CN102652799A - Method for refining water extract of traditional Chinese medicine (TCM) composition - Google Patents
Method for refining water extract of traditional Chinese medicine (TCM) composition Download PDFInfo
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Abstract
The invention discloses a method for refining water extract of a traditional Chinese medicine (TCM) composition. The TCM composition is composed of TCMs such as ginseng, radix ophiopogonis, fructus corni, salvia miltiorrhiza, fried spina date seeds, parasitic loranthus, red paeony root, ground beetle and rhizoma nardostachyos and can effectively treat premature ventricular contraction of coronary heart diseases. The method has the following beneficial effects: an inorganic ceramic membrane is adopted for filtration to refine the extract of the TCM composition; the active ingredients have high transfer rate; the extract can be industrially produced; the material liquid is simple to process; and the inorganic ceramic membrane is convenient to wash and can be regenerated.
Description
Technical field
The present invention relates to a kind of process for purification of traditional Chinese medicine composition water extract, particularly, relate to a kind of filterable process for purification of inorganic ceramic film of traditional Chinese medicine composition water extract.
Background technology
The main purpose of Chinese medicine preparation production technology is active constituent-enriched, removes invalid impurity.The refining many of Chinese medicine are the ultimate principle removing impurities with polarity difference between component (solvent deposition or extraction, adsorbing separation etc.); All there are some problems in they; Concentrated repeatedly or commentaries on classics long like the production cycle, medicinal liquid is dissolved and can be made loss of effective components or receive heat damage, causes drug effect reduction etc.Inorganic Ceramic Membranes is based on the screening principle, the particle of 0.05 ~ 10 μ m and some macromole impurity in the separable solution.Chinese medicine separates the use inorganic ceramic film and is mostly Al
2O
3Ceramic membrane, aperture are between the 30-800 nanometer, and it has, and chemical property is stable, high temperature resistant, pore-size distribution is narrow, the mechanical strength advantages of higher.For adopting inorganic ceramic membrane filtration working condition major influence factors to be: inorganic ceramic membrane aperture, operating pressure difference, water extract temperature and film flow velocity; For traditional Chinese medicine composition water extract of the present invention, membrane permeation flux, solid content clearance, the peoniflorin rate of transform are to need to investigate important indicator.
CN03143211.5 discloses a kind of Chinese medicine composition of treating Coronary heart disease ventricular early throb, and its composition comprises 75-300 parts of Radix Ginseng 45-180 part, Radix Ophiopogonis 50-200 parts, Fructus Corni 125-450 part, Radix Salviae Miltiorrhizae 125-450 part, Semen Ziziphi Spinosae (parched) 95-400 part, Herba Taxilli 95-400 part, Radix Paeoniae Rubra 45-200 part, Eupolyphaga Seu Steleophaga 35-150 part, Radix Et Rhizoma Nardostachyos 45-200 part, Rhizoma Coptidis 25-90 part, Fructus Schisandrae Chinensis 35-150 part, Os Draconis.Pharmacological testing research shows that this Chinese medicine composition is to CaCl
2The induced mice arrhythmia has obvious preventive effect, shows as incidence of arrhythmia and obviously reduces, and obviously reduces the rat ventricular persistent period due to the aconitine.
The present invention is the improvement invention of on No. 03143211.5 basis, carrying out, and the prescription and the preparation technology of this Chinese medicine composition put down in writing in this patent application, and the water extract among this preparation technology adopts common filtering technology remove impurity and active constituent-enriched.
Summary of the invention
The present invention provides a kind of process for purification of traditional Chinese medicine composition water extract, and this Chinese medicine composition is processed by following bulk drugs:
Radix Ginseng 45-180 part, Radix Ophiopogonis 50-200 part, Fructus Corni 125-450 part, Radix Salviae Miltiorrhizae 125-450 part, Semen Ziziphi Spinosae (parched) 95-400 part, Herba Taxilli 95-400 part, Radix Paeoniae Rubra 45-200 part, Eupolyphaga Seu Steleophaga 35-150 part, Radix Et Rhizoma Nardostachyos 45-200 part, Rhizoma Coptidis 25-90 part, Fructus Schisandrae Sphenantherae 35-150 part, Os Draconis 75-300 part.
The weight ratio of crude drug is preferably in the Chinese medicine composition of the present invention:
89 parts of Radix Ginsengs, 112 parts of Radix Ophiopogonis, 224 parts of Fructus Corni, 224 parts of Radix Salviae Miltiorrhizaes, 186 parts of Semen Ziziphi Spinosae (parched)s, 186 parts of Herba Taxillis, 89 parts of Radix Paeoniae Rubra, 75 parts of Eupolyphaga Seu Steleophagas, 89 parts of Radix Et Rhizoma Nardostachyos, 45 parts of Rhizoma Coptidis, 67 parts of Fructus Schisandrae Sphenantheraes, 149 parts of Os Draconis.
The weight ratio of crude drug also is preferably in the Chinese medicine composition of the present invention:
45 parts of Radix Ginsengs, 112 parts of Radix Ophiopogonis, 224 parts of Fructus Corni, 225 parts of Radix Salviae Miltiorrhizaes, 186 parts of Semen Ziziphi Spinosae (parched)s, 186 parts of Herba Taxillis, 89 parts of Radix Paeoniae Rubra, 45 parts of Radix Et Rhizoma Nardostachyos, 35 parts of Eupolyphaga Seu Steleophagas, 45 parts of Rhizoma Coptidis, 67 parts of Fructus Schisandrae Sphenantheraes, 149 parts of Os Draconis.
The weight ratio of crude drug also is preferably in the Chinese medicine composition of the present invention:
278 parts of 147 parts of Os Draconis of Radix Ginseng 85 parts of Fructus Schisandrae Sphenantheraes of 188 portions of Rhizoma Coptidis of 98 parts of Radix Et Rhizoma Nardostachyos of 188 parts of Eupolyphaga Seu Steleophagas of 396 parts of Radix Paeoniae Rubra of 395 parts of Herba Taxillis of 440 parts of Semen Ziziphi Spinosae (parched)s of 421 parts of Radix Salviae Miltiorrhizaes of 192 parts of Fructus Corni, 175 parts of Radix Ophiopogonis.
The weight ratio of crude drug also is preferably in the Chinese medicine composition of the present invention:
90 parts of Radix Ginsengs, 135 parts of Radix Ophiopogonis, 270 parts of Fructus Corni, 200 parts of Radix Salviae Miltiorrhizaes, 150 parts of Semen Ziziphi Spinosae (parched)s, 150 parts of Herba Taxillis, 100 parts of Radix Paeoniae Rubra, 100 parts of Eupolyphaga Seu Steleophagas, 95 parts of Radix Et Rhizoma Nardostachyos, 60 parts of Rhizoma Coptidis, 75 parts of Fructus Schisandrae Sphenantheraes, 150 parts of Os Draconis.
Chinese medicine composition according to the invention is with traditional Chinese medical science supplementing QI and nourishing YIN, promoting blood circulation to remove obstruction in the collateral, and clearing away heart-fire for tranquillization is theoretical, reaches the therapeutic purposes of recovering the heart normal cardiac rhythm through promoting blood circulation, the gas that nourishes heart.
The present invention uses said Chinese medicine can be had the Chinese medicine of same or similar effect fruit to replace, and these medical materials all can be concocted according to " national Chinese medicine processing standard " or " Chinese medicine voluminous dictionary ".
The present invention uses the active component of said Chinese medicine composition and is processed by following steps:
A) people participates in 70% alcohol reflux three times, and merge extractive liquid, filters, and concentrates oven dry, the fine powder that is ground into;
B) Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos add 70% alcohol reflux 3 times jointly, and merge extractive liquid, filters spissated extractum;
C) fine powder that is broken into of Eupolyph aga sinesis Walker;
D) Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water 2 times, merge extractive liquid,, refining, spissated extractum;
E) with step b) and d) merging of gained extractum, the fine drug powder of adding step c) gained, oven dry is ground into fine powder, adds step a) gained fine drug powder, and mixing promptly gets this Chinese medicine composition active component;
The object of the present invention is to provide a kind of process for purification of this traditional Chinese medicine composition water extract, i.e. the process for purification of above-mentioned steps (d) gained water extract, this method adopts inorganic ceramic film to filter this traditional Chinese medicine composition water extract is made with extra care.
This traditional Chinese medicine composition water extract of experiment confirm adopts inorganic ceramic film to filter, and under industrial generic condition, can effectively remove impurity, realizes the enrichment of effective ingredient.
The preferred working condition of process for purification of the present invention is: the inorganic ceramic membrane aperture is 50-200nm, and operation pressure reduction is 0.15-0.22Mpa.
Preferred working condition is: the inorganic ceramic membrane aperture is 100nm, and operation pressure reduction is 0.2Mpa.
Process for purification of the present invention need not heating, can realize under the room temperature that membrane flux can reach 600-1800ml/min, can satisfy industry and produce needs fast.
Process for purification of the present invention adopts the inorganic ceramic membrane filtration once can realize the enrichment of effective ingredient; When being preferably extracting solution residue original volume 10%, add water, continue to be filtered to extracting solution residue original volume 10% with volume; Can also add water once more, continue to be filtered to extracting solution residue original volume 10% with volume; Repeatedly remaining extracting solution is washed, help the enrichment of effective ingredient; But cyclic washing can increase the operating time and increase production cost.
Process for purification of the present invention has only played the enrichment of effective ingredient to the Chinese medicine composition among the present invention, whether the water extract that comprises identical flavour of a drug in other Chinese medicine compositions is played identical effect, and the present invention does not confirm.
In the actual production; The membrane permeation flux can constantly reduce; Thereby film pollutes mainly because which contaminant particles is held back in film absorption forms one deck pollutant on the film surface and cause in the system; Promptly form the surface deposition layer, and this resistance is one of the microfiltration performance of controlling diaphragm and main resistance of pollution condition.This regularly cleans film with regard to needs, to prolong the life-span of film, reduces production costs, and improves product yield.The method that native system adopts strong acid, highly basic alternately to clean; Stop the back in filtration and equipment is cleaned, wash secondary with deionized water earlier during cleaning, reuse deionized water preparation 2.0%NaOH cleans film at once; And add the thermal control temperature and be no more than 85 ℃; Clean after 40 minutes, with deionized water rinsing twice, reuse 1.0%HNO
3Film is cleaned, and the control temperature is no more than 55 ℃, cleans after 30 minutes acid solution to be drained, and with deionized water rinsing twice, equipment is washed into neutrality, and actual measurement shows that membrane flux obtains fine recovery after cleaning.
Process for purification of the present invention, the application in preparation medicine process also is a free-revving engine of the present invention.
The inventor utilizes ceramic membrane microfiltration technology; Composition water extract with embodiment 1; Traditional Chinese medicine composition water extract of the present invention is carried out filtering and impurity removing research; With membrane flux, water extract paste-forming rate and effective ingredient and finger printing is index, has compared the suitability of 3 kinds of different apertures ceramic membranes to traditional Chinese medicine composition water extract of the present invention remove impurity, filters out best membrane aperture and technological parameter; Result of the test proves that ceramic membrane microfiltration technology can effectively be improved the effect of traditional Chinese medicine composition water extract of the present invention remove impurity.
1 instrument and reagent
1.1 instrument
The Ceramic Composite film device, model SJM-FHM-05 (the outstanding film of Hefei generation Science and Technology Ltd. provides), filter area 0.5m
2Waters 2695-2998 high performance liquid chromatograph; The DAD detector; The Empower work station.METTLER TOLEDO AG135 type electronic balance.Electric heating constant temperature air dry oven DHG-9053A (going up the grand Science and Technology Ltd. of Nereid).
1.2 reagent and reference substance peoniflorin reference substance (lot number: 110736-200934) purchase in Nat'l Pharmaceutical & Biological Products Control Institute; Methanol (chromatographically pure); Acetonitrile (chromatographically pure); Other reagent is analytical pure.
Medical materials such as medical material Radix Ophiopogonis, Radix Paeoniae Rubra, Herba Taxilli are purchased in Anguo medical material market,, meet all that " relevant of Chinese pharmacopoeia 2010 editions (I portions) is regulation down through the check of quality inspection section of our company.
2 test methods
Water extract preparation takes by weighing by recipe quantity and Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis adds 9 times of water gagings and decoct 2 times, each 2 h, and merging filtrate behind the strainer filtering promptly gets.
The filtration test flow process is got an amount of medicinal liquid, adds ceramic membrane device feeding cylinder, and start continuous filtration is every at a distance from parameters such as 5min recording film flux, inlet hydraulics.
Paste-forming rate is measured and to be got above-mentioned water extract and each 50ml of inorganic ceramic film filtrate to the constant weight evaporating dish, and water-bath volatilizes, and 105 ℃ of oven dry 3h take out to put and cool off 0.5h in the exsiccator, weigh, and calculate paste-forming rate.
Paeoniflorin content assay method peoniflorin is by " the high effective liquid chromatography for measuring that 2010 editions I portions of Chinese pharmacopoeia record; With octadecylsilane key and silica gel is filler, is mobile phase with acetonitrile-0.1% phosphate aqueous solution (14:86), and the detection wavelength is 230nm; Flow velocity: 1ml/min; Column temperature: 30 ℃, sample size: 10 μ l, number of theoretical plate calculate by the peoniflorin peak should be not less than 3000.
Chromatogram finger print measuring method is that the filler chromatographic condition is with octadecylsilane key and silica gel:
Mobile phase: A=0.18% glacial acetic acid-methanol, B=0.3% glacial acetic acid-water, the detection wavelength is 248nm, flow velocity: 1ml/min, column temperature: 30 ℃, sample size: 10 μ l.Eluent gradient is seen table 1.
Table 1 eluent gradient
| Time (min) | 0 | 10 | 44 | 60 | 65 |
| A (%) | 5 | 16 | 36 | 42 | 60 |
| B (%) | 95 | 84 | 64 | 58 | 40 |
3 result of the tests
3.1 membrane aperture to influencing of membrane flux and cutoff performance traditional Chinese medicine composition water extract of the present invention 20 ℃ of temperature; Under inlet hydraulic 0.15 ~ 0.22MP condition, via hole diameter is 50nm respectively, 100nm; The ceramic membrane of 200nm is handled; With the membrane flux and the peoniflorin rate of transform is index, confirms to be suitable for the film model, and investigates the suitability of ceramic membrane to this system.The result sees table 2.
The rate of transform (%)=(penetrating fluid volume or component content ÷ stock solution volume or component content) * 100%
Solid content clearance (%)=(original liquid total solid-filtrate total solid)/original liquid total solid * 100%
Table 2 membrane aperture is to the influence of permeance property
| The aperture | Membrane flux (ml/min) | Solid content clearance (%) | The peoniflorin rate of transform (%) |
| 50nm | 888 | 36.24% | 86.46% |
| 100nm | 1620 | 37.36% | 95.53% |
| 200nm | 1184 | 41.81% | 84.54% |
Table 2 influences permeance property for membrane aperture; From table, can find out that the peoniflorin rate of transform of 100 nm films is all apparently higher than other two kinds, and membrane flux is moderate; Solid content clearance difference is little; Therefore, for traditional Chinese medicine composition water extract of the present invention, can be preferably and adopt 100 nm membrane aperture inorganic ceramic membrane filtrations.
3.2 filtration time writes down the membrane flux of ceramic membrane when different time of every kind of specification respectively to the influence of membrane flux; Observe membrane flux attenuation in time; With the filtration time is abscissa; Membrane flux is a vertical coordinate, draws the variation relation curve chart of membrane flux with filtration time, and the result sees Fig. 1.Find out that from Fig. 1 along with the increase of filtration time, the membrane flux of 3 kinds of aperture ceramic membranes is all in continuous reduction, in filtering preceding 5 min of beginning, the speed of The decline of membrane flux is bigger, and the speed of The decline of membrane flux is slower subsequently; This mainly is because before beginning to filter in the 5min; Form sedimentary deposit and membrane aperture obstruction on the film surface, and cause filtration resistance sharply to increase, the speed of The decline of membrane flux is bigger; Along with the obstruction of film surface deposition layer and film tends towards stability, it is slow that the speed of The decline of membrane flux also is tending towards.
3.3 membrane aperture has been measured content of paeoniflorin in the medicinal liquid of microfiltration front and back respectively to the inventor that influences of water extract character and active constituent content.The result sees table 3.
Effective ingredient relatively before and after table 3 microfiltration
Can know by table 3; Traditional Chinese medicine composition water extract of the present invention is behind 3 kinds of different apertures ceramic membrane filters; Medicinal liquid is all than obviously transparent before filtering, clarification; Paste-forming rate also descends to some extent, but behind the 100nm ceramic membrane filter in the medicinal liquid rate of transform of peoniflorin can reach more than 95%, the loss of filter process peoniflorin is minimum.
3.4 membrane aperture compares the chromatographic fingerprinting that filters front and back water extract the influence of chromatographic fingerprinting, investigates the influence of different membrane aperture to traditional Chinese medicine composition water extract chromatographic fingerprinting of the present invention, the result sees Fig. 2, Fig. 3, Fig. 4 respectively.Can find out that from above-mentioned several figure traditional Chinese medicine composition water extract of the present invention does not all have significant change at the chromatographic fingerprinting before and after 3 kinds of ceramic membrane remove impurity.
4 conclusions
It is feasible that the experiment proof adopts inorganic ceramic membrane microfiltration technology that traditional Chinese medicine composition water extract of the present invention is carried out impurity removal process; With respect to strainer filtering, medicinal liquid clarity is good behind the inorganic ceramic membrane filtration, and Impurity removal is more thorough; And feed liquid is handled simple, and the film cleaning and regeneration is all more convenient.Production cycle shortens, and reduces manpower consumption, reduces production costs.
Description of drawings
Fig. 1 membrane flux is with the variation relation curve chart of filtration time;
Finger printing compares A before and after the remove impurity of Fig. 2 50nm ceramic membrane: water extract stock solution; B: ceramic membrane micro-filtrate;
Finger printing compares A before and after the remove impurity of Fig. 3 100nm ceramic membrane: water extract stock solution; B: ceramic membrane micro-filtrate;
Finger printing compares A before and after the remove impurity of Fig. 4 200nm ceramic membrane: water extract stock solution; B: ceramic membrane micro-filtrate;
The specific embodiment
Following embodiment is used to illustrate process for purification of the present invention, but it can not constitute any restriction to scope of the present invention.
Embodiment 1:
The crude drug prescription does:
Radix Ginseng 89g 112g Radix Ophiopogonis Fructus Corni 224g Radix Salviae Miltiorrhizae 224g
Semen Ziziphi Spinosae (parched) 186g Herba Taxilli 186g Radix Paeoniae Rubra 89g Eupolyphaga Seu Steleophaga 75g
Radix Et Rhizoma Nardostachyos 89g Rhizoma Coptidis 45g Fructus Schisandrae Sphenantherae 67g Os Draconis 149g
Process for purification does:
(a) in the above-mentioned prescription, Radix Ginseng is with 70% alcohol reflux three times, and 3 hours for the first time, each 2 hours later on, merge extractive liquid, filtered, and reclaims ethanol, concentrates, and oven dry is ground into fine powder, and is subsequent use;
(b) in the above-mentioned prescription, Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos are with 70% alcohol reflux three times, and merge extractive liquid, filters, and reclaims ethanol, concentrate extractum, subsequent use;
(c) in the above-mentioned prescription, Eupolyph aga sinesis Walker is broken into fine powder, and is subsequent use;
(d) in the above-mentioned prescription, Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water secondary, merge extractive liquid; Filter screen filters, and filtrating filters with inorganic ceramic film, and the inorganic ceramic membrane aperture is 50nm; The extracting solution temperature is 20 ℃ during filtration; Operation pressure reduction is 0.15Mpa, and membrane flux is 988ml/min, must filtrate;
E) step (d) gained filtrating and step (b) gained extracting solution are merged, concentrate extractum, add the fine drug powder oven dry of step (c) gained, be ground into fine powder, add step (a) gained fine drug powder, mixing, 1000 capsules of packing into.
Purified effect:
The filterable refining effect of table 4 inorganic ceramic film
| Test item | Membrane flux (ml/min) | Solid content clearance (%) | The peoniflorin rate of transform (%) |
| The result | 988 | 35.8 | 84.3 |
Embodiment 2:
The crude drug prescription is:
Radix Ginseng 45g 112g Radix Ophiopogonis Fructus Corni 224g Radix Salviae Miltiorrhizae 225g Semen Ziziphi Spinosae (parched) 186g Herba Taxilli 186g Radix Paeoniae Rubra 89g Radix Et Rhizoma Nardostachyos 45g Eupolyphaga Seu Steleophaga 35g Rhizoma Coptidis 45g Fructus Schisandrae Sphenantherae 67g Os Draconis 149g.
Process for purification does:
(a) in the above-mentioned prescription, Radix Ginseng is with 70% alcohol reflux three times, and 3 hours for the first time, each 2 hours later on, merge extractive liquid, filtered, and reclaims ethanol, concentrates, and oven dry is ground into fine powder, and is subsequent use;
(b) in the above-mentioned prescription, Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos are with 70% alcohol reflux three times, and merge extractive liquid, filters, and reclaims ethanol, concentrate extractum, subsequent use;
(c) in the above-mentioned prescription, Eupolyph aga sinesis Walker is broken into fine powder, and is subsequent use;
(d) in the above-mentioned prescription, Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water secondary, merge extractive liquid,, filter screen filters; Filtrating filters with inorganic ceramic film, and the inorganic ceramic membrane aperture is 100nm, and the extracting solution temperature is 20 ℃ during filtration; Operation pressure reduction is 0.20Mpa, and membrane flux is 1685ml/min, during extracting solution residue original volume 10%; Adding continues to filter with the water of volume, must filtrate;
E) step (d) gained filtrating and step (b) gained extracting solution are merged, concentrate extractum, add the fine drug powder oven dry of step (c) gained, be ground into fine powder, add step (a) gained fine drug powder, mixing, 1000 capsules of packing into.
Purified effect:
The filterable refining effect of table 5 inorganic ceramic film
| Test item | Membrane flux (ml/min) | Solid content clearance (%) | The peoniflorin rate of transform (%) |
| The result | 1685 | 37.9 | 94.3 |
Embodiment 3:
The crude drug prescription is:
Radix Ginseng 175g 192g Radix Ophiopogonis Fructus Corni 421g Radix Salviae Miltiorrhizae 440g Semen Ziziphi Spinosae (parched) 395g Herba Taxilli 396g Radix Paeoniae Rubra 188g Eupolyphaga Seu Steleophaga 98g Radix Et Rhizoma Nardostachyos 188g Rhizoma Coptidis 85g Fructus Schisandrae Sphenantherae 147g Os Draconis 278g.
Process for purification does:
(a) in the above-mentioned prescription, Radix Ginseng is with 70% alcohol reflux three times, and 3 hours for the first time, each 2 hours later on, merge extractive liquid, filtered, and reclaims ethanol, concentrates, and oven dry is ground into fine powder, and is subsequent use;
(b) in the above-mentioned prescription, Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos are with 70% alcohol reflux three times, and merge extractive liquid, filters, and reclaims ethanol, concentrate extractum, subsequent use;
(c) in the above-mentioned prescription, Eupolyph aga sinesis Walker is broken into fine powder, and is subsequent use;
(d) in the above-mentioned prescription, Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water secondary, merge extractive liquid,, filter screen filters; Filtrating filters with inorganic ceramic film, and the inorganic ceramic membrane aperture is 200nm, and the extracting solution temperature is 20 ℃ during filtration, and operation pressure reduction is 0.22Mpa; Membrane flux is 1133ml/min, during extracting solution residue original volume 10%, adds the water with volume, continues to be filtered to extracting solution residue original volume 10%; Add water once more, continue to filter, must filtrate with volume;
E) step (d) gained filtrating and step (b) gained extracting solution are merged, concentrate extractum, add the fine drug powder oven dry of step (c) gained, be ground into fine powder, add step (a) gained fine drug powder, mixing, 1000 capsules of packing into.
Purified effect:
The filterable refining effect of table 6 inorganic ceramic film
| Test item | Membrane flux (ml/min) | Solid content clearance (%) | The peoniflorin rate of transform (%) |
| The result | 1133 | 41.6 | 85.3 |
Embodiment 4:
The crude drug prescription is:
Radix Ginseng 90g, Radix Ophiopogonis 135g, Fructus Corni 270g, Radix Salviae Miltiorrhizae 200g, Semen Ziziphi Spinosae (parched) 150g, Herba Taxilli 150g, Radix Paeoniae Rubra 100g, Eupolyphaga Seu Steleophaga 100g, Radix Et Rhizoma Nardostachyos 95g, Rhizoma Coptidis 60g, Fructus Schisandrae Sphenantherae 75g, Os Draconis 150g.
Process for purification does:
(a) in the above-mentioned prescription, Radix Ginseng is with 70% alcohol reflux three times, and 3 hours for the first time, each 2 hours later on, merge extractive liquid, filtered, and reclaims ethanol, concentrates, and oven dry is ground into fine powder, and is subsequent use;
(b) in the above-mentioned prescription, Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos are with 70% alcohol reflux three times, and merge extractive liquid, filters, and reclaims ethanol, concentrate extractum, subsequent use;
(c) in the above-mentioned prescription, Eupolyph aga sinesis Walker is broken into fine powder, and is subsequent use;
(d) in the above-mentioned prescription, Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water secondary, merge extractive liquid,, filter screen filters; Filtrating filters with inorganic ceramic film, and the inorganic ceramic membrane aperture is 150nm, and the extracting solution temperature is 20 ℃ during filtration; Operation pressure reduction is 0.18Mpa, and membrane flux is 1427ml/min, during extracting solution residue original volume 10%; Adding continues to filter with the water of volume, must filtrate;
E) step (d) gained filtrating and step (b) gained extracting solution are merged, concentrate extractum, add the fine drug powder oven dry of step (c) gained, be ground into fine powder, add step (a) gained fine drug powder, mixing, 1000 capsules of packing into.
Purified effect:
The filterable refining effect of table 7 inorganic ceramic film
| Test item | Membrane flux (ml/min) | Solid content clearance (%) | The peoniflorin rate of transform (%) |
| The result | 1127 | 38.9 | 89.1 |
Claims (8)
1. the process for purification of a traditional Chinese medicine composition water extract, this Chinese medicine composition is to be processed by following bulk drugs: Radix Ginseng 45-180 part, Radix Ophiopogonis 50-200 part, Fructus Corni 125-450 part, Radix Salviae Miltiorrhizae 125-450 part, Semen Ziziphi Spinosae (parched) 95-400 part, Herba Taxilli 95-400 part, Radix Paeoniae Rubra 45-200 part, Eupolyphaga Seu Steleophaga 35-150 part, Radix Et Rhizoma Nardostachyos 45-200 part, Rhizoma Coptidis 25-90 part, Fructus Schisandrae Sphenantherae 35-150 part, Os Draconis 75-300 part; This Chinese medicine composition active component is processed by following steps:
A) people participates in 70% alcohol reflux three times, and merge extractive liquid, filters, and concentrates oven dry, the fine powder that is ground into;
B) Fructus Schisandrae Sphenantherae, Fructus Corni, Radix Salviae Miltiorrhizae, Rhizoma Coptidis, Radix Et Rhizoma Nardostachyos add 70% alcohol reflux 3 times jointly, and merge extractive liquid, filters spissated extractum;
C) fine powder that is broken into of Eupolyph aga sinesis Walker;
D) Radix Ophiopogonis, Semen Ziziphi Spinosae (parched), Herba Taxilli, Radix Paeoniae Rubra, Os Draconis decocte with water 2 times, merge extractive liquid,, refining, spissated extractum;
E) with step b) and d) merging of gained extractum, the fine drug powder of adding step c) gained, oven dry is ground into fine powder, adds step a) gained fine drug powder, and mixing promptly gets this Chinese medicine composition active component;
The process for purification that it is characterized in that step (d) gained water extract is that inorganic ceramic film filters.
2. process for purification according to claim 1 is characterized in that said inorganic ceramic membrane aperture is 50-200nm, and operation pressure reduction is 0.15-0.22Mpa.
3. process for purification according to claim 2 is characterized in that said inorganic ceramic membrane aperture is 100nm, and operation pressure reduction is 0.2Mpa.
4. process for purification according to claim 1 when it is characterized in that extracting solution residue original volume 10%, adds the water with volume, continues to filter, and must filtrate.
5. according to each described process for purification of claim 1-4, it is characterized in that said Chinese medicine composition processed by following bulk drugs:
89 parts of Radix Ginsengs, 112 parts of Radix Ophiopogonis, 224 parts of Fructus Corni, 224 parts of Radix Salviae Miltiorrhizaes, 186 parts of Semen Ziziphi Spinosae (parched)s, 186 parts of Herba Taxillis, 89 parts of Radix Paeoniae Rubra, 75 parts of Eupolyphaga Seu Steleophagas, 89 parts of Radix Et Rhizoma Nardostachyos, 45 parts of Rhizoma Coptidis, 67 parts of Fructus Schisandrae Sphenantheraes, 149 parts of Os Draconis.
6. according to each described process for purification of claim 1-4, said Chinese medicine composition is processed by following bulk drugs:
45 parts of Radix Ginsengs, 112 parts of Radix Ophiopogonis, 224 parts of Fructus Corni, 225 parts of Radix Salviae Miltiorrhizaes, 186 parts of Semen Ziziphi Spinosae (parched)s, 186 parts of Herba Taxillis, 89 parts of Radix Paeoniae Rubra, 45 parts of Radix Et Rhizoma Nardostachyos, 35 parts of Eupolyphaga Seu Steleophagas, 45 parts of Rhizoma Coptidis, 67 parts of Fructus Schisandrae Sphenantheraes, 149 parts of Os Draconis.
7. according to each described process for purification of claim 1-4, said Chinese medicine composition is processed by following bulk drugs:
278 parts of 147 parts of Os Draconis of Radix Ginseng 85 parts of Fructus Schisandrae Sphenantheraes of 188 portions of Rhizoma Coptidis of 98 parts of Radix Et Rhizoma Nardostachyos of 188 parts of Eupolyphaga Seu Steleophagas of 396 parts of Radix Paeoniae Rubra of 395 parts of Herba Taxillis of 440 parts of Semen Ziziphi Spinosae (parched)s of 421 parts of Radix Salviae Miltiorrhizaes of 192 parts of Fructus Corni, 175 parts of Radix Ophiopogonis.
8. according to each described process for purification of claim 1-4, said Chinese medicine composition is processed by following bulk drugs:
90 parts of Radix Ginsengs, 135 parts of Radix Ophiopogonis, 270 parts of Fructus Corni, 200 parts of Radix Salviae Miltiorrhizaes, 150 parts of Semen Ziziphi Spinosae (parched)s, 150 parts of Herba Taxillis, 100 parts of Radix Paeoniae Rubra, 100 parts of Eupolyphaga Seu Steleophagas, 95 parts of Radix Et Rhizoma Nardostachyos, 60 parts of Rhizoma Coptidis, 75 parts of Fructus Schisandrae Sphenantheraes, 150 parts of Os Draconis.
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| CN103550655A (en) * | 2013-11-06 | 2014-02-05 | 刘洁 | Medicament for treating premature beat |
| CN104906342A (en) * | 2014-03-11 | 2015-09-16 | 河北以岭医药研究院有限公司 | Applications of traditional Chinese medicine composition in preparation of post-myocardial infarction neural remodeling inhibition drugs |
| CN105079442A (en) * | 2015-09-21 | 2015-11-25 | 成都艾比科生物科技有限公司 | Extraction process applied to pilot production of Shensong heart-nourishing capsule |
| CN105726943A (en) * | 2016-04-15 | 2016-07-06 | 南方医科大学 | Medicine for treating ventricular premature beat and preparing method |
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| CN1403148A (en) * | 2002-10-24 | 2003-03-19 | 河北以岭医药研究院有限公司 | Medicines composition for treating coronary heart disease ventricular premature beat and its prepn |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103550655A (en) * | 2013-11-06 | 2014-02-05 | 刘洁 | Medicament for treating premature beat |
| CN104906342A (en) * | 2014-03-11 | 2015-09-16 | 河北以岭医药研究院有限公司 | Applications of traditional Chinese medicine composition in preparation of post-myocardial infarction neural remodeling inhibition drugs |
| CN105079442A (en) * | 2015-09-21 | 2015-11-25 | 成都艾比科生物科技有限公司 | Extraction process applied to pilot production of Shensong heart-nourishing capsule |
| CN105726943A (en) * | 2016-04-15 | 2016-07-06 | 南方医科大学 | Medicine for treating ventricular premature beat and preparing method |
| CN105726943B (en) * | 2016-04-15 | 2019-10-18 | 南方医科大学 | A kind of drug and preparation method of propafenone on ventricular premature beats |
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