CN1969963A - Method for extracting medicament effective component for treating hepatitis and medicinal composition thereof - Google Patents
Method for extracting medicament effective component for treating hepatitis and medicinal composition thereof Download PDFInfo
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Abstract
Disclosed is a process for extracting effective compositions of medicament for treating hepatitis, and the medicinal combinations thereof, wherein the raw materials include herb of stringy stonecrop, giant knotweed rhizome, root of red rooted saliva, glossy ganoderma and pharmaceutically allowable excipient. The preparation can be made into dose forms of tablets, capsules, granules and oral liquids. The obtained product contains polysaccharides, glycosides, anthraquinones and flavones.
Description
Technical field
The present invention relates to a kind of medicine active ingredient extracting method and drug regimen thereof for the treatment of hepatitis, belong to technical field of medicaments.
Background technology
The peaceful drug prescription of hepatoprotective is to form with Chinese medicine Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae and Ganoderma, with Herba Sedi, Rhizoma Polygoni Cuspidati eliminating damp-heat, invigorate blood circulation, go obstinate disease in the liver with tonneau arteries and veins water, Radix Salviae Miltiorrhizae removing blood stasis with potent drugs, Ganoderma can promote the metabolism of liver to medicine, poisonous substance, and full side reaches and improves liver function, protects the liver, the effect of hepatoprotective, thereby reach clearing away heat-damp and promoting diuresis, the liver benefiting blood stasis dispelling, Shugan Zhitong is adapted to various acute hepatitises and chronic hepatitis.To liver pain, uncomfortable in chest, inappetence, abdominal distention, abdominal distention are just clear etc., and symptom can be improved rapidly, and to great three positive, small three positive is turned out cloudy rapidly efficient, to fatty liver, hepatic ascites, liver cirrhosis and complication thereof all have treatment and preventive effect.。Show that according to modern pharmacology experiment its pharmacological action has: 1, start the liver self-healing system: can impel the human body immunologic function of bringing into normal play, start the liver self-healing system, blocking-up autoimmune response, health invigorating and opposing virus capable; 2, improve liver function: recover the normal function of detoxification of liver, make people's running body normal; 3, the liver protecting: anti-liver injury, suppress the rising of LDH in serum SGQT and SGOT rising and the serum; 4, rise hemoglobin: obviously increase blood plasma Hb content.Domestic a lot of research worker has been carried out number of research projects, as: number of patent application is " 2005100012323.3 ", the name be called "
The manufacture method of capsules of Huganning for liver" application; though its product has certain clinical effectiveness clinically; in preparation method, all exist effective component extracting incomplete; or the macromolecular components impurity that exists in the extract such as phlegmatic temperament, natural gum are more etc.; make the drug loading of product unit dose lower; cause drug effect not give full play of or drug effect reduces, usually make the patient will reach therapeutic purposes, must strengthen taking dose, cause the patient to take too much adjuvant, bring unnecessary burden and misery to the patient, bring the hidden danger of drug safety simultaneously; According to the current research result, the active ingredient of Herba Sedi is sarmentosin, flavone and glycosides thereof, triterpene and sterols composition, has the inhibition inflammatory exudation, reduces the effect of hepatocyte injury; The active ingredient of Rhizoma Polygoni Cuspidati is then for being the anthraquinones of representative with the emodin and being the diphenylethylene compounds of representative with the resveratrol, have anti-inflammation, anticancer, protect the liver, effect such as antioxidation; The active ingredient of Radix Salviae Miltiorrhizae is tanshinone and salvianolic acid B; The active ingredient of Ganoderma is a ganoderan etc., and thus, the preparation technology that the demonstration prior art provides is unreasonable; In light of this situation, be badly in need of a kind of more stable quality, technology is feasible product rationally.
Summary of the invention
The invention provides a kind of more stable quality, safer, reasonable feasible a kind of medicine active ingredient extracting method and the drug regimen thereof for the treatment of hepatitis of technology of medication, to solve the problem that prior art exists.The present invention constitutes like this, a kind of medicine active ingredient extracting method for the treatment of hepatitis, it is to be formed by Herba Sedi 850g, Rhizoma Polygoni Cuspidati 500g, Radix Salviae Miltiorrhizae 250g, Ganoderma 200g prescription, calculates by weight, and gets Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, the Ganoderma of recipe quantity, pulverize separately, with water insoluble active ingredients such as ethanol extraction flavones ingredient, anthraquinone component and middle small molecule active compositions, collect these water insoluble active ingredient extracts, refining, concentrate, standby; Medicinal residues are collected these water soluble ingredient extracts with water soluble ingredients such as water extraction glycoside composition, polysaccharide components, and are refining, concentrate, standby; Get the mixture of Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, Ganoderma extract or their extract, make corresponding pharmaceutical preparation with the method for routine.
Described a kind of medicine active ingredient extracting method for the treatment of hepatitis, carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 8 times of amounts, each 1～3 hour, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 50～80%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 50～80%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 70～90% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter merging filtrate, be concentrated into the thick paste shape, add ethanol and make and contain alcohol amount and reach 50～70%, left standstill 12 hours, get supernatant and reclaim ethanol, above-mentioned ethanol extract and precipitate with ethanol supernatant are merged, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, gets extractum C, and is standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, reclaim ethanol, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, and is standby; Medicinal residues add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 70～90%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby;
Described a kind of medicine active ingredient extracting method for the treatment of hepatitis, carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, and each 1～3 hour, filter, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 20000～1000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, and liquid is standby under the film; Liquid filters with the nanofiltration device that the NF membrane that can cut 100～300 molecular weight is housed under the film, liquid on the film is separated with liquid under the film, liquid discards under the film, liquid on the collection membrane, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 thick paste, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 5000～1000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 2000～1000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum C, standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 50000～5000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum D, standby;
Described a kind of medicine active ingredient extracting method for the treatment of hepatitis, carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, each 1～3 hour, filter, merging filtrate concentrates, concentrated solution filters the chromatograph post with gel to be separated, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 20～30MPa, 40～60 ℃ of temperature; Extraction-container pressure is 5～7MPa, and temperature is 40～50 ℃, and cycling extraction 4 hours is collected extract, and is standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter merging filtrate, merging filtrate, filtrate is concentrated into 60 ℃, and to measure relative densities be 1.25～1.30 thick paste, extract with one or more the mixture as solvent in n-butyl alcohol, ethyl acetate, chloroform, ether, petroleum ether, benzene, the toluene, collect extract, reclaim extract, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, with above-mentioned supercritical CO
2Extract mixes with aqueous extract extractum, gets extractum B, and is standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 15～30MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues are entrainer again with ethanol, regulate extraction kettle pressure 20～40MPa, and 60～70 ℃ of temperature began to extract 4 hours, collected extract, merged two kinds of extracts, reclaimed ethanol, got extractum C, and are standby;
(4) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 25～35MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 70～90%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby;
Described a kind of medicine active ingredient extracting method for the treatment of hepatitis, carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, each 1～3 hour, filter, merging filtrate, filtrate is separated with macroporous adsorptive resins, carry out eluting with 30～70% ethanol, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is used the macroporous adsorbent resin eluting, use 0～50% alcoholic solution eluting respectively, collect eluent, above-mentioned ethanol extract and eluent merging are condensed into relative density and are 1.25～1.30 extractum, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is used the macroporous adsorbent resin eluting, use 50～70% alcoholic solution eluting respectively, collect eluent, above-mentioned ethanol extract and eluent merging are condensed into relative density and are 1.25～1.30 extractum, get extractum C, standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is precipitated with protein precipitant, and precipitant comprises: tannic acid, trichloroacetic acid, aluminum acetate, ethacridine, ionic surfactant, Polyethylene Glycol, ammonium sulfate, perchloric acid, wolframic acid, pyrophosphoric acid, zinc salt, mantoquita; Leave standstill, supernatant reuse 80% ethanol precipitation, the collecting precipitation thing gets extractum D, and is standby;
Described a kind of medicine active ingredient extracting method for the treatment of hepatitis, the method for ethanol extraction can be selected a kind of in extracting of reflux, extract,, percolation extraction, supersound extraction, microwave extraction and dipping for use.
Described a kind of drug regimen for the treatment of the medicine active ingredient of hepatitis, it is by Herba Sedi 850g, Rhizoma Polygoni Cuspidati 500g, Radix Salviae Miltiorrhizae 250g, Ganoderma woman's 200g prescription is after extract effective part group, adding an amount of excipient is prepared from, effective part group through extracting can be an extractum A, extractum B, extractum C, a kind of among the extractum D or their mixture, add the excipient that pharmaceutically allows to use and make corresponding pharmaceutical preparation, comprising: injection, the powder pin, freeze-dried powder, gel, tablet, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, all acceptable dosage forms on the pharmaceutics such as extractum and membrane.
Described a kind of drug regimen for the treatment of the medicine active ingredient of hepatitis, the pharmaceutical preparation of making can be tablet, capsule, soft capsule, granule, pill, drop pill and oral liquid.
Among the present invention, extract have protect the liver, the multiple ingredient of hepatoprotective, comprising: containing in the Herba Sedi with the sarmentosin is the glycoside composition of representative, flavones ingredient, alkaloid and the triterpenes components that tricin is representative; Flavones ingredient and phenolic constituents such as anthraquinone components such as the emodin that contains in the Rhizoma Polygoni Cuspidati, physcione, resveratrol, Quercetin; Contain triterpene substances such as ganoderan, Ganodenic acid in tanshinone that contains in the Radix Salviae Miltiorrhizae and salvianolic acid constituents, the Ganoderma and be the adenosine class active substance of essential structure with nucleoside and purine.
Compared with the prior art, technology of the present invention is more rationally feasible, it is effective to make preparation safety, and production is with low cost.The applicant finds through lot of experiments, in the prior art, Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, Ganoderma is all adopted the ethanol cold extraction, the operation that back reuse water normal pressure extracts, though it is method preferably that this method is extracted heat sensitive ingredient, but, just can not extract fully for the insensitive composition of heat, and extract is not made with extra care, impurity in the extract such as phlegmatic temperament, macromolecular substances such as natural gum are not removed, tool is not protected the liver yet, the composition of hepatoprotective separates, and makes and mainly contains the effective component content reduction in the extract, the preparation unit dose drug loading of making is low, and pharmacological action is not obvious, also has zest; Simultaneously, the method for the controlling content of not being correlated with in the quality standard, technology is obviously unreasonable, and the wasting manpower and material resources increases cost, and the products obtained therefrom curative effect does not improve; The invention solves these problems, adopt medical material difference or mixing, at first adopt reflux, extract,, percolation extraction, microwave extraction or adopt carbon dioxide supercritical fluid extraction with ethanol; Medicinal residues extracting in water water soluble ingredient material, water extract concentrate the back and use ethanol precipitation, precipitate water again and return moltenly, and irreversible owing to the macromolecular substances dissolution properties can be removed macromolecular substances such as phlegmatic temperament, natural gum etc.; Perhaps medicinal residues extracting in water water soluble ingredient material adopts membrane separation technique to separate then, according to needed molecular weight size, adopts the film of different molecular weight to separate, and makes the effective ingredient purification; Perhaps medicinal residues extracting in water water soluble ingredient material adopts absorption with macroporous adsorbent resin, gel chromatographic columns separation etc. then.By extracting method of the present invention, the preparation unit's drug loading that is prepared from is had comparatively significantly improve, patient's dose reduces, and drug effect strengthens, and drug safety is guaranteed.A kind of treatment hepatitis medicament effective ingredient provided by the invention and drug regimen thereof provide the extracting method of this effective ingredient, can directly instruct actual production; The effective ingredient that extracts can be prepared into different preparations, selects for clinical worker, and the patient selects to take according to the characteristics of oneself
The conventional method of mentioning in the preparation method provided by the invention, prior art etc. are meant the method that the professional and technical personnel in disclosed technology, this field can consult, implement.
In order to confirm effectiveness of the present invention, the applicant has done a large amount of experiments:
Experimental example I Pharmacodynamic test of active extract
1. materials and methods
1.1 laboratory animal
Kunming mouse (male and female dual-purpose), body weight 18～22g.
1.2 medicine and equipment
The peaceful granule of hepatoprotective is provided specification by Guizhou Xinbang Pharmacy Stock Co., Ltd: the 6g/ bag; Positive reference substance: liver-protecting tablet (5 constant virtues sunflower pharmaceutical factory, lot number: 20001011); Kit for determining alanine aminopherase (east, Wenzhou bowl biological engineering company limited); Automatic biochemistry analyzer (day island proper Tianjin).
1.3 experiment grouping
(1) group: the blank group gavages normal saline 0.2ml/10g by body weight.
(2) group: positive controls gavages liver-protecting tablet 0.2ml/10g (being 0.56g/kg, the clinical equivalent amount).
(3) group: model group gavages normal saline 0.2ml/10g.
(4) group: low dose group gavages the peaceful granule 0.2ml/10g of hepatoprotective (being 0.683g/kg, the clinical equivalent amount).
(5) group: middle dosage group gavages the peaceful granule 0.2ml/10g of hepatoprotective (being 1.365g/kg, the clinical equivalent amount).
(6) group: high dose group gavages the peaceful granule 0.2ml/10g of hepatoprotective (being 2.730g/kg, the clinical equivalent amount).
1.4 experimental technique
15 of every treated animals (random packet), (1) group and (3) group gavage normal saline 0.2ml/10g, 1 time/day; (2) group gavages liver-protecting tablet 0.56g/kg (0.2ml/10g), 1 time/day; (4) (5) (6) group gavages the peaceful granule liquid of the hepatoprotective 0.2ml/10g of respective concentration, 1 time/day.Except that (1) group, other respectively organizes equal modeling: since the CCL of subcutaneous injection 10% on the 1st
4, every 10g body weight 0.1ml, the next day 1 time, inject altogether 4 times.Each is organized drug treatment and is 12d, behind the drug withdrawal 24h (promptly the 13rd day), gets blood, liver mensuration corresponding index.
2. experimental result
Press the kit for determining alanine aminopherase explanation, measure glutamate pyruvate transaminase (ALT), glutamic oxaloacetic transaminase, GOT (AST) content in the serum, the results are shown in Table 1.The pathological examination result of hepatic tissue, 1. model group: it is the hepatocyte edema or the hepatocyte diffusivity edema at center that the liver of each animal all has with the central vein, and the necrosis of hepatic tissue kitchen range shape, lamellar necrosis arranged, companion's lymphocyte, neutrophil infiltration, cell infiltration also has around blood vessel and vasculolymphatic
The peaceful granule of table 1 hepatoprotective is to CCL
4Cause in the mice serum of hepatic injury
(ALT), the influence of (AST) content (X ± SD)
| The group number | The Mus number | ALT(U/100ml) | GOT(U/100ml) |
| 1 3 5 6 | 15 12 15 13 | 467.3±42 788.7±44 633.7±4 605.9±4 | 13 644.4±5 14 679.9±5 |
Annotate: compare * P＜0.01 with model group; Compare #P＜0.01, Δ P＞0.05 with the blank group.
The peaceful granule of table 2 hepatoprotective is to CCL
4Cause the influence of the liver organization of hepatic injury mice
| Group | Mus number (only) | The kitchen range edema | The diffusivity edema | The necrosis of kitchen range shape | The lamellar necrosis | The portal area | Inflammatory cell | Soak into | ||||||||
| + | ++ | +++ | + | ++ | +++ | + | ++ | +++ | + | ++ | +++ | + | ++ | +++ | ||
| 1 2 3 4 5 6 | 10 10 8 9 10 10 | 2 2* 2 - - 2* | 1 - 1 - 1 - | - - - - - - | - 2* - 3* 2* 1 | - 2 3 - 1 - | - - 5 1 - - | - 1 1 2 3* 2* | - 1 3 1 - - | - 1 4 - 1 - | - - - - 2* 1 | - 2 1 3 - - | - - 7 2 1 - | 1 7* - 5* 3* 3 | 1 - 1 - 1 2 | - 1 7 - - - |
Annotate: the equal minute quantity of *.
Characteristics; 2. normal group: animal livers is organized normal substantially; 3. positive controls: the part animal liver tissue has hydropic degeneration, and necrosis less and gently; 4. low dose group: the part animal liver cell has hydropic degeneration and necrosis, but lighter; 5. middle dosage group: the part animal liver cell has hydropic degeneration and necrosis, but less and gently; 6. high dose group: the part animal has hepatocyte edema and the cell infiltration around blood vessel, and hepatic necrosis is slight (seeing Table 2).Each treated animal all has portal area cell infiltration in various degree, and the kind of inflammatory cell mainly is neutrophilic granulocyte and mononuclear cell.
3. experiment conclusion
3.1 the peaceful granule of hepatoprotective can obviously reduce CCL
4The content of poisoning mice serum alt and AST compares P＜0.01 with model group; High dose group (4 times of clinical equivalent dosage) does not have significant difference (P＞0.05) to influence and the blank group of AST; In, low dose group and blank group relatively, P＜0.01; High, medium and low dosage group compares there was no significant difference (P＞0.05) to influence and the positive controls of ALT and AST in the poisoning mice serum.
3.2 the peaceful granule of hepatoprotective is to CCL
4The hepatic tissue of poisoning mice has significant protective effect.
4. discuss
The peaceful granule of hepatoprotective is made up of medicines such as Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, Ganodermas, meets the prescription theory of motherland's medicine fully.Its main component sarmentosin has facilitation to the hepatocyte metabolism, can improve the detoxification ability of liver; Rhizoma Polygoni Cuspidati can reduce in the liver free fatty acid and ALT in the lipids and serum, AST content etc.Each medicine compatibility can be brought into play clearing away heat-damp and promoting diuresis, the liver benefiting blood stasis dispelling, the effect of Shugan Zhitong jointly in the peaceful granule of hepatoprotective.
Specific embodiment
Embodiment 1
(1) get the 850g Herba Sedi and be ground into coarse powder, with 70% alcohol reflux 3 times, each 2 hours, merge ethanol extract, standby; Medicinal residues add the water extraction 2 times of 8 times of amounts, each 1.5 hours, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 65%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum A, standby;
(2) get the 500g Rhizoma Polygoni Cuspidati and be ground into coarse powder, 80% alcohol reflux 2 times, each 2 hours, merge ethanol extract, standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 2 hours, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 65%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum B, standby;
(3) get the 250g Radix Salviae Miltiorrhizae powder and be broken into coarse powder, 80% alcohol reflux 2 times, each 2 hours, merge ethanol extract, standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 1 hour, filter merging filtrate, be concentrated into the thick paste shape, add ethanol and make and contain alcohol amount and reach 60%, left standstill 12 hours, get supernatant and reclaim ethanol, above-mentioned ethanol extract and precipitate with ethanol supernatant are merged, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, gets extractum C, and is standby;
(4) get the 200g Ganoderma powder and be broken into coarse powder, 90% alcohol reflux 2 times, each 4 hours, merge ethanol extract, reclaim ethanol, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, and is standby; Medicinal residues add the water extraction 2 times of 14 times of amounts, each 3 hours, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 80%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby;
(5) it is an amount of to get purified water, adds extractum A, extractum B, extractum C, extractum D, adds stevioside 10g, mixing, filter, filtrate was boiled 1 hour, was cooled to room temperature, added sodium sorbate and made dissolving, add orange oil and purified water to 1000ml, make oral liquid, the 10ml/ bottle, promptly.
Embodiment 2
(1) get the 1700g Herba Sedi and be ground into coarse powder, with 70% ethanol microwave extraction 5 times, each 10 minutes, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 2 times, and each 1.5 hours, filter, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 20000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, and liquid is standby under the film; Liquid filters with the nanofiltration device that the NF membrane that can cut 150 molecular weight is housed under the film, liquid on the film is separated with liquid under the film, liquid discards under the film, liquid on the collection membrane, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 thick paste, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum A, standby;
(2) get the 1000g Rhizoma Polygoni Cuspidati and be ground into coarse powder, 80% ethanol microwave extraction 3 times, each 8 minutes, merge ethanol extract, standby; The water extraction of 10 times of amounts of medicinal residues 3 times, each 2 hours, filter merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 5000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum B, standby;
(3) get the 500g Radix Salviae Miltiorrhizae powder and be broken into coarse powder, 80% ethanol microwave extraction 2 times, each 20 minutes, merge ethanol extract, standby; The water extraction of 10 times of amounts of medicinal residues 3 times, each 1 hour, filter merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 2000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum C, standby;
(4) get the 400g Ganoderma powder and be broken into coarse powder, 90% ethanol extraction 5 times, each 10 minutes, merge ethanol extract, standby; Medicinal residues add the water extraction 2 times of 14 times of amounts, each 3 hours, filter merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 50000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum D, standby;
(5) get extractum A, extractum B, extractum C, extractum D, put in the microwave drying oven, dry below 70 ℃, pulverized 40 mesh sieves, add 5% micropowder silica gel, mix homogeneously, filled capsules is made every 0.25g, promptly.
Embodiment 3
(1) get the 850g Herba Sedi and be ground into coarse powder, with 70% alcohol reflux 3 times, each 2 hours, merge ethanol extract, standby; The decocting that medicinal residues add 8 times of amounts boils 2 times, each 1.5 hours, filter, merging filtrate concentrates, concentrated solution filters the chromatograph post with gel to be separated, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) get the 500g Rhizoma Polygoni Cuspidati and be ground into coarse powder, put supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 20～30MPa, 40～60 ℃ of temperature; Extraction-container pressure is 5～7MPa, and temperature is 40～50 ℃, and cycling extraction 4 hours is collected extract, and is standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 2 hours, filter merging filtrate, merging filtrate, filtrate is concentrated into 60 ℃, and to measure relative densities be 1.25～1.30 thick paste, extract with one or more the mixture as solvent in n-butyl alcohol, ethyl acetate, chloroform, ether, petroleum ether, benzene, the toluene, collect extract, reclaim extract, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, with above-mentioned supercritical CO
2Extract mixes with aqueous extract extractum, gets extractum B, and is standby;
(3) get the 250g Radix Salviae Miltiorrhizae powder and be broken into coarse powder, put supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 15～30MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues are entrainer again with ethanol, regulate extraction kettle pressure 20～40MPa, and 60～70 ℃ of temperature began to extract 4 hours, collected extract, merged two kinds of extracts, reclaimed ethanol, got extractum C, and are standby;
(4) get 200 Ganoderma powder and be broken into coarse powder, put supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 25～35MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues add the water extraction 2 times of 14 times of amounts, each 3 hours, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 70～90%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby;
(5) get above-mentioned extractum A, extractum B, extractum C, extractum D, add pregelatinized Starch 100g, mixing is used 70% alcohol granulation, cold drying, granulate adds an amount of magnesium stearate, mixing, be pressed into tablet, the 300mg/ sheet, with 5% Eudragit E solution wrap film coated tablet, the packing, promptly.
Embodiment 4
(1) get the 850g Herba Sedi and be ground into coarse powder, with 70% alcohol reflux 3 times, each 2 hours, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 2 times, each 1.5 hours, filter, merging filtrate, filtrate is separated with macroporous adsorptive resins, carry out eluting with 40% ethanol, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) get the 500g Rhizoma Polygoni Cuspidati and be ground into coarse powder, 80% alcohol reflux 2 times, each 2 hours, merge ethanol extract, standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 1 hour, filter merging filtrate, filtrate is used the macroporous adsorbent resin eluting, uses 30% alcoholic solution eluting respectively, collects eluent, and above-mentioned ethanol extract and eluent merge, be condensed into relative density and be 1.25～1.30 extractum, extractum B, standby;
(3) get the 250g Radix Salviae Miltiorrhizae powder and be broken into coarse powder, 90% alcohol reflux 2 times, each 2 hours, merge ethanol extract, standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 1 hour, filter merging filtrate, filtrate is used the macroporous adsorbent resin eluting, uses 60% alcoholic solution eluting respectively, collects eluent, and above-mentioned ethanol extract and eluent merge, be condensed into relative density and be 1.25～1.30 extractum, extractum C, standby;
(4) get the 200g Ganoderma powder and be broken into coarse powder, 90% ethanol extraction 3 times, each 1 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 3 times of 10 times of amounts, each 3 hours, filter, merging filtrate, filtrate is precipitated with protein precipitant, and precipitant comprises: tannic acid, trichloroacetic acid, aluminum acetate, ethacridine, ionic surfactant, Polyethylene Glycol, ammonium sulfate, perchloric acid, wolframic acid, pyrophosphoric acid, zinc salt, mantoquita; Leave standstill, supernatant reuse 80% ethanol precipitation, the collecting precipitation thing gets extractum D, and is standby;
(5) getting lactose 460g, soluble starch 440g, Aspartane 7g puts in the mixer and mixed 20 minutes, add above-mentioned extractum A, extractum B, extractum C, extractum D, continue to mix 20 minutes, 14 mesh sieves are granulated, 70 ℃ of dryings, 14 mesh sieve granulate, sift out following fine powder of 40 orders and the above coarse granule of 12 orders with shaking screen, make 1200g altogether, packing, every bag of 6g, promptly.
Claims (8)
1. medicine active ingredient extracting method for the treatment of hepatitis, it is to be formed by Herba Sedi 850g, Rhizoma Polygoni Cuspidati 500g, Radix Salviae Miltiorrhizae 250g, Ganoderma 200g prescription, it is characterized in that: calculate by weight, get Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, the Ganoderma of recipe quantity, pulverize separately is with water insoluble active ingredients such as ethanol extraction flavones ingredient, anthraquinone component and middle small molecule active compositions, collect these water insoluble active ingredient extracts, refining, concentrate, standby; Medicinal residues are collected these water soluble ingredient extracts with water soluble ingredients such as water extraction glycoside composition, polysaccharide components, and are refining, concentrate, standby; Get the mixture of Herba Sedi, Rhizoma Polygoni Cuspidati, Radix Salviae Miltiorrhizae, Ganoderma extract or their extract, make corresponding pharmaceutical preparation with the method for routine.
2. a kind of medicine active ingredient extracting method for the treatment of hepatitis according to claim 1 is characterized in that: extract and carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 8 times of amounts, each 1～3 hour, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 50～80%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, be concentrated into 60 ℃ and measure relative densities 1.10～1.15, add 95% ethanol and carry out precipitate with ethanol, make to contain the alcohol amount and reach 50～80%, filter, decompression filtrate recycling ethanol merges above-mentioned ethanol extract and precipitate with ethanol supernatant, and being concentrated into 60 ℃ in the lump, to measure relative densities be 1.25～1.30 extractum, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 70～90% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter merging filtrate, be concentrated into the thick paste shape, add ethanol and make and contain alcohol amount and reach 50～70%, left standstill 12 hours, get supernatant and reclaim ethanol, above-mentioned ethanol extract and precipitate with ethanol supernatant are merged, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, gets extractum C, and is standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, reclaim ethanol, the mensuration relative density is 1.35～1.40 thick paste when being concentrated into 50 ℃, and is standby; Medicinal residues add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 70～90%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby.
3, a kind of medicine active ingredient extracting method for the treatment of hepatitis according to claim 1 is characterized in that: extract and carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, and each 1～3 hour, filter, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 20000～1000 molecular weight ultrafilter membranes is housed, and liquid on the film is separated with liquid under the film, and liquid discards on the film, and liquid is standby under the film; Liquid filters with the nanofiltration device that the NF membrane that can cut 100～300 molecular weight is housed under the film, liquid on the film is separated with liquid under the film, liquid discards under the film, liquid on the collection membrane, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 thick paste, the thick paste of above-mentioned ethanol extraction is mixed with the thick paste that water is carried, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 5000～1000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 2000～1000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum C, standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues are waved most ethanol, add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate, merging filtrate, filtrate is filtered with the ultrafiltration apparatus that can cut 50000～5000 molecular weight ultrafilter membranes is housed, liquid on the film is separated with liquid under the film, liquid discards on the film, and liquid is concentrated into 60 ℃ to measure relative densities is 1.25～1.30 thick paste under the film, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum D, standby.
4, a kind of medicine active ingredient extracting method for the treatment of hepatitis according to claim 1 is characterized in that: extract and carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, each 1～3 hour, filter, merging filtrate concentrates, concentrated solution filters the chromatograph post with gel to be separated, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 20～30MPa, 40～60 ℃ of temperature; Extraction-container pressure is 5～7MPa, and temperature is 40～50 ℃, and cycling extraction 4 hours is collected extract, and is standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter merging filtrate, merging filtrate, filtrate is concentrated into 60 ℃, and to measure relative densities be 1.25～1.30 thick paste, extract with one or more the mixture as solvent in n-butyl alcohol, ethyl acetate, chloroform, ether, petroleum ether, benzene, the toluene, collect extract, reclaim extract, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, with above-mentioned supercritical CO
2Extract mixes with aqueous extract extractum, gets extractum B, and is standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 15～30MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues are entrainer again with ethanol, regulate extraction kettle pressure 20～40MPa, and 60～70 ℃ of temperature began to extract 4 hours, collected extract, merged two kinds of extracts, reclaimed ethanol, got extractum C, and are standby;
(4) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, puts supercritical CO
2In the extraction kettle, add dehydrated alcohol, regulate extraction kettle pressure 25～35MPa, 40～50 ℃ of temperature begin extraction, and behind extraction 2～4h, the decompression discharging is also collected extract; Medicinal residues add the water extraction 1～5 time of 14 times of amounts, each 1～3 hour, filter, merging filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain alcohol amount and reach 70～90%, left standstill 12 hours, supernatant discards after reclaiming ethanol, and precipitation adds hot water makes dissolving fully, filters, the mensuration relative density was 1.35～1.40 thick paste when filtrate was concentrated into 50 ℃, merge above-mentioned two kinds of extractum, get extractum D, standby.
5, a kind of medicine active ingredient extracting method for the treatment of hepatitis according to claim 1 is characterized in that: extract and carry out according to following steps:
(1) calculate by weight, the Herba Sedi of getting recipe quantity is ground into coarse powder, with 50～90% ethanol extractions 1～5 time, and each 0～5 hour, merge ethanol extract, being evaporated to 60 ℃, to measure relative densities be 1.25～1.30 extractum, standby; The decocting that medicinal residues add 8 times of amounts boils 1～5 time, each 1～3 hour, filter, merging filtrate, filtrate is separated with macroporous adsorptive resins, carry out eluting with 30～70% ethanol, collect eluent, being concentrated into 60 ℃, to measure relative densities be 1.25～1.30 extractum, and the thick paste that the thick paste and the water of above-mentioned ethanol extraction are carried mixes, get extractum A, standby;
(2) calculate by weight, the Rhizoma Polygoni Cuspidati of getting recipe quantity is ground into coarse powder, 70～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is used the macroporous adsorbent resin eluting, use 0～50% alcoholic solution eluting respectively, collect eluent, above-mentioned ethanol extract and eluent merging are condensed into relative density and are 1.25～1.30 extractum, get extractum B, standby;
(3) calculate by weight, the Radix Salviae Miltiorrhizae powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is used the macroporous adsorbent resin eluting, use 50～70% alcoholic solution eluting respectively, collect eluent, above-mentioned ethanol extract and eluent merging are condensed into relative density and are 1.25～1.30 extractum, get extractum C, standby;
(4) calculate by weight, the Ganoderma powder of getting recipe quantity is broken into coarse powder, 80～95% ethanol extractions 1～5 time, and each 1～5 hour, merge ethanol extract, standby; Medicinal residues add the water extraction 1～5 time of 10 times of amounts, each 1～3 hour, filter, merging filtrate, filtrate is precipitated with protein precipitant, and precipitant comprises: tannic acid, trichloroacetic acid, aluminum acetate, ethacridine, ionic surfactant, Polyethylene Glycol, ammonium sulfate, perchloric acid, wolframic acid, pyrophosphoric acid, zinc salt, mantoquita; Leave standstill, supernatant reuse 80% ethanol precipitation, the collecting precipitation thing gets extractum D, and is standby.
6, according to the described a kind of medicine active ingredient extracting method for the treatment of hepatitis of claim 2～5, it is characterized in that: the method for ethanol extraction can be selected a kind of in extracting of reflux, extract,, percolation extraction, supersound extraction, microwave extraction and dipping for use.
7, a kind of drug regimen for the treatment of the medicine active ingredient of hepatitis, it is by Herba Sedi 850g, Rhizoma Polygoni Cuspidati 500g, Radix Salviae Miltiorrhizae 250g, Ganoderma woman's 200g prescription is after extract effective part group, adding an amount of excipient is prepared from, effective part group through extracting can be an extractum A, extractum B, extractum C, a kind of among the extractum D or their mixture, add the excipient that pharmaceutically allows to use and make corresponding pharmaceutical preparation, comprising: injection, the powder pin, freeze-dried powder, gel, tablet, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, all acceptable dosage forms on the pharmaceutics such as extractum and membrane.
8, a kind of drug regimen for the treatment of the medicine active ingredient of hepatitis according to claim 7, it is characterized in that: the pharmaceutical preparation of making can be tablet, capsule, granule, pill.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2353602A3 (en) * | 2009-08-07 | 2011-11-23 | Zheming Jin | Natural pharmaceutical preparations for increasing albumin |
| CN106581186A (en) * | 2016-12-28 | 2017-04-26 | 哈尔滨珍宝制药有限公司 | Pharmaceutical composition and preparation method and application thereof |
| CN106822152A (en) * | 2016-12-28 | 2017-06-13 | 哈尔滨珍宝制药有限公司 | A kind of pharmaceutical composition and its application |
| CN107595714A (en) * | 2017-10-31 | 2018-01-19 | 广东丸美生物技术股份有限公司 | A kind of Gentrin Knotweed P.E and preparation method thereof and the application in cosmetics |
-
2006
- 2006-09-25 CN CN 200610051223 patent/CN1969963A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2353602A3 (en) * | 2009-08-07 | 2011-11-23 | Zheming Jin | Natural pharmaceutical preparations for increasing albumin |
| CN106581186A (en) * | 2016-12-28 | 2017-04-26 | 哈尔滨珍宝制药有限公司 | Pharmaceutical composition and preparation method and application thereof |
| CN106822152A (en) * | 2016-12-28 | 2017-06-13 | 哈尔滨珍宝制药有限公司 | A kind of pharmaceutical composition and its application |
| CN107595714A (en) * | 2017-10-31 | 2018-01-19 | 广东丸美生物技术股份有限公司 | A kind of Gentrin Knotweed P.E and preparation method thereof and the application in cosmetics |
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