CN101085190B - Pulse engendendering active component composition and its preparation - Google Patents

Pulse engendendering active component composition and its preparation Download PDF

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Publication number
CN101085190B
CN101085190B CN200610014219.2A CN200610014219A CN101085190B CN 101085190 B CN101085190 B CN 101085190B CN 200610014219 A CN200610014219 A CN 200610014219A CN 101085190 B CN101085190 B CN 101085190B
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ginseng
medical material
total
ethanol
fructus schisandrae
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CN101085190A (en
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杨悦武
叶正良
郑永锋
李旭
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Tianjin Tasly Zhijiao Pharmaceutical Co Ltd
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Tianjin Tasly Zhijiao Pharmaceutical Co Ltd
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Abstract

The invention belongs to medical preparation field, specifically discloses a sheng mai effective fraction composition and its preparation. The sheng mai effective fraction composition comprises mixed saponins extract of Panax ginseng and Ophiopogon japonicus and total lignanoid of Schisandra Chinesis. Inventive sheng mai effective fraction composition can be made into different kinds of dosage forms with any adjuvants such as injection, tablet, sustained release tablet, dripping pill, granule, powder injection, capsule and fine granule. The invention Chinese medicinal composition has easily accessible resource, easy industrialization; can be made into different kinds of dosage forms, provides Chinese traditional medicine with conveniece, efficiency and controlled quality, and bring benefit for patient; thereby generating giant social benefit.

Description

The preparation method of pulse engendendering active component composition and preparation thereof
Technical field
The invention belongs to pharmaceutical product, specifically, relate to pulse engendendering active component composition and preparation thereof.
background technology
Current existing formulation of ' Sheng Mai ' is to be all that raw material is made by Radix Ginseng Rubra, Radix Ophiopogonis and Fructus Schisandrae Chinensis, the party comes from the SHENGMAI YIN of Jin Dynasty Li Gao < < differentiation on endogenous > >, the clinical syndrome that is widely used in deficiency of both QI and YIN, all has good curative effect to acute stage, septic shock and other multiple critical illness such as the stable phase of patients with coronary heart disease, acute myocardial infarction, cardiogenic shock, arrhythmia.Also can be used as the paramedicines for the treatment of cancer, the untoward reaction causing for alleviating chemotherapy, radiotherapy.But there is extraction process imperfection in existing formulation of ' Sheng Mai ', extracts active ingredients is incomplete, control of product quality difficulty is large, low and the imperfection of preparation quality standard, the Tween class cosolvent that has for example used cardiovascular diseases medication to add in pulse restoring injection, drug level is low, and quantity is large, and transports, stores also all inconvenient.Therefore, provide the preparation of convenient effective pulse engendendering active component composition to have great importance.
summary of the invention
The object of the present invention is to provide a kind of quality controllable, pulse engendendering active component composition and preparation thereof that stability is high.
The present invention is implemented by following technical proposals.
Pulse engendendering active component composition of the present invention, is comprised of ginseng, dwarf lilyturf tuber mixing saponin extract and Fructus Schisandrae Chinensis total lignanoid.
Pulse engendendering active component composition of the present invention, is comprised of following component by weight percentage: ginseng, dwarf lilyturf tuber mixing saponin extract 40%~98%, Fructus Schisandrae Chinensis total lignanoid 60%~2%.
Pulse engendendering active component composition of the present invention, is preferably by weight percentage and is comprised of following component: ginseng, dwarf lilyturf tuber mixing saponin extract 70%~95%, Fructus Schisandrae Chinensis total lignanoid 30%~5%.
Pulse engendendering active component composition of the present invention, is more preferably comprised of following component by weight percentage: ginseng, dwarf lilyturf tuber mixing saponin extract 75%~93%, Fructus Schisandrae Chinensis total lignanoid 25%~7%.
Total Ginsenosides Content 20%~94% in above-mentioned ginseng, dwarf lilyturf tuber mixing saponin extract, Radix Ophiopogonis total saponins 5%~79%, Radix Ginseng total saponins and Radix Ophiopogonis total saponins sum 70%~99%, the best is 85%~99%; Total lignans content 50%~99% in Fructus Schisandrae Chinensis total lignanoid, the best is 70%~99%.
Ginseng, dwarf lilyturf tuber mixing saponin extract in pulse engendendering active component composition of the present invention can obtain by prior art, but need the refining standard that reaches Radix Ginseng total saponins and Radix Ophiopogonis total saponins sum 70%~99%, also can the specific method of the present invention prepare ginseng, dwarf lilyturf tuber mixing saponin extract.
The preparation of ginseng, dwarf lilyturf tuber mixing saponin extract: get by a certain percentage Radix Ginseng or Folium Ginseng medical material and Radix Ophiopogonis medical material, add water or 40~80% ethanol, regulator solution pH value is to alkalescence, heating or supersound extraction 2~4 times, merge extractive liquid,, filters, the macroporous type alkali anion exchange column of having handled well on filtrate, first with aqueous alkali, rinse, rear by pure water rinsing, flushing liquor discards; With 50~95% ethanol, carry out eluting again, collect eluent, eluent is concentrated into thick paste, dry, must mix the ginseng, dwarf lilyturf tuber mixing saponin extract that total saponin content is greater than 70%.In ginseng, dwarf lilyturf tuber mixing saponin extract, the mensuration of Radix Ginseng total saponins is referring to document (Anhui Chinese Medicine College journal, in August, 2003,22 (4): 51), the mensuration of Radix Ophiopogonis total saponins is referring to document (Chinese herbal medicine, in December, 2003,34 (12): 1090), ginseng, dwarf lilyturf tuber mixing saponin is both sums.
Fructus Schisandrae Chinensis total lignanoid in pulse engendendering active component composition of the present invention can obtain by prior art, but needs the refining standard that reaches total lignans content 50%~99%, also can the specific method of the present invention prepare Fructus Schisandrae Chinensis total lignanoid.
The preparation of Fructus Schisandrae Chinensis total lignanoid: get schisandra chinensis medicinal material, the sodium carbonate or the sodium bicarbonate that add 30~80% ethanol and 0.2~1.5% medical material amount, heating or supersound extraction 2~4 times, merge extractive liquid,, filters, filtrate decompression is concentrated into without after alcohol taste, be dissolved in water, on the macroporous adsorptive resins handled well, first with aqueous alkali, rinse, after use pure water rinsing, flushing liquor discards; With 50~95% ethanol, carry out eluting again, collect eluent, eluent is concentrated into thick paste, dry, obtains total lignans and be 50%~99% Fructus Schisandrae Chinensis total lignanoid.The mensuration of Fructus Schisandrae Chinensis total lignanoid is referring to document (northwest pharmaceutical journal, in October, 1999,14 (5): 197).
The preparation of above-mentioned Fructus Schisandrae Chinensis total lignanoid or be: get schisandra chinensis medicinal material, the sodium carbonate or the sodium bicarbonate that add 30~80% ethanol and 0.2~1.5% medical material amount, heating or supersound extraction 2~4 times, merge extractive liquid,, filters, filtrate decompression is concentrated into without after alcohol taste, be dissolved in water, on the macroporous adsorptive resins handled well, first with aqueous alkali, rinse, after use pure water rinsing, flushing liquor discards; With 50~95% ethanol, carry out eluting again, collect eluent; Eluent is crossed polyamide resin column, collects effluent, then 70~95% ethanol elutions, collects effluent, merges effluent, is concentrated into thick paste, dry, obtains total lignans and be 50%~99% Fructus Schisandrae Chinensis total lignanoid.The mensuration of Fructus Schisandrae Chinensis total lignanoid is referring to document (northwest pharmaceutical journal, in October, 1999,14 (5): 197).
Pulse engendendering active component composition of the present invention, the various dosage forms that can be mixed as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, glycine, HP-β-CD etc. with adjuvant on any or more than one pharmaceuticss, for example, can be made into injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule, microgranule.Preferred dosage form is injectable powder, drop pill, capsule.
The clinical diseases such as heart source property, septic shock, cardiomyopathy, coronary heart disease, the more remarkable treatment effect of being used for the treatment of of the present invention.Pharmacological evaluation shows: with existing formulation of ' Sheng Mai ' comparison, the Acute Myocardial Ischemia in Rats that pulse engendendering active component composition of the present invention and preparation thereof cause pituitrin has obvious antagonism (P < 0.01), non-specific antiinflammatory action is higher, cellular immunization and the humoral immune function of obvious enhancing body, obviously improve the tolerance of body to anoxia, and toxicity is little, without obvious irritative response.
Raw material sources of the present invention are easy to get, and are easy to industrialization; Can make as required various dosage forms, for clinical provide convenient, more effectively, the more controlled modern Chinese medicine of quality, for patient brings more interests, thereby produce huge social benefit.
The specific embodiment
With reference to the following example, will be easier to understand the present invention, providing embodiment is in order to illustrate the present invention, rather than in order to limit the scope of the invention.
The preparation of embodiment mono-ginseng, dwarf lilyturf tuber mixing saponin extract
Method 1:
In the ratio of 1: 0.9 weight portion take Folium Ginseng and Radix Ophiopogonis medical material, adding water boil extracts three times and controls acid-base value, be the Na2CO3 of 6 times of water yields and the 0.7% medical material amount of medical material amount for the first time, being the Na2CO3 of 4 times of water yields and the 0.3% medical material amount of medical material amount for the second time, is 4 times of water yields of medical material amount for the third time; Side circulated in countercurrent is extracted, and keeps respectively 1.5,1,1 hours after boiling; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D392 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2%NaOH solution of 2 times of resin bed volumes, and flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 70% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 80.1%, Radix Ophiopogonis total saponins content 6.6%, mixes total saponin content 86.7%).
Method 2:
In the ratio of 1: 2.2 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, adding water boil extracts three times and controls acid-base value, be the Na2CO3 of 5 times of water yields and the 0.7% medical material amount of medical material amount for the first time, being the Na2CO3 of 4 times of water yields and the 0.3% medical material amount of medical material amount for the second time, is 4 times of water yields of medical material amount for the third time; Side circulated in countercurrent is extracted, and keeps respectively 1.5,1,1 hours after boiling; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D380 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2%NaOH solution of 2 times of resin bed volumes, and flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 80% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 71.1%, Radix Ophiopogonis total saponins content 15.0%, mixes total saponin content 86.1%).
Method 3:
In the ratio of 1: 3.0 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, adding water boil extracts three times and controls acid-base value, be the NaHCO3 of 6 times of water yields and the 0.9% medical material amount of medical material amount for the first time, being the NaHCO3 of 4 times of water yields and the 0.5% medical material amount of medical material amount for the second time, is 4 times of water yields of medical material amount for the third time; Side circulated in countercurrent is extracted, and keeps respectively 1.5,1,1 hours after boiling; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type strong alkalinity anion D201 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2%NaOH solution of 2 times of resin bed volumes, and flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 65% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 66.7%, Radix Ophiopogonis total saponins content 19.1%, mixes total saponin content 85.8%).
Method 4:
In the ratio of 1: 1.4 weight portion take Folium Ginseng and Radix Ophiopogonis medical material, add water supersound extraction four times and control acid-base value, be the Na2CO3 of 5 times of water yields and the 0.7% medical material amount of medical material amount for the first time, being the Na2CO3 of 4 times of water yields and the 0.3% medical material amount of medical material amount for the second time, is for for the third time with four time 3 times of water yields of medical material amount; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D382 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2.5%NaOH solution of 1.5 times of resin bed volumes, and flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; 75% ethanol elution with 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 76.0%, Radix Ophiopogonis total saponins content 10.4%, mixes total saponin content 86.4%).
Method 5:
In the ratio of 1: 4.8 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, add water supersound extraction four times and control acid-base value, be the NaHCO3 of 5 times of water yields and the 0.9% medical material amount of medical material amount for the first time, being the NaHCO3 of 4 times of water yields and the 0.5% medical material amount of medical material amount for the second time, is for for the third time with four time 3 times of water yields of medical material amount; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type strong alkalinity anion D201 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2.5%NaOH solution of 1.5 times of resin bed volumes, and flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; 85% ethanol elution with 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 58.3%, Radix Ophiopogonis total saponins content 27.0%, mixes total saponin content 85.4%).
Method 6:
In the ratio of 1: 4.1 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, add water supersound extraction four times and control acid-base value, be the NaHCO3 of 5 times of water yields and the 0.9% medical material amount of medical material amount for the first time, being the NaHCO3 of 4 times of water yields and the 0.5% medical material amount of medical material amount for the second time, is for for the third time with four time 3 times of water yields of medical material amount; Medicinal liquid merging is chilled to room temperature, filters, and the macroporous type weakly-basic anion D371 exchange column (Chemical Plant of Nankai Univ.) of having handled well on medicinal liquid filtrate, rinses with the 2.5%NaOH solution of 1.5 times of resin bed volumes, and flushing liquor discards; 4 times of pure water rinsing again, aqueous rinse solution discards; 70% ethanol elution with 8 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 61.5%, Radix Ophiopogonis total saponins content 24.1%, mixes total saponin content 85.5%).
The preparation of embodiment bis-ginseng, dwarf lilyturf tuber mixing saponin extracts
Method 1:
In the ratio of 1: 6.9 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, add 50% alcohol reflux three times and control acid-base value, be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount for the first time, being the Na2CO3 of 4 times of 50% amount of alcohol and the 0.5% medical material amount of medical material amount for the second time, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract,, refluxes and starts rear maintenance respectively 1.5,1,1 hours; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous type weakly-basic anion D382 exchange column (Chemical Plant of Nankai Univ.) of having handled well on diluent, with the 2%NaOH solution of 2 times of resin bed volumes, rinse, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 70% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 51.2%, Radix Ophiopogonis total saponins content 33.8%, mixes total saponin content 84.9%).
Method 2:
In the ratio of 1: 2.2 weight portion take Folium Ginseng and Radix Ophiopogonis medical material, add 60% ethanol ultrasonic extraction three times and control acid-base value, be the Na2CO3 of 5 times of 50% amount of alcohol and the 1% medical material amount of medical material amount for the first time, being the Na2CO3 of 4 times of 60% amount of alcohol and the 0.5% medical material amount of medical material amount for the second time, is 4 times of 60% amount of alcohol of medical material amount for the third time; Medicinal liquid merging is chilled to room temperature, filter, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous type weakly-basic anion D392 exchange column (Chemical Plant of Nankai Univ.) of having handled well on diluent, with the 2%NaOH solution of 2 times of resin bed volumes, rinse, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 80% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 71.4%, Radix Ophiopogonis total saponins content 14.7%, mixes total saponin content 86.1%).
Method 3:
In the ratio of 1: 25.6 weight portion take Radix Ginseng Rubra and Radix Ophiopogonis medical material, add 65% alcohol reflux three times and control acid-base value, be the NaHCO3 of 5 times of 65% amount of alcohol and the 1.5% medical material amount of medical material amount for the first time, being the NaHCO3 of 4 times of 65% amount of alcohol and the 0.7% medical material amount of medical material amount for the second time, is 4 times of 50% amount of alcohol of medical material amount for the third time; Side circulated in countercurrent reflux, extract,, refluxes and starts rear maintenance respectively 1.5,1,1 hours; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous type weakly-basic anion D380 exchange column (Chemical Plant of Nankai Univ.) of having handled well on diluent, with the 2%NaOH solution of 2 times of resin bed volumes, rinse, flushing liquor discards; 3 times of pure water rinsing again, aqueous rinse solution discards; 75% ethanol elution with 7 times of resin bed volumes, collect eluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain ginseng, dwarf lilyturf tuber mixing saponin extract (total Ginsenosides Content 24.2%, Radix Ophiopogonis total saponins content 59.2%, mixes total saponin content 83.4%).
The preparation of embodiment tri-Fructus Schisandrae Chinensis total lignanoids
Method 1:
Get schisandra chinensis medicinal material, add 50% alcohol reflux three times and control acid-base value, being 50% ethanol of 5 times of medical material amounts and the Na2CO3 of 1% medical material amount for the first time, is 50% ethanol of 4 times of medical material amounts and the Na2CO3 of 0.5% medical material amount for the second time, is 50% ethanol of 4 times of medical material amounts for the third time; Side circulated in countercurrent is extracted, and refluxes and starts rear maintenance respectively 1.5,1,1 hours; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous adsorptive resins D101 having handled well on diluent, with the 0.4%NaOH of 2 times of resin bed volumes, rinse, flushing liquor discards; 2 times of pure water rinsing again, flushing liquor discards; Then 70% ethanol elution of 5 times of resin bed volumes, collects eluent, is concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtains Fructus Schisandrae Chinensis total lignanoid (total lignans content 67.3%).
Method 2:
Get schisandra chinensis medicinal material, add 60% ethanol ultrasonic extraction four times and control acid-base value, be 50% ethanol of 5 times of medical material amounts and the NaHCO3 of 1.5% medical material amount for the first time, being 50% ethanol of 4 times of medical material amounts and the NaHCO3 of 1% medical material amount for the second time, is for for the third time with four time 50% ethanol of 4 times of medical material amounts; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous adsorptive resins D201 having handled well on diluent, with the 0.4%NaOH of 2 times of resin bed volumes, rinse, flushing liquor discards; 2 times of pure water rinsing again, flushing liquor discards; Then 65% ethanol elution of 6 times of resin bed volumes, collects eluent, is concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtains Fructus Schisandrae Chinensis total lignanoid (total lignans content 71.1%).
Method 3:
Get schisandra chinensis medicinal material, add 55% alcohol reflux three times and control acid-base value, being 50% ethanol of 5 times of medical material amounts and the Na2CO3 of 1% medical material amount for the first time, is 50% ethanol of 4 times of medical material amounts and the Na2CO3 of 0.5% medical material amount for the second time, is 50% ethanol of 4 times of medical material amounts for the third time; Side circulated in countercurrent is extracted, and refluxes and starts rear maintenance respectively 1.5,1,1 hours; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous adsorptive resins D101 having handled well on diluent, with the 0.4%NaOH of 2 times of resin bed volumes, rinse, flushing liquor discards; 2 times of pure water rinsing again, flushing liquor discards; Then 65% ethanol elution of 5 times of resin bed volumes, collects eluent.Eluent is crossed polyamide resin column, collect effluent, 2 times of 85% ethanol elution again, collect effluent, merge effluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain Fructus Schisandrae Chinensis total lignanoid (total lignans content 75.4%).
Method 4:
Get schisandra chinensis medicinal material, add 60% ethanol ultrasonic extraction four times and control acid-base value, be 50% ethanol of 5 times of medical material amounts and the NaHCO3 of 1.5% medical material amount for the first time, being 50% ethanol of 4 times of medical material amounts and the NaHCO3 of 1% medical material amount for the second time, is for for the third time with four time 50% ethanol of 4 times of medical material amounts; Medical filtration merging filtrate, at 70 ℃ of filtrates, be evaporated to without after alcohol taste, it is 1: 1.5 that concentrated solution is diluted with water to medical material medicinal liquid ratio, the macroporous adsorptive resins D201 having handled well on diluent, with the 0.4%NaOH of 2 times of resin bed volumes, rinse, flushing liquor discards; 2 times of pure water rinsing again, flushing liquor discards; Then 70% ethanol elution of 6 times of resin bed volumes, collects eluent.Eluent is crossed polyamide resin column, collect effluent, 2 times of 80% ethanol elution again, collect effluent, merge effluent, be concentrated into thick paste (at 50 ℃, relative density is 1.28~1.33), dry with dynamic belt drying equipment, obtain Fructus Schisandrae Chinensis total lignanoid (total lignans content 72.7%).
Embodiment tetra-pulse engendendering active component compositions
The ginseng, dwarf lilyturf tuber mixing saponin extract of embodiment mono-or the ginseng, dwarf lilyturf tuber mixing saponin extract of embodiment bis-of getting arbitrary proportion, evenly mix with the Fructus Schisandrae Chinensis total lignanoid of embodiment tri-, obtains pulse engendendering active component composition.
Embodiment five pulse engendendering active component injectable powder
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 1) 8.7g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 1) 0.3g, mix homogeneously, adds 5 times of waters for injection, stirs after lower heating makes to dissolve first coarse filtration while hot, filtrate for later use; HP-β-CD 225g, adds appropriate water for injection, and heating filters after making to dissolve while hot; Filtrate is mixed with medicinal liquid, stirs after 60 minutes at 60 ℃, stops heating; Add mannitol 115g, be stirred to dissolve, adjust pH to 6.5~7.0, inject water to cumulative volume, continue to stir after 10 minutes, are chilled to room temperature, aseptic filtration.Filtrate fill is in cillin bottle, and lyophilization, tamponade, adds a cover, and obtains.
Embodiment six pulse engendendering active component injectable powder
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 2) 8.2g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 2) 0.8g, mix homogeneously, add each 115g of lecithin and mannitol, appropriate water for injection, after heating makes to dissolve, adjust pH to 6.5~7.0, inject water to cumulative volume, stir 10 minutes, be chilled to after room temperature aseptic filtration; Filtrate fill is in cillin bottle, and lyophilization, tamponade, adds a cover, and obtains.
Embodiment seven pulse engendendering active component injectable powder
Get Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 3) 3.0g, add appropriate dissolve with ethanol and filter filtrate for later use; HP-β-CD 225g, adds appropriate water for injection, after heating makes to dissolve, filters while hot, adds Fructus Schisandrae Chinensis total lignanoid filtrate, stirs after 60 minutes at 60 ℃, boils off ethanol, filters, standby.Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 3) 6.0g, 115g mixes with mannitol, adds 5 times of waters for injection, stir lower heating and make after dissolving, first coarse filtration, mixes with Fructus Schisandrae Chinensis total lignanoid medicinal liquid while hot, adjust pH to 6.5~7.0, inject water to cumulative volume, stir after 10 minutes, be chilled to room temperature, aseptic filtration, fill in cillin bottle, lyophilization, tamponade, add a cover, obtain.
Embodiment eight pulse engendendering active component injections
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 4) 7.1g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 4) 1.9g, mix homogeneously, adds 5 times of waters for injection, stirs after lower heating makes to dissolve first coarse filtration while hot, filtrate for later use; HP-β-CD 225g, adds appropriate water for injection, and heating filters after making to dissolve while hot; Filtrate is mixed with medicinal liquid, stirs after 60 minutes at 60 ℃, stops heating; Add mannitol 115g, be stirred to dissolve, adjust pH to 6.5~7.0, inject water to cumulative volume, continue to stir after 10 minutes, are chilled to room temperature, and aseptic filtration, obtains injection.
Embodiment nine pulse engendendering active component capsules
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 5) 8.5g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 1) 0.5g, mix homogeneously with 40g microcrystalline Cellulose, add 3% polyvidone alcoholic solution soft material processed, cross 18 mesh sieve granule processed, 600 ℃ are dried 30~45 minutes, granulate, add 4g Pulvis Talci, mix, fill in capsule, obtain.
Embodiment ten pulse engendendering active component tablets
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment mono-method 6) 7.5g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 2) 1.5g, mix homogeneously with 40g microcrystalline Cellulose, add 3% polyvidone alcoholic solution soft material processed, cross 18 mesh sieve granule processed, 600 ℃ are dried 30~45 minutes, granulate, add 4g Pulvis Talci, mix, mix, tabletting, obtains.
Embodiment 11 pulse engendendering active component granules
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment bis-methods 1) 8.5g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 3) 0.5g, mix homogeneously with 40g microcrystalline Cellulose, add 3% polyvidone alcoholic solution soft material processed, cross 18 mesh sieve granule processed, 600 ℃ are dried 30~45 minutes, granulate, add 4g Pulvis Talci, mix, granulate, pack, obtains.
Embodiment 12 pulse engendendering active component drop pills
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment bis-methods 2) 3.9g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 4) 5.1g, mix homogeneously with 700g PEG-4000, melting, splash in cryogenic liquid paraffin, select ball, except liquid paraffin, obtain.
Embodiment 13 pulse engendendering active component drop pills
Get ginseng, dwarf lilyturf tuber mixing saponin extract (embodiment bis-methods 3) 7.2g, Fructus Schisandrae Chinensis total lignanoid (embodiment tri-methods 1) 1.8g, mix homogeneously with 250g PEG-4000 and 450g PEG-4000, melting, splash in low temperature methyl-silicone oil, select ball, except methyl-silicone oil, obtain.

Claims (3)

1. the preparation method of a pulse-promoting powder injection, injectable powder is comprised of ginseng, dwarf lilyturf tuber mixing saponin extract and Fructus Schisandrae Chinensis total lignanoid, and its percentage by weight is: ginseng, dwarf lilyturf tuber mixing saponin extract 43.3%~96.7%, Fructus Schisandrae Chinensis total lignanoid 56.7%~3.3%; In wherein said ginseng, dwarf lilyturf tuber mixing saponin extract, total Ginsenosides Content is 24.2%~80.1%, Radix Ophiopogonis total saponins content is 6.6%~59.2%, Radix Ginseng total saponins and Radix Ophiopogonis total saponins sum are 83.4%~86.7%, and in Fructus Schisandrae Chinensis total lignanoid, total lignans content is 67.3%~75.4%;
Described ginseng, dwarf lilyturf tuber mixing saponin extract is to be prepared from by following methods: by 1: 0.9~25.6 get Radix Ginseng or Folium Ginseng medical material and Radix Ophiopogonis medical material, add water or 50~65% ethanol, regulator solution pH value is to alkalescence, heating or supersound extraction 2~4 times, merge extractive liquid,, filters, the macroporous type alkali anion exchange column of having handled well on filtrate, first with aqueous alkali, rinse, rear by pure water rinsing, flushing liquor discards; With 65~85% ethanol, carry out eluting again, collect eluent, eluent is concentrated into thick paste, dry, obtains;
Described Fructus Schisandrae Chinensis total lignanoid is to be prepared from by following methods: get schisandra chinensis medicinal material, the sodium carbonate or the sodium bicarbonate that add 50~60% ethanol and 1.5~2.5% medical material amounts, heating or supersound extraction 3~4 times, merge extractive liquid,, filters, filtrate decompression is concentrated into without after alcohol taste, be dissolved in water, on the macroporous adsorptive resins handled well, first with aqueous alkali, rinse, after use pure water rinsing, flushing liquor discards; With 65~70% ethanol, carry out eluting again, collect eluent, eluent is concentrated into thick paste, dry, obtains;
Get ginseng, dwarf lilyturf tuber mixing saponin extract and Fructus Schisandrae Chinensis total lignanoid that said extracted obtains, mix homogeneously, add lecithin and mannitol and appropriate water for injection, after heating makes to dissolve, adjust pH to 6.5~7.0, inject water to specified volume, stir, cold putting, filters, filtrate lyophilization, obtains;
Or get ginseng, dwarf lilyturf tuber mixing saponin extract and Fructus Schisandrae Chinensis total lignanoid that said extracted obtains, mix homogeneously, adds water for injection, stir lower heating and make, after dissolving, to filter while hot, filtrate and HP-β-CD aqueous solution, stir; Add mannitol again, be stirred to dissolve, adjust pH to 6.5~7.0, inject water to specified volume, stir, and cold putting, filters, and filtrate lyophilization, obtains.
2. preparation method according to claim 1, it is characterized in that, described macroporous type alkali anion exchange column is macroporous type weakly-basic anion D392 exchange column, macroporous type weakly-basic anion D380 exchange column, macroporous type weakly-basic anion D382 exchange column, macroporous type weakly-basic anion D371 exchange column or macroporous type strong alkalinity anion D201 exchange column.
3. preparation method according to claim 1, is characterized in that, described Fructus Schisandrae Chinensis total lignanoid is to be prepared from by following methods: get schisandra chinensis medicinal material, the sodium carbonate or the sodium bicarbonate that add 55~60% ethanol and 1.5~2.5% medical material amounts, heating or supersound extraction 3~4 times, merge extractive liquid,, filters, filtrate decompression is concentrated into without after alcohol taste, be dissolved in water, on the macroporous adsorptive resins handled well, first with aqueous alkali, rinse, after use pure water rinsing, flushing liquor discards; With 65~70% ethanol, carry out eluting again, collect eluent; Eluent is crossed polyamide resin column, collects effluent, then 80~85% ethanol elutions, collects effluent, merges effluent, is concentrated into thick paste, dry, obtains.
CN200610014219.2A 2006-06-08 2006-06-08 Pulse engendendering active component composition and its preparation Expired - Fee Related CN101085190B (en)

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CN101745012B (en) * 2008-12-05 2012-09-19 天津天士力之骄药业有限公司 Method for extracting ginseng, dwarf lilyturf tuber and schisandra chinensis and preparation thereof
CN101745014B (en) * 2008-12-05 2013-03-13 天津天士力之骄药业有限公司 Extraction method for ginseng, ophiopogon root and schisandra chinensis and preparation thereof
CN101745013B (en) * 2008-12-05 2012-09-19 天津天士力之骄药业有限公司 Extraction method for ginseng, ophiopogon root and schisandra chinensis and preparation thereof
CN101745001B (en) * 2008-12-05 2012-09-19 天津天士力之骄药业有限公司 Extraction method of ophiopogon root, ginseng and shiandra and preparation thereof
CN110279770B (en) * 2019-06-28 2021-08-20 神威药业集团有限公司 Extraction of schisandra chinensis medicinal component, formula granule and preparation method of formula granule

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