CN1899333A - Bupleurum root extract, its preparing method and its use - Google Patents
Bupleurum root extract, its preparing method and its use Download PDFInfo
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- CN1899333A CN1899333A CN 200610099498 CN200610099498A CN1899333A CN 1899333 A CN1899333 A CN 1899333A CN 200610099498 CN200610099498 CN 200610099498 CN 200610099498 A CN200610099498 A CN 200610099498A CN 1899333 A CN1899333 A CN 1899333A
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Abstract
The present invention is a kind of bupleurum root extract and its extracting process and medicinal use, and belongs to the field of Chinese medicine technology. The bupleurum root extract is obtained through extracting bupleurum root with alcohol solution, and contains bupleurum saponin-a in 20-30 wt% and bupleurum saponin-d in 10-20 wt%. The preparation process includes crushing bupleurum root, extraction, concentration, column chromatography, eliminating saccharide, depurating, eluting, decolorizing, concentrating, drying and other steps. The extract has high effective component content, high purity, and excellent medicinal application for resisting inflammation, resisting virus, resisting tumor, regulating incretion, etc.
Description
Technical field
The present invention relates to a kind of Radix Bupleuri extract, its preparation method and application thereof, belong to technical field of Chinese medicines.
Background technology
Radix Bupleuri is Umbelliferae Bupleurum plant, and root is used as medicine.This platymiscium has kind more than 120, and there are 42 kinds, 17 mutation in China, extensive use among the people have 10 surplus kind.Recording only has Radix Bupleuri Scorzonerifolii Bupleu rumscorzonerifolium Willd and a Radix Bupleuri B.chinense DC in the Pharmacopoeia of the People's Republic of China.Its bitter in the mouth, cool in nature is gone into liver, gallbladder meridian.Have reconciling superficies and interior, soothing the liver, yang invigorating function.Cure mainly alternate attacks of chills and fever, fullness in the chest costalgia, bitter taste deafness, headache and dizziness, malaria, dysentery proctoptosis, menoxenia, uterine prolapse etc.
By chemical constitution study, therefrom tell saponin, flavone, lignanoid, coumarin, sterol, polysaccharide, poly alkynes, phenethyl alcohol glycoside, prenol glycosides, volatilization wet goods.Saponin component is its main component, up to the present, kind of saponin constituent surplus therefrom having told about 60, it is oleanane type and Folium Vaccinii vitis-idaeae alkane type that its aglycon of saikoside mainly is divided into two big classes, the former is divided into ether epoxy (I-1), different ring diene (I-2) again, 12-alkene (I-3), same ring diene (I-4), 12-alkene-28-carboxylic acid (I-5), different ring diene-30-carboxylic acid (I-6), 18-alkene type (I-7); The latter is divided into 11-alkene 16-hydroxyl-ether epoxy (II-1), 11-alkene-16,23-hydroxyl-ether epoxy (II-2), 11-alkene-16,20-hydroxyl-ether epoxy (II-3), 12-alkene-11,16,28-hydroxyl-ether epoxy (II-4), 12-alkene-11,28-hydroxyl-15,16-ether epoxy (II-5) etc.Its polysaccharide part is common glucose, rhamnose, sugar, xylose, the pentitol etc. of muttering of barking.
Saikoside can be divided into a, b, c, d, e, f and h, and the wherein active composition of tool is saikoside a and d.Discover that saikoside has effects such as antiinflammatory, antiviral, antitumor, endocrine regulation and immune system.At present, Chinese scholars is applied to saikoside treatment of diseases such as nephropathy, hepatic fibrosis, tumor, has obtained gratifying achievements.
The various preparations of Radix Bupleuri are a lot of on the domestic market now, are used for the treatment of multiple heating diseases such as upper respiratory tract infection, pneumonia, influenza clinically, are a kind of curative effect antipyretic that induces sweat preferably, brought into play important effect in clinical treatment.But owing to use medical material kind confusion, the medicinal part disunity, add its complex chemical composition, active constituent content differs greatly, caused Radix Bupleuri and quality of the pharmaceutical preparations instability thereof, all existed certain problem at aspects such as its curative effect or uses: oral formulations such as tablet, granule, electuary etc. exist dosage big, the defective of DeGrain, need take 4-6 sheet or 10-20g at every turn, make troubles to the patient; Injection then exists toxic and side effects big, causes defectives such as untoward reaction generation.It is reported that the main adverse reaction of injection of Radix Bupleuri has: 1, anaphylactic shock: at routine dose, shock symptom promptly appears in the fastest person of time that reacts in injection process, the slowest after injection 1.5h shock symptom appears, in 5min, fall ill mostly.Show as dizziness, nervous, rapid breathing, pale complexion, extreme cold of the limbs, blood pressure drops etc.2, respiratory response: after the routine dose injection, in 5min, occur breathing hard, symptoms such as uncomfortable in chest, nervous, die Blausucht, asthma, dyspnea.3, cardiovascular system reaction: can cause decreased heart rate, paroxysmal tachycardia.4, dermoreaction: the routine dose injection, the time that reacts falls ill about 30min mostly from injecting back 5min-2d.Show as erubescence, pruritus, red pimple, urticaria, fixed drug eruption etc.
In recent years along with many countries in the world to the further investigation of Radix Bupleuri, consistently think that saikoside is the effective constituent that mainly contains of Radix Bupleuri, the saikoside that obtains through modern Chinese medicine extraction means has peculiar advantage evident in efficacy, that side effect is little than Radix Bupleuri crude drug, and its physiological action and clinical meaning constantly enlarge.At present, in the existing saikoside product, active constituent content is low, and the impurity content height is unfavorable for the performance of medicine effect, and the development of relevant dosage form, so the development of high-purity saikoside product is particularly important.
Summary of the invention
The object of the present invention is to provide a kind of Radix Bupleuri extract, contain the saikoside a and the saikoside d of high level in this extract.
Another object of the present invention is to provide the preparation method of above-mentioned Radix Bupleuri extract.
A further object of the present invention is to provide the application of above-mentioned Radix Bupleuri extract in preparation antiinflammatory, antiviral, antitumor, endocrine regulation and disease of immune system medicine.
Radix Bupleuri extract of the present invention is extracted through alcoholic solution by bupleurum Chinese and obtains, and wherein contains the saikoside a of 20-30% weight portion, the saikoside d of 10-20% weight portion.
Different according to raw material, technology and operation, saikoside a and saikoside d sum preferably account for the 40-50% weight portion of extract total amount in the said extracted thing.In this scope, by the screening of raw material, the optimization of technology, and the good control of operation, can realize that saikoside a and saikoside d sum account for the extract total amount up to 50% result, this is the prior art height that is beyond one's reach, and helps the further utilization of Radix Bupleuri effective ingredient.
Saikoside a and saikoside d sum preferably account under the situation of 40-50% weight portion of extract total amount in the said extracted thing, comprise that the total amount of whole saikosides of saikoside a and saikoside d can account for the 50-90% weight portion of extract total amount, its purity and content have reached high level.
Preparation method of extract of the present invention comprises that dry Radix Bupleuri is pulverized, extracts, concentrated, column chromatography, remove operating process such as sugar, the removal of impurity, eluting, decolouring, concentrated, drying, is specially following steps:
I. Radix Bupleuri is pulverized, the alcoholic solution that adds 6-10 times of Radix Bupleuri weight reflux, extract, 1-3 time in 75-85 ℃ of water-bath was extracted 1-3 hour at every turn, merge extractive liquid,, and at 35-50 ℃ of following concentrating under reduced pressure, must concentrated solution, make a living 2-4 times of weight of dose of concentrated liquid measure;
II. concentrated solution is passed through the D101 macroporous resin column, standing adsorption 2-3 hour, the distillation washing post with 8-12 times of resin column loading amount volume removed sugar then, and the 40-60% ethanol of reuse 1-2 times of resin column loading amount volume is washed the post removal of impurity;
III. use the alcoholic solution of 4-6 times of resin column loading amount volume to carry out eluting, collect eluent, by the decolouring of D280 decolorizing column, the decolouring back is at 35-50 ℃ of following concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain at 1.05-1.20.
Among the step I of above-mentioned preparation method, preferred Radix Bupleuri grinding mode is that Radix Bupleuri is crushed to the 10-20 order.
Alcoholic solution among described step I and the III is preferably the 60-80% ethanol water.
Among the described step I, the alcoholic solution consumption is preferably 8 times of Radix Bupleuri weight, and bath temperature is preferably 80 ℃, and extraction time is preferably 3 times, each 1 hour; Concentrated liquid measure is preferably 3 times of weight of crude drug amount.
Among the described Step II I, the alcoholic solution consumption is preferably 5 times of resin column loading amount volumes.
In the described Step II, the distilled water consumption is preferably 10 times of resin column loading amount volumes, washes the ethanol water concentration that the post removal of impurity uses and is preferably 50%.
Extract active constituent content height of the present invention, purity height in antiinflammatory, antiviral, antitumor, endocrine regulation and disease of immune system, have fine medicinal application.According to the actual drug needs, can be prepared into injection or solid orally ingestible.
Radix Bupleuri extract of the present invention can add one or more pharmaceutically acceptable carriers, make pharmaceutical preparation, described pharmaceutically acceptable carrier is meant the various kinds of drug adjuvant of pharmaceutical field routine, includes but not limited to: mannitol, sorbitol, dextran, glucose, lactose, sucrose, sodium chloride, hypromellose, low-substituted hydroxypropyl cellulose, crospolyvinylpyrrolidone, polyvinylpyrrolidone, microcrystalline Cellulose, poloxamer, Tween 80, carboxymethyl starch sodium, pregelatinized Starch, starch, silicon dioxide, xylitol, Macrogol 4000-6000, beta-schardinger dextrin-, cross-linking sodium carboxymethyl cellulose, carboxymethylcellulose calcium or acrylic resin or its combination in any.
Above-mentioned pharmaceutical preparation is according to the needs of different way of administration, can be made into injection, oral formulations, snuffing is gone into or parenteral formulations, is applied to the patient of different crowd.
Be used for when oral, can be made into conventional solid preparation, as tablet, powder, granule, capsule etc.; Make liquid preparation, as water or oil-suspending agent or other liquid preparation, as syrup, elixir etc.; Preferred form is lyophilized injectable powder, tablet, capsule, injection, and wherein tablet can be ordinary tablet, dispersible tablet, oral cavity disintegration tablet, slow releasing tablet, controlled release tablet, effervescent tablet, general thin coated tablet etc.
Described injection includes but not limited to: little liquid drugs injection, freeze-dried powder, powder pin or intravenous fluid etc.
Described solid orally ingestible includes but not limited to: conventional tablet, oral cavity disintegration tablet, dispersible tablet, slow releasing tablet, controlled release tablet, effervescent tablet, thin membrane coated tablet, hard capsule, slow releasing capsule, controlled release capsule, soft capsule, drop pill, granule, effervescent granule etc.
The inventor goes out cover bupleurum root medicinal preparation prescription and preparation method thereof through studying for many years, testing with modernization of Chinese medicine theory and method summary, and is specific as follows:
The saikoside lyophilized injectable powder, its key component is by weight:
Radix Bupleuri extract 1-500 part
Mannitol 1-200 part
Water for injection 10-1000ml
Preparation method: Radix Bupleuri extract, mannitol are accurately claimed to decide by prescription, with the water for injection dissolving fully, add the 0.1-3% activated carbon, (under 20-60 ℃ of situation, stirring 10-100 minute) stirs, adding hydrochloric acid or sodium hydroxide adjusting PH is between the 2-7.0, decarburization is filtered, and the filter membrane with 0.1-0.9 μ m filters 1-3 time then, gets final product packing, the false add plug advances the freeze drying box drying.
Saikoside injection (50-100ml), its key component is by weight:
Radix Bupleuri extract 25-100 part
Tween 80 1-5 part
Chitosan (self-control deacylated tRNA degree 92%) solution (1.5mg/ml) 0.1-50 part
Sodium chloride (9g/1000ml) 0.1-9 part
Water for injection adds to 10-1000ml
Preparation method: principal agent is dissolved in the proper amount of water for injection, adds chitosan solution, heated and stirred again, 40-70 ℃ of insulation is after 20-60 minute, add tween 80, sodium chloride, stirred 10-50 minute, regulate pH value between the 3-8, add the 0.05-6% activated carbon, stirred 10-50 minute, decarburization is filtered, and adds the injection water and puts in place, with 0.1-6 μ filtering with microporous membrane, get final product fill.
The dispersible tablet of saikoside, its key component is by weight:
Radix Bupleuri extract 25-100 part
Microcrystalline Cellulose 30-200 part
Pregelatinized Starch 10-50 part
Silicon dioxide 5-20 part
Aspartame 1-10 part
Orange flavor 1-7 part
Carboxymethyl starch sodium 1-8 part
Magnesium stearate 0.5-5 part
2% polyvinylpyrrolidone K30 (ethanol: solution (binding agent) 2-20 part water=2: 8)
Preparation method: with Radix Bupleuri extract, microcrystalline Cellulose, pregelatinized Starch, silicon dioxide mix homogeneously, cross the 30-150 mesh sieve, mix, (ethanol: water=2: 8) solution is made soft material to add 1-20% polyvinylpyrrolidone K30, granulate with the 20-50 order, under 50-60 ℃ of condition aeration-drying 1-9 hour,, add aspartame, orange flavor, carboxymethyl starch sodium, magnesium stearate etc. and always mix promptly with 10-20 order granulate.
The saikoside oral cavity disintegration tablet, its key component is by weight:
Radix Bupleuri extract 25-100 part
Microcrystalline Cellulose 30-200 part
Crospolyvinylpyrrolidone 10-150 part
Silicon dioxide 5-20 part
Mannitol 10-50 part
Menthol 0.5-5 part
Aspartame 1-15 part
Essence 1-15 part
Preparation method: after accurately title was decided by prescription with main auxiliary material, fully mix homogeneously was crossed 20-60 mesh sieve twice, gets final product tabletting (direct pressure closing).
The effervescent tablet of saikoside, its key component is by weight:
Radix Bupleuri extract 25-100 part
Anhydrous citric acid 50-1000 part
Sodium bicarbonate 50-1000 part
Lactis Anhydrous 20-200 part
Aspartame 5-100 part
Polyethylene glycol 6000 10-100 part
Crospolyvinylpyrrolidone 1-20 part
Dehydrated alcohol 20-200 part
Essence 1-5 part
Preparation method:
1) crospolyvinylpyrrolidone, dehydrated alcohol are made into the 1-15% ethanol solution, standby.
2) Radix Bupleuri extract, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous are fed intake surely by the accurate title of prescription, with 30-60 ℃ of aeration-drying, 12-36 hour standby.
3) with dried Radix Bupleuri extract, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous mix homogeneously, add above-mentioned stock solution and make soft material, to granulate with the 10-30 order, 30-60 ℃ of aeration-drying is with 10-20 order granulate.
4) add aspartame, polyethylene glycol 6000 mix homogeneously behind the granulate after, get final product tabletting.
The general thin coated tablet of saikoside, its key component is by weight:
Radix Bupleuri extract 25-100 part
Starch 10-80 part
Microcrystalline Cellulose 5-30 part
Hydroxypropyl emthylcellulose 1-5 part
Silicon dioxide 2-20 part
Carboxymethyl starch sodium 1-10 part
Magnesium stearate 1-5 part
Preparation method:
1) Radix Bupleuri extract, starch, microcrystalline Cellulose are accurately claimed fully mix homogeneously of fixed back, make soft material with 1-20% hydroxypropyl emthylcellulose aqueous solution, with 10-30 mesh sieve system granule.
2) granule is with 30-60 ℃ of aeration-drying, and moisture Control is between 1.5%-10%, with 10-30 mesh sieve granulate.
3) add silicon dioxide, carboxymethyl starch sodium, magnesium stearate mix homogeneously after, get final product tabletting.
4) preparation of coating solution (by weight)
Hydroxypropyl emthylcellulose 1-5 part
Polyethylene glycol 6000 0.5-3 part
Oleum Ricini 0.5-3 part
Diethyl phthalate 0.5-3 part
95% ethanol 1-10 part
It is fixed that above supplementary material is accurately claimed, stirs, and until dissolving fully, it is standby to cross the 50-150 mesh sieve.
5) pack film-coat according to a conventional method.
The hard capsule of saikoside, its key component is by weight:
Radix Bupleuri extract 25-100 part
Carboxymethyl starch sodium 10-100 part
Silicon dioxide 2-20 part
Magnesium stearate 0.5-5 part
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, last fully-automatic capsule filling machine fill hard capsule.
The granule of saikoside (Sugarless type), its key component is by weight:
Radix Bupleuri extract 25-100 part
Xylitol 20-200 part
Sucrose 20-200 part
Microcrystalline Cellulose 20-100 part
Hypromellose 1-5 part
Silica 1-20 part
Preparation method: it is fixed that main and auxiliary raw material is accurately claimed by prescription, add 3-30% hydroxypropyl emthylcellulose aqueous solution, make soft material, granulate with the 10-30 mesh sieve, with 30-70 ℃ of aeration-drying, with 80 orders and the screening of 10 mesh sieves, behind the granule of removal＜80 and＞10 mesh sieves, pack promptly with particles packing machine.
In the above-mentioned preparation, Radix Bupleuri extract and adjuvant preferred weight proportioning are 1: 1-1: 100, be preferably 1: 20-1: and 60, most preferably be 1: 40.
Radix Bupleuri extract of the present invention can be according to variations such as the type of route of administration, patient's age, body weight, the disease for the treatment of and the orders of severity, and its daily dose can be the 0.01-10mg/kg body weight, and preferred 0.1-5mg/kg body weight can be used by one or many.
Radix Bupleuri extract preparation method of the present invention is pharmacy theory and the method with the modernization of Chinese medicine, extraction, separation, purification Chinese medicine, the control of technology, especially temperature controlling, make active component saikoside a, saikoside d in the Radix Bupleuri be able to maximum reservation, become the key component of extract, and qualitative, quantitative with modern detection means, the active component in the Radix Bupleuri is quantized in pharmaceutical preparation first.
The inventor finds that by the Radix Bupleuri extract of the inventive method preparation, at aspects such as antiinflammatory, antiviral, antitumor, endocrine regulation and immune systems, under same condition, therapeutic effect is more remarkable than existing bupleurum preparation.
The inventor finds that also because the saponin component is single in the prepared Radix Bupleuri extract, the purity height make it show very low toxicity in pharmaceutical applications, and side effect is little.
Description of drawings
Fig. 1: saikoside standard substance finger printing
Saikoside a (24.229), saikoside d (35.364)
Fig. 2: embodiment 1 product fingerprint collection of illustrative plates
Saikoside a (24.234), saikoside d (36.137)
The specific embodiment
Embodiment 1
After the Radix Bupleuri clean dry, be crushed to 10 orders, 70% ethanol that adds 8 times of Radix Bupleuri weight reflux, extract, 3 times in 80 ℃ of water-baths each 1 hour, merges three times extracting solution, at 45 ℃ of concentrating under reduced pressure, concentrated liquid measure is controlled to be 3 times of Radix Bupleuri crude drug amount, with D101 macroporous resin column on the concentrated solution, and standing adsorption 2 hours, distillation washing post with 10 times of resin column loading amount volumes removes sugar then, and 50% ethanol of 1 times of resin column loading amount of reuse volume is washed the post removal of impurity; 70% ethanol elution with 5 times of resin column loading amount volumes, collect eluent, last D280 decolorizing column, the decolouring back is at 45 ℃ of concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain Radix Bupleuri extract 1.05, after testing, saikoside a content is 25.33%, and saikoside d content is 15.41%, and total saponin content is 53.65%.
Embodiment 2
After the Radix Bupleuri clean dry, be crushed to 20 orders, 60% ethanol that adds 10 times of Radix Bupleuri weight reflux, extract, 2 times in 85 ℃ of water-baths, each 2 hours, merge extractive liquid,, at 40 ℃ of concentrating under reduced pressure, concentrated liquid measure is controlled to be 2 times of Radix Bupleuri crude drug amount, with D101 macroporous resin column on the concentrated solution, and standing adsorption 3 hours, distillation washing post with 8 times of resin column loading amount volumes removes sugar then, and 40% ethanol of 2 times of resin column loading amounts of reuse volume is washed the post removal of impurity; 60% ethanol elution with 6 times of resin column loading amount volumes, collect eluent, last D280 decolorizing column, the decolouring back is at 40 ℃ of concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain Radix Bupleuri extract 1.20, after testing, saikoside a content is 29.25%, and saikoside d content is 12.85%, and total saponin content is 56.20%.
Embodiment 3
After the Radix Bupleuri clean dry, be crushed to 20 orders, 80% ethanol that adds 6 times of Radix Bupleuri weight reflux, extract, 3 hours in 75 ℃ of water-baths, with extracting solution at 50 ℃ of concentrating under reduced pressure, concentrated liquid measure is controlled to be 4 times of Radix Bupleuri crude drug amount, with D101 macroporous resin column on the concentrated solution, and standing adsorption 2 hours, distillation washing post with 12 times of resin column loading amount volumes removes sugar then, and 60% ethanol of 1.5 times of resin column loading amounts of reuse volume is washed the post removal of impurity; 80% ethanol elution with 4 times of resin column loading amount volumes, collect eluent, last D280 decolorizing column, the decolouring back is at 50 ℃ of concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain Radix Bupleuri extract 1.10, after testing, saikoside a content is 20.91%, and saikoside d content is 11.15%, and total saponin content is 78.55%.
Embodiment 4
After the Radix Bupleuri clean dry, be crushed to 10 orders, 75% ethanol that adds 9 times of Radix Bupleuri weight reflux, extract, 3 times in 80 ℃ of water-baths each 2 hours, merges three times extracting solution, at 45 ℃ of concentrating under reduced pressure, concentrated liquid measure is controlled to be 2 times of Radix Bupleuri crude drug amount, with D101 macroporous resin column on the concentrated solution, and standing adsorption 2 hours, distillation washing post with 9 times of resin column loading amount volumes removes sugar then, and 55% ethanol of 2 times of resin column loading amounts of reuse volume is washed the post removal of impurity; 75% ethanol elution with 5.5 times of resin column loading amount volumes, collect eluent, last D280 decolorizing column, the decolouring back is at 45 ℃ of concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain Radix Bupleuri extract 1.15, after testing, saikoside a content is 21.65%, and saikoside d content is 17.24%, and total saponin content is 65.66%.
Embodiment 5
After the Radix Bupleuri clean dry, be crushed to 20 orders, 65% ethanol that adds 7 times of Radix Bupleuri weight reflux, extract, 2 times in 65 ℃ of water-baths each 3 hours, merges extracted twice liquid, at 35 ℃ of concentrating under reduced pressure, concentrated liquid measure is controlled to be 3 times of Radix Bupleuri crude drug amount, with D101 macroporous resin column on the concentrated solution, and standing adsorption 2.5 hours, distillation washing post with 11 times of resin column loading amount volumes removes sugar then, and 45% ethanol of 2 times of resin column loading amounts of reuse volume is washed the post removal of impurity; 65% ethanol elution with 4.5 times of resin column loading amount volumes, collect eluent, last D280 decolorizing column, the decolouring back is at 35 ℃ of concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain Radix Bupleuri extract 1.20, after testing, saikoside a content is 28.75%, and saikoside d content is 13.54%, and total saponin content is 89.36%.
Embodiment 6
The preparation of saikoside lyophilized injectable powder.
Get following weight portion meter component:
Embodiment 1 product 1g
Mannitol 200g
Water for injection 1000ml
Preparation method: embodiment 1 product, mannitol are accurately claimed to decide by prescription, with the water for injection dissolving fully, add 0.1% pin activated carbon, (under 60 ℃ of situations, stirring 10 minutes) stirs, adding hydrochloric acid or sodium hydroxide adjusting PH is 2, decarburization is filtered, and the filter membrane with 0.4 μ m and 0.22 μ m respectively filters once then, gets final product packing, the false add plug advances the freeze drying box drying.
Embodiment 7
The preparation of saikoside lyophilized injectable powder.
Get following weight portion meter component:
Embodiment 2 product 500g
Mannitol 1g
Water for injection 1000ml
Preparation method: embodiment 1 product, mannitol are accurately claimed to decide by prescription, with the water for injection dissolving fully, add 30% pin activated carbon, (under 20 ℃ of situations, stirring 100 minutes) stirs, adding hydrochloric acid or sodium hydroxide adjusting PH is 7.0, decarburization is filtered, and the filter membrane with 0.4 μ m and 0.22 μ m respectively filters once then, gets final product packing, the false add plug advances the freeze drying box drying.
Embodiment 8
The preparation of saikoside lyophilized injectable powder.
Get following weight portion meter component:
Embodiment 3 product 250g
Mannitol 100g
Water for injection 1000ml
Preparation method: embodiment 1 product, mannitol are accurately claimed to decide by prescription, with the water for injection dissolving fully, add 15% pin activated carbon, (under 30 ℃ of situations, stirring 60 minutes) stirs, adding hydrochloric acid or sodium hydroxide adjusting PH is 4.0, decarburization is filtered, and the filter membrane with 0.4 μ m and 0.22 μ m respectively filters once then, gets final product packing, the false add plug advances the freeze drying box drying.
Embodiment 9
The preparation of saikoside injection liquor (50-100ml).
Get following weight portion meter component:
Embodiment 4 product 25g
Tween 80 5g
Chitosan (self-control deacylated tRNA degree 92%) solution (1.5mg/ml) 2.5% 0.1g
Sodium chloride (9g/1000ml) 9g
Water for injection adds to 1000ml.
Preparation method: principal agent is dissolved in the proper amount of water for injection, adds chitosan solution, heated and stirred again, 40 ℃ of insulations are after 60 minutes, add tween 80, sodium chloride, stirred 10 minutes, regulate between the pH value to 8, add 0.05% activated carbon, stirred 50 minutes, decarburization is filtered, and adds the injection water and puts in place, with 0.22 μ m and 0.4 μ m filtering with microporous membrane, get final product fill.
Embodiment 10
The preparation of saikoside injection (50-100ml).
Get following weight portion meter component:
Embodiment 5 product 60g
Tween 80 2.5g
Chitosan (self-control deacylated tRNA degree 92%) solution (1.5mg/ml) 2.5% 25g
Sodium chloride (9g/1000ml) 4.5g
Water for injection adds to 500ml
Preparation method: principal agent is dissolved in the proper amount of water for injection, adds chitosan solution, heated and stirred again, 50 ℃ of insulations are after 40 minutes, add tween 80, sodium chloride, stirred 30 minutes, regulate pH value to 5, add 3% activated carbon, stirred 30 minutes, decarburization is filtered, and adds the injection water and puts in place, with 0.22 μ m and 0.4 μ m filtering with microporous membrane, get final product fill.
Embodiment 11
The preparation of saikoside injection liquor (50-100ml).
Get following weight portion meter component:
Embodiment 1 product 100g
Tween 80 1g
Chitosan (self-control deacylated tRNA degree 92%) solution (1.5mg/ml) 2.5% 50g
Sodium chloride (9g/1000ml) 0.1g
Water for injection adds to 10ml
Preparation method: principal agent is dissolved in the proper amount of water for injection, adds chitosan solution, heated and stirred again, 70 ℃ of insulations are after 20 minutes, add tween 80, sodium chloride, stirred 50 minutes, regulate between the pH value to 3, add 6% activated carbon, stirred 10 minutes, decarburization is filtered, and adds the injection water and puts in place, with 0.22 μ m and 0.4 μ m filtering with microporous membrane, get final product fill.
Embodiment 12
The preparation of saikoside dispersible tablet.
Get following weight portion meter component:
Embodiment 2 product 25g
Microcrystalline Cellulose 200g
Pregelatinized Starch 10g
Silicon dioxide 20g
Aspartame 1g
Orange flavor 7g
Carboxymethyl starch sodium 1g
Magnesium stearate 5g
2% polyvinylpyrrolidone K30 (ethanol: solution (binding agent) 2g water=2: 8)
Preparation method: with embodiment 1 product, microcrystalline Cellulose, pregelatinized Starch, silicon dioxide mix homogeneously, cross 30 mesh sieves, mix, (ethanol: water=2: 8) solution is made soft material to add 20% polyvinylpyrrolidone K30, granulate with 20 orders, aeration-drying is 1 hour under 60 ℃ of conditions, with 20 order granulate, adds aspartame, orange flavor, carboxymethyl starch sodium, magnesium stearate etc. and always mixes promptly.
Embodiment 13
The preparation of saikoside dispersible tablet.
Get following weight portion meter component:
Embodiment 3 product 100g
Microcrystalline Cellulose 30g
Pregelatinized Starch 50g
Silicon dioxide 5g
Aspartame 10g
Orange flavor 1g
Carboxymethyl starch sodium 8g
Magnesium stearate 0.5g
2% polyvinylpyrrolidone K30 (ethanol: solution (binding agent) 20g water=2: 8)
Preparation method: with embodiment 1 product, microcrystalline Cellulose, pregelatinized Starch, silicon dioxide mix homogeneously, cross 150 mesh sieves, mix, (ethanol: water=2: 8) solution is made soft material to add 1% polyvinylpyrrolidone K30, granulate with 50 orders, aeration-drying is 9 hours under 50 ℃ of conditions, with 10 order granulate, adds aspartame, orange flavor, carboxymethyl starch sodium, magnesium stearate etc. and always mixes promptly.
Embodiment 14
The preparation of saikoside dispersible tablet.
Get following weight portion meter component:
Embodiment 4 product 60g
Microcrystalline Cellulose 115g
Pregelatinized Starch 30g
Silica 1 2g
Aspartame 6g
Orange flavor 4g
Carboxymethyl starch sodium 5g
Magnesium stearate 3g
2% polyvinylpyrrolidone K30 (ethanol: solution (binding agent) 10g water=2: 8)
Preparation method: with embodiment 1 product, microcrystalline Cellulose, pregelatinized Starch, silicon dioxide mix homogeneously, cross 90 mesh sieves, mix, (ethanol: water=2: 8) solution is made soft material to add 10% polyvinylpyrrolidone K30, granulate with 35 orders, aeration-drying is 5 hours under 55 ℃ of conditions, with 30 order granulate, adds aspartame, orange flavor, carboxymethyl starch sodium, magnesium stearate etc. and always mixes promptly.
Embodiment 15
The preparation of saikoside oral cavity disintegration tablet.
Get following weight portion meter component:
Embodiment 5 product 25g
Microcrystalline Cellulose 200g
Crospolyvinylpyrrolidone 10g
Silicon dioxide 20g
Mannitol 10g
Menthol 5g
Aspartame 1g
Essence 15g
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, cross 20,30 mesh sieves each once, get final product tabletting (direct pressure closing).
Embodiment 16
The preparation of saikoside oral cavity disintegration tablet.
Get following weight portion meter component:
Embodiment 1 product 100g
Microcrystalline Cellulose 30g
Crospolyvinylpyrrolidone 150g
Silicon dioxide 5g
Mannitol 50g
Menthol 0.5g
Aspartame 15g
Essence 1g
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, cross 50,60 mesh sieves each once, get final product tabletting (direct pressure closing).
Embodiment 17
The preparation of saikoside oral cavity disintegration tablet.
Get following weight portion meter component:
Embodiment 2 product 60g
Microcrystalline Cellulose 110g
Crospolyvinylpyrrolidone 80g
Silica 1 2g
Mannitol 30g
Menthol 2.5g
Aspartame 8g
Essence 8g
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, cross 30,40 mesh sieves each once, get final product tabletting (direct pressure closing).
Embodiment 18
The preparation of saikoside effervescent tablet.
Get following weight portion meter component:
Embodiment 3 product 25g
Anhydrous citric acid 1000g
Sodium bicarbonate 50g
Lactis Anhydrous 200g
Aspartame 5g
Polyethylene glycol 6000 100g
Crospolyvinylpyrrolidone 1g
Dehydrated alcohol 200g
Essence 1g
Preparation method:
1) crospolyvinylpyrrolidone, dehydrated alcohol are made into 1% ethanol solution, standby.
2) embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous are fed intake surely by the accurate title of prescription, with 60 ℃ of aeration-dryings, 12 hours standby.
3) with dried embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous mix homogeneously, add above-mentioned stock solution and make soft material, granulate with 10 orders, 60 ℃ of aeration-dryings are with 10 order granulate.
4) add aspartame, polyethylene glycol 6000 mix homogeneously behind the granulate after, get final product tabletting.
Embodiment 19
The preparation of saikoside effervescent tablet.
Get following weight portion meter component:
Embodiment 4 product 100g
Anhydrous citric acid 50g
Sodium bicarbonate 1000g
Lactis Anhydrous 20g
Aspartame 100g
Polyethylene glycol 6000 10g
Crospolyvinylpyrrolidone 20g
Dehydrated alcohol 20g
Essence 5g
Preparation method:
1) crospolyvinylpyrrolidone, dehydrated alcohol are made into 15% ethanol solution, standby.
2) embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous are fed intake surely by the accurate title of prescription, with 30 ℃ of aeration-dryings, 36 hours standby.
3) with dried embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous mix homogeneously, add above-mentioned stock solution and make soft material, granulate with 10 orders, 60 ℃ of aeration-dryings are with 10 order granulate.
4) add aspartame, polyethylene glycol 6000 mix homogeneously behind the granulate after, get final product tabletting.
Embodiment 20
The preparation of saikoside effervescent tablet.
Get following weight portion meter component:
Embodiment 5 product 60g
Anhydrous citric acid 500g
Sodium bicarbonate 500g
Lactis Anhydrous 110g
Aspartame 50g
Polyethylene glycol 6000 55g
Crospolyvinylpyrrolidone 10g
Dehydrated alcohol 110g
Essence 2.5g
Preparation method:
1) crospolyvinylpyrrolidone, dehydrated alcohol are made into 8% ethanol solution, standby.
2) embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous are fed intake surely by the accurate title of prescription, with 45 ℃ of aeration-dryings, 24 hours standby.
3) with dried embodiment 1 product, anhydrous citric acid, sodium bicarbonate, Lactis Anhydrous mix homogeneously, add above-mentioned stock solution and make soft material, granulate with 20 orders, 45 ℃ of aeration-dryings are with 15 order granulate.
4) add aspartame, polyethylene glycol 6000 mix homogeneously behind the granulate after, get final product tabletting.
Embodiment 21
The preparation of saikoside general thin coated tablet.
Get following weight portion meter component:
Embodiment 1 product 25g
Starch 80g
Microcrystalline Cellulose 5g
Hydroxypropyl emthylcellulose 5g
Silicon dioxide 2g
Carboxymethyl starch sodium 10g
Magnesium stearate 1g
Preparation method:
1) saikoside, starch, microcrystalline Cellulose are accurately claimed fully mix homogeneously of fixed back, make soft material with 1% hydroxypropyl emthylcellulose aqueous solution, with 30 mesh sieve system granules.
2) granule is with 30 ℃ of aeration-dryings, and moisture Control is 10%, with 10 mesh sieve granulate.
3) add silicon dioxide, carboxymethyl starch sodium, magnesium stearate mix homogeneously after, get final product tabletting.
4) preparation of coating solution (by weight)
Hydroxypropyl emthylcellulose 1g
Polyethylene glycol 6000 3g
Oleum Ricini 0.5g
Diethyl phthalate 3g
95% ethanol 1g
It is fixed that above supplementary material is accurately claimed, stirs, and until dissolving fully, it is standby to cross 50 mesh sieves.
5) pack film-coat according to a conventional method.
Embodiment 22
The preparation of saikoside general thin coated tablet.
Get following weight portion meter component:
Embodiment 2 product 100g
Starch 10g
Microcrystalline Cellulose 30g
Hydroxypropyl emthylcellulose 1g
Silicon dioxide 20g
Carboxymethyl starch sodium 1g
Magnesium stearate 5g
Preparation method:
1) saikoside, starch, microcrystalline Cellulose are accurately claimed fully mix homogeneously of fixed back, make soft material with 20% hydroxypropyl emthylcellulose aqueous solution, with 10 mesh sieve system granules.
2) granule is with 60 ℃ of aeration-dryings, and moisture Control is 1.5%, with 30 mesh sieve granulate.
3) add silicon dioxide, carboxymethyl starch sodium, magnesium stearate mix homogeneously after, get final product tabletting.
4) preparation of coating solution (by weight)
Hydroxypropyl emthylcellulose 5g
Polyethylene glycol 6000 0.5g
Oleum Ricini 3g
Diethyl phthalate 0.5g
95% ethanol 10g
It is fixed that above supplementary material is accurately claimed, stirs, and until dissolving fully, it is standby to cross 150 mesh sieves.
5) pack film-coat according to a conventional method.
Embodiment 23
The preparation of saikoside general thin coated tablet.
Get following weight portion meter component:
Embodiment 3 product 60g
Starch 45g
Microcrystalline Cellulose 17g
Hydroxypropyl emthylcellulose 3g
Silica 1 1g
Carboxymethyl starch sodium 5g
Magnesium stearate 3g
Preparation method:
1) saikoside, starch, microcrystalline Cellulose are accurately claimed fully mix homogeneously of fixed back, make soft material with 10% hydroxypropyl emthylcellulose aqueous solution, with 15 mesh sieve system granules.
2) granule is with 45 ℃ of aeration-dryings, and moisture Control is 5%, with 20 mesh sieve granulate.
3) add silicon dioxide, carboxymethyl starch sodium, magnesium stearate mix homogeneously after, get final product tabletting.
4) preparation of coating solution (by weight)
Hydroxypropyl emthylcellulose 3g
Polyethylene glycol 6000 1.7g
Oleum Ricini 1.8g
Diethyl phthalate 1.7g
95% ethanol 5.5g
It is fixed that above supplementary material is accurately claimed, stirs, and until dissolving fully, it is standby to cross 100 mesh sieves.
5) pack film-coat according to a conventional method.
Embodiment 24
The preparation of saikoside hard capsule.
Get following weight portion meter component:
Embodiment 4 product 25g
Carboxymethyl starch sodium 100g
Silicon dioxide 2g
Magnesium stearate 5g
Preparation method:
With main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, last fully-automatic capsule filling machine fill hard capsule.
Embodiment 25
The preparation of saikoside hard capsule.
Get following weight portion meter component:
Embodiment 5 product 100g
Carboxymethyl starch sodium 10g
Silicon dioxide 20g
Magnesium stearate 0.5g
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, last fully-automatic capsule filling machine fill hard capsule.
Embodiment 26
The preparation of saikoside hard capsule.
Get following weight portion meter component:
Embodiment 1 product 60g
Carboxymethyl starch sodium 55g
Silica 1 1g
Magnesium stearate 2.5g
Preparation method: with main auxiliary material by prescription accurately claim fixed after, abundant mix homogeneously, last fully-automatic capsule filling machine fill hard capsule.
Embodiment 27
The preparation of saikoside granule (Sugarless type).
Get following weight portion meter component:
Embodiment 2 product 25g
Xylitol 200g
Sucrose 20g
Microcrystalline Cellulose 100g
Hypromellose 1g
Titanium dioxide 20g
Preparation method: it is fixed that main and auxiliary raw material is accurately claimed by prescription, adds 3% hydroxypropyl emthylcellulose aqueous solution, makes soft material, granulate with 30 mesh sieves, with 30 ℃ of aeration-dryings, with 80 orders and the screening of 10 mesh sieves, behind the granule of removal＜80 and＞10 mesh sieves, pack promptly with particles packing machine.
Embodiment 28
The preparation of saikoside granule (Sugarless type).
Get following weight portion meter component:
Embodiment 3 product 100g
Xylitol 20g
Sucrose 200g
Microcrystalline Cellulose 20g
Hypromellose 5g
Silica 1 g
Preparation method: it is fixed that main and auxiliary raw material is accurately claimed by prescription, adds 30% hydroxypropyl emthylcellulose aqueous solution, makes soft material, granulate with 10 mesh sieves, with 70 ℃ of aeration-dryings, with 80 orders and the screening of 10 mesh sieves, behind the granule of removal＜80 and＞10 mesh sieves, pack promptly with particles packing machine.
Embodiment 29
The preparation of saikoside granule (Sugarless type).
Get following weight portion meter component:
Embodiment 4 product 60g
Xylitol 110g
Sucrose 110g
Microcrystalline Cellulose 60g
Hypromellose 2.5g
Silica 1 0g
Preparation method: it is fixed that main and auxiliary raw material is accurately claimed by prescription, adds 15% hydroxypropyl emthylcellulose aqueous solution, makes soft material, granulate with 20 mesh sieves, with 50 ℃ of aeration-dryings, with 80 orders and the screening of 10 mesh sieves, behind the granule of removal＜80 and＞10 mesh sieves, pack promptly with particles packing machine.
Test example 1
This test example causes the inhibitory action test of mice ear for embodiment 1 product xylol.
Get 30 of healthy Kunming mouses, body weight 20-24g.Be divided into matched group, Radix Bupleuri oral liquid group, embodiment 1 group of products at random.Every group 10, male and female half and half, sub-cage rearing.With the conversion of people's conventional therapy dosage is the dosage of mice.The conversion formula is: the body surface area ratio of the body surface area ratio/known animal of tested animal metering=known animals administer dosage * tested animal on probation.Matched group is given and distilled water, successive administration 7 days, after last 1 administration 30 minutes, the two sides is smeared dimethylbenzene 0.03ml and is caused inflammation before and after every mice left side ear, animal is put to death in the cervical vertebra dislocation after 30 minutes, cut two ears along the auricle baseline, lay round auricle at same antimere respectively with 9mm diameter card punch, torsion balance is weighed, the left auricle of every Mus heavily deducts auris dextra sheet weight and is the swelling degree, calculates and respectively organizes the average and the standard deviation of swelling degree, and make t and check, the comparable group differences calculates swelling by following formula and suppresses percentage rate: suppression ratio=(the even swelling degree of the matched group-even swelling degree of administration the group)/average swelling degree of matched group * 100%.The results are shown in Table 1.
Table 1: xylol causes the inhibitory action (X ± SD) of mice ear
| Group | Mus number (only) | Ear swelling rate (%) | Suppression ratio (%) |
| Matched group | 10 | 13.06±2.23 | - |
| The Radix Bupleuri oral liquid group | 10 | 12.47±2.51 * | 16.7 |
| Embodiment 1 group of products | 10 | 10.82±2.58 *# | 32.2 |
Annotate: compare with matched group:
*P＜0.01;
Compare with the Radix Bupleuri oral liquid group: #P＜0.05
Embodiment 1 product and Radix Bupleuri oral liquid xylol cause mice ear all inhibitory action (P＜0.01); Embodiment 1 product is compared with Radix Bupleuri oral liquid, and xylol causes mice ear also variant (P＜0.05).Illustrate: the pharmacological action of embodiment 1 product is better than Radix Bupleuri oral liquid.
Test example 2
This test example is that compare the hot-plate analgesic test of embodiment 2 products.
Water temperature is constant in 55 ± 0.5 ℃, gets 30 of the qualified mices of preliminary election, divides 3 groups at random.Matched group, Radix Bupleuri oral liquid group, embodiment 2 group of products.Each group difference successive administration 7 days, 1h measures the pain threshold of each mice after the last administration.The results are shown in Table 2.
Table 2: xylol causes the inhibitory action (X ± SD) of mice ear
| Group | Mus number (only) | Pain threshold (s) | |
| Before the administration | After the administration | ||
| Matched group | 10 | 17.83±4.23 | 18.75±3.18 |
| The Radix Bupleuri oral liquid group | 10 | 17.47±4.73 | 23.38±4.52 * |
| Embodiment 2 group of products | 10 | 17.94±4.55 | 27.33±5.22 *3 |
Annotate: compare with matched group:
*P＜0.01;
Compare with the Radix Bupleuri oral liquid group: #P＜0.05
Embodiment 1 product and Radix Bupleuri oral liquid all can significantly increase the pain threshold (P＜0.01) of mice; Embodiment 2 products are compared with Radix Bupleuri oral liquid, and pain threshold improves also variant (P＜0.05).
Illustrate: the pharmacological action of embodiment 2 products is better than Radix Bupleuri oral liquid.
Above pharmacological evaluation proves that embodiment 2 products have better drug effect.
Other embodiment products have the drug effect effect identical with embodiment 1 or 2.
Claims (10)
1, a kind of Radix Bupleuri extract is characterized in that, described extract is extracted through alcoholic solution by bupleurum Chinese and obtains, and wherein contains the saikoside a of 20-30% weight portion, the saikoside d of 10-20% weight portion.
2, extract according to claim 1 is characterized in that, saikoside a and saikoside d sum account for the 40-50% weight portion of extract in the described extract.
3, extract according to claim 2 is characterized in that, in the described extract, the summation of each saikoside accounts for the 50-90% weight portion of extract.
4, any described preparation method of extract of claim 1-3 is characterized in that, said method comprising the steps of:
I. Radix Bupleuri is pulverized, the alcoholic solution that adds 6-10 times of Radix Bupleuri weight reflux, extract, 1-3 time in 75-85 ℃ of water-bath was extracted 1-3 hour at every turn, merge extractive liquid,, and at 35-50 ℃ of following concentrating under reduced pressure, must concentrated solution, make a living 2-4 times of weight of dose of concentrated liquid measure;
II. concentrated solution is passed through the D101 macroporous resin column, standing adsorption 2-3 hour, the distillation washing post with 8-12 times of resin column loading amount volume removed sugar then, and the 40-60% ethanol of reuse 1-2 times of resin column loading amount volume is washed the post removal of impurity;
III. use the alcoholic solution of 4-6 times of resin column loading amount volume to carry out eluting, collect eluent, by the decolouring of D280 decolorizing column, the decolouring back is at 35-50 ℃ of following concentrating under reduced pressure, and the specific gravity control of concentrated solution is drying to obtain at 1.05-1.20.
5, preparation method according to claim 4 is characterized in that, among the described step I, it is that Radix Bupleuri is crushed to the 10-20 order that Radix Bupleuri is pulverized.
6, preparation method according to claim 4 is characterized in that, the alcoholic solution among described step I and the III is the 60-80% ethanol water.
7, preparation method according to claim 6 is characterized in that, among the described step I, the alcoholic solution consumption is 8 times of Radix Bupleuri weight, and bath temperature is 80 ℃, and extraction time is 3 times, each 1 hour; Make a living 3 times of weight of dose of concentrated liquid measure.
8, preparation method according to claim 6 is characterized in that, among the described Step II I, the alcoholic solution consumption is 5 times of resin column loading amount volumes.
9, preparation method according to claim 4 is characterized in that, in the described Step II, the distilled water consumption is 10 times of resin column loading amount volumes, and washing the ethanol water concentration that the post removal of impurity uses is 50%.
10, the application of any described extract of claim 1-3 in preparation antiinflammatory, antiviral, antitumor, endocrine regulation and disease of immune system medicine; The dosage form of described medicine is preferably injection or solid orally ingestible; Described injection is preferably little liquid drugs injection, freeze-dried powder or intravenous fluid; Described solid orally ingestible is preferably conventional tablet, oral cavity disintegration tablet, dispersible tablet, slow releasing tablet, controlled release tablet, effervescent tablet, thin membrane coated tablet, hard capsule, slow releasing capsule, controlled release capsule, soft capsule, drop pill, granule, effervescent granule.
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| CNB2006100994987A CN100540012C (en) | 2005-07-25 | 2006-07-24 | A kind of Radix Bupleuri extract, its preparation method and application thereof |
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| CN200510085183.2 | 2005-07-25 | ||
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| CN101013110A (en) * | 2007-01-25 | 2007-08-08 | 北京华医神农医药科技有限公司 | Quality controlling method of Bupleurum injection |
| CN101946771A (en) * | 2010-09-26 | 2011-01-19 | 云南省农业科学院生物技术与种质资源研究所 | Application of Saikosaponin A to preparing pesticide for resisting tobacco mosaic virus (TMV) |
| CN101428049B (en) * | 2008-12-11 | 2011-08-31 | 江苏省中国科学院植物研究所 | Upper respiratory tract infection resistant medicament composition, preparation and uses thereof |
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| CN103098949A (en) * | 2012-11-13 | 2013-05-15 | 苏州谷力生物科技有限公司 | Preparation method of radix bupleuri flavor for tea |
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| CN101013110A (en) * | 2007-01-25 | 2007-08-08 | 北京华医神农医药科技有限公司 | Quality controlling method of Bupleurum injection |
| CN101428049B (en) * | 2008-12-11 | 2011-08-31 | 江苏省中国科学院植物研究所 | Upper respiratory tract infection resistant medicament composition, preparation and uses thereof |
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| US9060989B2 (en) | 2010-06-30 | 2015-06-23 | Industrial Technology Research Institute | Method for treating or relieving inflammatory bowel disease |
| US8597693B2 (en) | 2010-07-01 | 2013-12-03 | Industrial Technology Research Institute | Pharmaceutical composition with immunomodulating function |
| CN101946771B (en) * | 2010-09-26 | 2013-04-03 | 云南省农业科学院生物技术与种质资源研究所 | Application of Saikosaponin A to preparing pesticide for resisting tobacco mosaic virus (TMV) |
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| CN103098949A (en) * | 2012-11-13 | 2013-05-15 | 苏州谷力生物科技有限公司 | Preparation method of radix bupleuri flavor for tea |
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