PDFInfo
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- CN1709416A CN1709416A CN 200510075383 CN200510075383A CN1709416A CN 1709416 A CN1709416 A CN 1709416A CN 200510075383 CN200510075383 CN 200510075383 CN 200510075383 A CN200510075383 A CN 200510075383A CN 1709416 A CN1709416 A CN 1709416A
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Abstract
The present invention relates to a Java elder fruit extract and its preparation method. Said preparation method includes the following steps: 1. utilizing solvent to extract Chinese medicinal material Java elder fruit, concentrating to obtain extractum; and 2. making the extractum obtained by step 1 undergo the processes of adsorption and elution so as to obtain the invented extract.
Description
Technical field
The present invention relates to a kind of natural plant extracts and preparation method thereof, particularly Sambucus Chinensis extract and preparation method thereof and the application in the hepatitis disease treatment.
Background technology
Viral hepatitis is a kind of pernicious infectious disease of high incidence, and wherein the highest and all over the world with the hepatitis B sickness rate especially, China is the district occurred frequently of hepatitis B virus, and 1.2 hundred million hepatitis B virus carrierss are now arranged approximately.Hepatitis B can cause various types of hepatopathys such as chronic hepatitis, liver cirrhosis and primary hepatic carcinoma, seriously jeopardizes human health.The treatment hepatitis B medicine mainly comprises medicine alpha-interferon and the lamivudine at virus replication at present, and the immunomodulator of auxiliary treatment, symptomatic treatment and hepatic etc.Alpha-interferon is the comparatively sure anti-hepatic-B virus medicine of present curative effect, but only effective to 20%～30% case.Nucleoside analogues medicine lamivudine can suppress hepatitis B virus DNA polymerase activity, and the hepatitis B virus DNA titre obviously descends in the patient's serum of treatment back, but is prone to the strain of drug resistance variant viral.The treatment to the compound hepatitis of chronic hepatitis B and multiple cross infection at present still lacks specific medicament.From traditional Chinese medicine therapy, seek active drug, become the focus that people pay close attention to treatment hepatitis and other hepatopathy.
Herba Sambuci Chiensis is the herb of Caprifoliaceae Sambucus plant Herba Sambuci Chiensis (Sambucus Chinensis Lindl.), have another name called Herba sambuci chinensis, Sambucus chinensis, Rhizoma seu Herba Elatostematis stewardii etc., it is China's medical herbs commonly used among the people, effects such as promoting blood circulation to remove blood stasis, anti-inflammatory analgetic, diuresis, spasmolytic detumescence, dispelling, collateral-activating are arranged, be mainly used in diseases such as traumatic injury, rheumatism, beriberi swelling, oedema due to nephritis, icterohepatitis, acute bacillary dysentery, pneumonia.The end of the seventies, promptly create with Herba Sambuci Chiensis decoct, syrup, electuary treatment acute viral hepatitis 1115 examples in the area, Yichuan, cure rate 83.95%, effective percentage 98.2%, effect [Yichun Medical Inst., Jiangxi's volume that obviously is better than the Chinese medicine and western medicine Comprehensive Treatment matched group same period, the medical scientific research data, 1978,13-14].Mainly contain α-and triterpene and sterols chemical constituent such as β-Amyrin, maloic acid, oleanolic acid, cupreol in the Herba Sambuci Chiensis, wherein with the content of maloic acid higher (0.4%～0.8%).Maloic acid and oleanolic acid all have tangible antihepatitic activity, clinical practice maloic acid treatment viral hepatitis is evident in efficacy, definite, be the main active [Chen Wu etc. of anti-hepatitis in the Herba Sambuci Chiensis, the research of Herba Sambuci Chiensis antihepatitic activity composition, University Of Nanchang's journal (natural sciences version), the 25th the 2nd phase of volume of calendar year 2001].
More than existing achievement in research shows that Herba Sambuci Chiensis has acute viral hepatitis effect preferably.At present existing Herba Sambuci Chiensis sheet (Ministry of Public Health ministry standard WS
3-B-0294-90), Herba Sambuci Chiensis electuary (Ministry of Public Health ministry standard WS
3-B-0295-90) and Herba Sambuci Chiensis syrup (Ministry of Public Health ministry standard WS
3-B-0296-90) wait preparation as the drug use for the treatment of acute viral hepatitis.But such medicine is water and obtains through refining fully, and technology is comparatively coarse, has shortcomings such as taking dose is big, effective ingredient is unclear, dosage form is simple.To the pharmacodynamic study of Herba Sambuci Chiensis seldom, only be confined to carbon tetrachloride (CCl simultaneously
4) the acute liver damage Study of model.Pharmacodynamic feature and preparation technology to Herba Sambuci Chiensis still await further further investigation.
The present invention be directed to the treatment of existing viral hepatitis and other liver disease drug as be easy to generate limitation such as drug resistance, relapse rate height, side effect are big; and above existing Herba Sambuci Chiensis medicine is simple as technology; taking dose is big; effective ingredient is unclear; quality is not easy control; shortcomings such as pharmacological action is unclear have clear and definite antiviral, protection hepatocyte for society provides a kind of, improve the natural drug Sambucus Chinensis extract of effects such as immunity.
Summary of the invention
The purpose of this invention is to provide a kind of Sambucus Chinensis extract for the treatment of hepatitis and preparation method thereof.
Another object of the present invention provides the application of this extract in liver disease.
Sambucus Chinensis extract of the present invention is characterized in that, in order to the preparation of below method, described preparation method may further comprise the steps:
(1) with solvent extraction Herba Sambuci Chiensis medical material, gets extractum after concentrating;
(2) extractum of step (1) is through absorption, and elution process gets extract.
Herba Sambuci Chiensis medical material described in the step (1) is that process is chosen the Herba Sambuci Chiensis medical material, cutting, and natural drying obtains.
Solvent is selected from water, alcohol, ether, ketone, ester or their mixture described in the step (1).
Extract described in the step (1) and be selected from: immersion, decoction, percolation, extraction, backflow, described concentrating is selected from: natural drying, heat drying, concentrating under reduced pressure, spray drying or lyophilization.
Absorption described in the step (2) is through with step (1) gained Herba Sambuci Chiensis extractum, dissolves, and filters; Filtrate is through adsorbing with resin, kieselguhr, silica gel, aluminium oxide or the polyamide chromatography method as adsorbent.
Eluting described in the step (2) is with alcohol, water or pure water mixed solvent eluting.
Extract of the present invention is collected eluent after also comprising eluting in its preparation process, and drying eliminates solvent, the process of Sambucus Chinensis extract.
Extract of the present invention preferably prepares through following steps:
(1) chooses Herba Sambuci Chiensis medical material, cutting, natural drying;
(2) adopt water, alcohol (less than five carbon) or pure water mixed solvent, percolation or heating and refluxing extraction by (1) gained Herba Sambuci Chiensis medical material; Add 5-10 and doubly measure solvent, heating and refluxing extraction 1-4 time, each 0.5-3 hour, extract obtained corresponding Herba Sambuci Chiensis fluid extract through concentrating under reduced pressure or lyophilization;
(3) restrain crude drug in whole/milliliter with 40-80 degree hot water dissolving to being equivalent to 0.5 approximately by (2) gained Herba Sambuci Chiensis fluid extract, filter; Filtrate is through resin, kieselguhr, silica gel, aluminium oxide or polyamide adsorbents adsorb, alcohol (less than five carbon) or pure water mixed solvent eluting; Collect eluent, natural evaporation, concentrating under reduced pressure, vacuum drying, spray drying or lyophilization eliminate solvent, promptly get Sambucus Chinensis extract.
Wherein select 40-90% alcohol-water mixed solvent heating and refluxing extraction in the step (2) for use, measure solvents with 8 times in the step (2), heating and refluxing extraction 3 times, each 1 hour, extract obtained corresponding Herba Sambuci Chiensis fluid extract through concentrating under reduced pressure, and step is selected macroporous resin for use in (3), select 60-95% alcohol-water mixed solvent eluting in the step (3) for use, preferred 75% ethanol mixed solvent heating and refluxing extraction contains maloic acid and oleanolic acid in extract obtained, and wherein maloic acid is not less than 1% of extract weight.
The present invention also comprises any pharmaceutical preparation of making as active constituents of medicine with extract of the present invention.
Sambucus Chinensis extract of the present invention, technology is made any pharmaceutical dosage forms that meets the preparation requirement routinely, as tablet, granule, capsule, oral liquid and injection etc.
The present invention also comprises, with the application of Sambucus Chinensis extract of the present invention in liver disease, comprises especially hepatitis B of various viral hepatitis, and has following a kind of or several effects: (1) is to the protective effect of carbon tetrachloride induced mice acute liver damage; (2) to the protective effect of mice D galactosamine hydrochlorate acute liver damage model; (3) to the protective effect of rat carbon tetrachloride chronic hepatic injury model; (4) to the inhibitory action of external 2215 hepatitis B viruss; (5) to the mice spleen lymphocytes proliferation effect; (6) strengthen the macrophage phagocytosis of mice effect; (7) to the choleretic effect of normal rat.
The invention has the advantages that this extract is extracted, concentrates, makes with extra care and form through modern scientific method; no reagent contamination simple for process, safe, non-environmental-pollution; the active constituent content (about 10 times) and the yield of crude drug have been improved; reduced taking dose (about 10 times); adopt conventional method to be processed into various modern preparations easily, for society provides a kind of anti-hepatitis natural drug that has clear and definite antiviral, protection hepatocyte, improves effects such as immunity, function of gallbladder promoting.
Content of the present invention is to finish on the research work bases in a large number in pharmacological screening and component separating, Study on Preparation and optimization, the pharmacological action etc. of Herba Sambuci Chiensis effective site.
1, the Study on Preparation of Sambucus Chinensis extract
Follow the tracks of through the pharmacologically active screening, we adopt alcohol extraction, macroporous resin purification techniques, have obtained Herba Sambuci Chiensis effective site.Identify through plant separation and structure, from Herba Sambuci Chiensis effective site, separate obtaining maloic acid, oleanolic acid, cupreol isoreactivity composition, wherein higher with the yield of maloic acid.We are leading indicator with antihepatitic activity composition maloic acid, and the preparation technology of Sambucus Chinensis extract has been carried out optimizing research.
(1) selection of extraction solvent
Respectively get Herba Sambuci Chiensis 40g, adopt 10 times of water gagings, methanol, 35% ethanol, 55% ethanol, 75% ethanol, 95% ethanol respectively, heating and refluxing extraction 2 times, each 1 hour.Filter, merge extractive liquid, is evaporated to the thick paste shape, and vacuum drying is weighed to doing, and calculating is respectively organized extract and must be measured and yield, sees Table 1.
The different extraction solvent result of the tests of table 1 Herba Sambuci Chiensis
| Solvent | Medical material amount (g) | Extract weight (g) | Extraction ratio (%) | Maloic acid content (%) | Maloic acid yield (%) |
| Water | ????40.2 | ????16.0 | ????39.9 | ????0.117 | ????4.7 |
| Water extract-alcohol precipitation 35% ethanol 55% ethanol 75% alcohol 95 % ethanol methanol | ????40.1 ????39.8 ????40.1 ????39.9 ????40.1 ????40.0 | ????3.8 ????11.9 ????12.5 ????13.3 ????11.2 ????15.3 | ????10.5 ????29.8 ????31.2 ????33.4 ????28.0 ????38.3 | ????0.372 ????0.148 ????0.179 ????0.413 ????0.439 ????0.367 | ????3.9 ????4.4 ????5.6 ????13.8 ????12.3 ????14.0 |
Result of the test shows that each solvent group extraction ratio and maloic acid content and yield difference are bigger, and be the highest with 75% ethanol and methanol, and maloic acid content and yield are less in traditional water extraction process.Each organizes ethanol and water extraction extractum shows through the pharmacological screening result, and 75% ethanol extraction effect is best.Consider that from drug effect, safety and practicality aspect our preferred 75% ethanol is extraction solvent.
We are extraction solvent with 75% ethanol, and to the ethanol consumption (A) in the extraction process, extraction time (C), extraction time (B), concentration of alcohol factors such as (D), it is preferred to be with extraction ratio and maloic acid content that index is carried out extraction conditions.Result of the test shows that C is the principal element (P＜0.01) that influences extraction ratio, and the influence of A, B is very little.Consider that from producing practical situation optimum extraction process is A
2B
1C
2, promptly each 8 times of 75% alcohol heating reflux to the medical material amount extract 3 times, and each 1 hour, extraction ratio was about 36%, maloic acid content 0.47%.
(2) macroporous resin process for refining examination result
We have carried out big quantity research to the macroporous resin process for refining, content comprises blade diameter length ratio, resin regeneration and the service life of the kind of macroporous resin and model, resin applied sample amount, resin absorption performance, resin, and the last sample concentration of medicinal liquid, resin washing water consumption, the yield of variable concentrations eluting solvent, the flow velocity of eluting solvent etc.Final process optimization result, to adopt polystyrene macroporous resin, 30-95 (80) % alcohol-water mixed solvent eluting is best.Last sample medicinal liquid is for being equivalent to crude drug in whole 0.5g/ml concentration, and the eluting water consumption is 5 times of resin column volumes, and eluting is 3 times of amount column volumes with 30-95 (80) % amount of alcohol.The preferred concentrating under reduced pressure of eluent, 65 ℃ of vacuum dryings.Under this optimal condition, the Sambucus Chinensis extract total yield is the highest, is about 9.7%.Maloic acid content wherein is about 1.7%.
The different eluting group of table 2 macroporous resin yield result of the test
| Medical material amount (g) | Eluting solvent | Extract weight (g) | Extraction ratio (%) |
| ????30 ????30 | Water 30% ethanol 60% alcohol 95 % ethanol 80% ethanol | ????2 ????1.5 ????1 ????0.5 ????2.9 | ????6.7 ????5.0 ????3.3 ????1.7 ????9.7 |
2, pharmacological research work summary
Pharmacological experiments shows that Sambucus Chinensis extract has following several respects pharmacological action: (1) is to the protective effect of carbon tetrachloride induced mice acute liver damage; (2) to the protective effect of mice D galactosamine hydrochlorate acute liver damage model; (3) to the protective effect of rat carbon tetrachloride chronic hepatic injury model; (4) to the inhibitory action of DHB; (5) to the mice spleen lymphocytes proliferation effect; (6) strengthen the macrophage phagocytosis of mice effect; (7) to the choleretic effect of normal rat.Above pharmacological research proves that Sambucus Chinensis extract has effects such as significant antiviral, protection hepatocyte, raising immunity, can be used for the hepatitis disease treatment, comprises especially hepatitis B of various viral hepatitis.
Outstanding feature of the present invention is that extract of the present invention is extracted, concentrates through modern scientific method, refining forming, improved active constituent content, improve curative effect, reduced taking dose and side effect, and simple for process, the no reagent contamination of safety.
The specific embodiment
Sambucus Chinensis extract of the present invention, and the extract pharmacologically active is that involved method is the technological means that those skilled in the art can grasp and use by represented method manufacturing of following embodiment or discovery.But following examples must not be interpreted as the restriction to claim of the present invention of going up in all senses.
Embodiment 1: the preparation of Sambucus Chinensis extract (1)
Get Herba Sambuci Chiensis medical material 100 grams, add 800 milliliters of fluid extracts, add water and make 0.5g crude drug/ml medicinal liquid, stir evenly, filter, filtrate is extracted 3 times by polystyrene type macropore 75% alcohol heating reflux, each 1 hour, merging filtrate, decompression recycling ethanol, simmer down to resin column, first water elution with 5 times of resin volumes, discard water lotion, 80% ethanol elution of 3 times of amounts of reuse column volume is collected 80% ethanol elution, concentrating under reduced pressure, 65 ℃ of degree vacuum dryings get Sambucus Chinensis extract 10.4 grams, and maloic acid content wherein is 0.47%.
Embodiment 2: the preparation of Sambucus Chinensis extract (2)
Get 10 kilograms of Herba Sambuci Chiensis medical materials, adding 80 liter of 75% alcohol heating reflux extracts 3 times, each 1 hour, merging filtrate, being evaporated to relative density is 1.15～1.20 (45 ℃) fluid extract, add water and make 0.5g crude drug/ml medicinal liquid, the high speed centrifugation after-filtration, filtrate is passed through the polystyrene macroporous resin post, first water elution with 5 times of resin volumes, 70% ethanol elution of 3 times of amounts of reuse column volume, collect 70% ethanol elution, decompression (0.09MPa, 65 ℃) concentrates, get Sambucus Chinensis extract 945 grams, maloic acid content wherein is 1.7%.
Embodiment 3: the preparation of Herba Sambuci Chiensis sheet
Prescription:
Sambucus Chinensis extract 380g, starch 40g, dextrin 60g, sucrose 20g, magnesium stearate 3.6g
Method for making: get the Sambucus Chinensis extract by embodiment 2 preparations, add starch, dextrin, sucrose, mixing is granulated, and is dry below 80 ℃, adds magnesium stearate, mix homogeneously, and tabletting, the bag film-coat is made as 1000 altogether.
Embodiment 4: the preparation of laying particle agent
Prescription: Sambucus Chinensis extract 135g, sucrose 600g, dextrin 200g
Method for making: get the Sambucus Chinensis extract by embodiment 2 preparations, with sucrose, dextrin, mixing is granulated, and is dry below 80 ℃, is made as 1000g altogether, the 8g/ bag.
Embodiment 5: the preparation of Herba Sambuci Chiensis syrup
Prescription: Sambucus Chinensis extract 150g, sucrose 500g
Method for making: get the Sambucus Chinensis extract by embodiment 2 preparations, with sucrose, sodium benzoate (in right amount), add water 1000ml stirring and dissolving, 100 ℃ of sterilization 15min filter, and are packed as 10ml/ and prop up.
Claims (10)
1, a kind of Sambucus Chinensis extract for the treatment of hepatopathy is characterized in that, in order to the preparation of below method, described preparation method may further comprise the steps:
(1) with solvent extraction Herba Sambuci Chiensis medical material, gets extractum after concentrating;
(2) extractum of step (1) is through absorption, and elution process gets extract.
2, the extract of claim 1 is characterized in that, Herba Sambuci Chiensis medical material described in the step (1) is that process is chosen the Herba Sambuci Chiensis medical material, cutting, and natural drying obtains.
3, the extract of claim 1 is characterized in that, solvent is selected from water, alcohol, ether, ketone, ester or their mixture described in the step (1).
4, the extract of claim 1 is characterized in that, extracts described in the step (1) to be selected from: immersion, decoction, percolation, extraction, backflow, described concentrating is selected from: natural drying, heat drying, concentrating under reduced pressure, spray drying or lyophilization.
5, the extract of claim 1 is characterized in that, absorption described in the step (2) is through with step (1) gained Herba Sambuci Chiensis extractum, dissolves, and filters; Filtrate is through adsorbing with resin, kieselguhr, silica gel, aluminium oxide or the polyamide chromatography method as adsorbent.
6, the extract of claim 1 is characterized in that, eluting described in the step (2) is with alcohol, water or pure water mixed solvent eluting.
7, the extract of claim 1 is characterized in that, collects eluent after also comprising eluting, and drying eliminates solvent, the process of Sambucus Chinensis extract.
8, the extract of claim 1 is characterized in that, is to prepare through following steps:
(1) chooses Herba Sambuci Chiensis medical material, cutting, natural drying;
(2) adopt water, alcohol (less than five carbon) or pure water mixed solvent, percolation or heating and refluxing extraction by (1) gained Herba Sambuci Chiensis medical material; Add 5-10 and doubly measure solvent, heating and refluxing extraction 1-4 time, each 0.5-3 hour, extract obtained corresponding Herba Sambuci Chiensis fluid extract through concentrating under reduced pressure or lyophilization;
(3) restrain crude drug in whole/milliliter with 40-80 degree hot water dissolving to being equivalent to 0.5 approximately by (2) gained Herba Sambuci Chiensis fluid extract, filter; Filtrate is through resin, kieselguhr, silica gel, aluminium oxide or polyamide adsorbents adsorb, alcohol (less than five carbon) or pure water mixed solvent eluting; Collect eluent, natural evaporation, concentrating under reduced pressure, vacuum drying, spray drying or lyophilization eliminate solvent, promptly get Sambucus Chinensis extract.
9, the extract of claim 8, it is characterized in that, select 40-90% alcohol-water mixed solvent heating and refluxing extraction in the step (2) for use, measure solvents, heating and refluxing extraction 3 times, each 1 hour with 8 times in the step (2), extract obtains corresponding Herba Sambuci Chiensis fluid extract through concentrating under reduced pressure, step is selected macroporous resin for use in (3), selects 60-95% alcohol-water mixed solvent eluting in the step (3) for use, contains in extract obtained to be not less than 1% maloic acid.
10, any pharmaceutical preparation of making as active constituents of medicine with the extract of claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664429B (en) * | 2009-09-15 | 2011-07-20 | 江西天施康中药股份有限公司 | Method for preparing traditional Chinese medicine preparation containing Sambucus chinensis Lindl. extracts |
| US20130287873A1 (en) * | 2012-04-27 | 2013-10-31 | Industrial Technology Research Institute | Pharmaceutical composition and method for preparing a medication for promoting wound healing |
| CN112546085A (en) * | 2020-12-11 | 2021-03-26 | 广西云康健健康管理有限公司 | Sambucus chinensis extract for treating gout and preparation method thereof |
-
2005
- 2005-06-16 CN CNB200510075383XA patent/CN100531748C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664429B (en) * | 2009-09-15 | 2011-07-20 | 江西天施康中药股份有限公司 | Method for preparing traditional Chinese medicine preparation containing Sambucus chinensis Lindl. extracts |
| US20130287873A1 (en) * | 2012-04-27 | 2013-10-31 | Industrial Technology Research Institute | Pharmaceutical composition and method for preparing a medication for promoting wound healing |
| CN112546085A (en) * | 2020-12-11 | 2021-03-26 | 广西云康健健康管理有限公司 | Sambucus chinensis extract for treating gout and preparation method thereof |
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| CN100531748C (en) | 2009-08-26 |
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