CN1778339B - Medicine dropping pill for treating coronary heart disease and angina cordis - Google Patents
Medicine dropping pill for treating coronary heart disease and angina cordis Download PDFInfo
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- CN1778339B CN1778339B CN 200410072944 CN200410072944A CN1778339B CN 1778339 B CN1778339 B CN 1778339B CN 200410072944 CN200410072944 CN 200410072944 CN 200410072944 A CN200410072944 A CN 200410072944A CN 1778339 B CN1778339 B CN 1778339B
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- 208000029078 coronary artery disease Diseases 0.000 title claims abstract description 5
- 229940079593 drug Drugs 0.000 title claims description 25
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Landscapes
- Medicines Containing Plant Substances (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
A Chinese medicine in the form of dripping pill for treating coronary heart disease and angina pectoris is prepared from red sage root, notoginseng and ginseng or pilose asiabell root and borneol through extracting the liquid extract from red sage root, notoginseng, borneol, and ginseng or pilose asiabell root in water or alcohol, clarifying, ultrafiltering, concentrating, adding borneol and shaping.
Description
Technical field
The present invention relates to a kind of Chinese medicine of using the ultrafiltration technology preparation.Particularly, the present invention relates to a kind of Chinese medicine dripping pills of using the ultrafiltration technology preparation.
Background technology
Membrane separation technique (Membrane Separation Technique) is an emerging high efficient separation technology, by internationally recognized be a most rising great high production tech of mid-term 20 end of the centurys to 21 century.Ultrafiltration (Ultrafiltration, UF) technology is a kind of membrane separation technique, its ultimate principle is to utilize fenestra selectivity sieve performance, with separation, purification and condensed matter.Hyperfiltration process is that the anisotropic membrane (being asymmetric membrane) that utilizes macromolecular material to make is a filter medium, under normal temperature condition, relies on certain pressure and flow velocity, makes flow of solution through face, forces low molecular weight substance to see through film, and polymer substance is trapped.
Because hyperfiltration process is a physical method; do not have and must heat repeatedly; there be not " phase " to change; the probability of destroying effective ingredient is few than other universal method; characteristics such as technological process is short; thereby its be applied to extract in the research of pharmaceutically active ingredient become increasingly active; portioned product moves towards commercial production from laboratory research. and human ultrafiltrations such as 304 Wang Shiling of hospital of PLA are extracted effective ingredient baicalin in the Radix Scutellariae; the result shows that ultrafiltration is at productive rate; the purity aspect is excellent than well-established law all; and a ultrafiltration can reach the injection requirement; do not need again row refining; technology is simple; production cycle can shorten 1～2 times of (Wang Shiling; Zheng Dianbao " ultrafiltration is extracted the preliminary investigation of baicalin "; Chinese patent medicine research; 1988 (3): 5). Wang Shiling etc. have also further studied the optimum process condition of ultrafiltration extraction baicalin; it is the key that improves baicalin yield and quality that the experimental result proof is selected the ultrafilter membrane in suitable aperture (molecular cut off is 6000～10000) for use; the fluid temperature that raises simultaneously or reduction concentration; strict control pH value (pH=1.5 during acidify; pH=7.0 when alkali is molten); can significantly improve ultrasiltrated rate; obtain best output effect (Wang Shiling; " ultrafiltration is once extracted the technical study of baicalin "; Chinese patent medicine; 1994; 16 (3): 2). Xu Jinlin etc. are with ultrafiltration (polysulfone membrane; molecular cut off 6000) is used for the preparation of phytic acid; the phytic acid yield is 86.4%; improve 12.6% than conventional phytate method; and ultrafiltration gained phytic acid contains Phos hardly, appearance transparent is close to colourless (Xu Jinlin, Xu Jie; Wang Yuanjin " membrane separation technique prepares the research of phytic acid "; Chinese Journal of Pharmaceuticals, 1994,25 (4): 150). He Changsheng etc. use hyperfiltration technique separation and purification steviol glycosides; adopting ultrathin plate-type hyperfiltration device and molecular cut off is that 10000 cellulose acetate membrane (CA film) purifies field experimentation to steviol glycosides; its technological process is rationally feasible. the ultrafilter stable performance, and the decoloration performance and the removal of impurity of film are respond well, bubble problem (He Changsheng in the time of can solving precipitation that steviol glycosides usually occurs in producing and embedding preferably; WangBing Nan; Zhu Shanshan " applied research of steviol glycosides ultrafiltration ", water technology, 1994; 20 (2): 89). Huang is improved oneself and is adopted the refining sasanguasaponin of ultrafilter membrane (molecular cut off is 4000 and 10000 polysulfone membrane); with the domestic bleaching that mostly adopts; the recrystallize method; the alcohol ether sedimentation method and the basic salt sedimentation method compare, and the ultrafiltration flow process is simple, the efficient height; expense is low; to removing the oils and fats in the thick sasanguasaponin; pigment; saccharide and the strong impurity of other hydrophilic, can both producing a desired effect, (Huang is improved oneself, " ultrafiltrationmembrane process is made with extra care the sasanguasaponin pre-test " water technology; 1995; 21 (2): 99). Guo Li Wei of Nanjing University of Traditional Chinese Medicine etc. has relatively studied the influence of water alcohol method and ultrafiltration clarification Fructus Corni preparation to its preparation ingredient, and the result confirms that ultrafiltration is more effective to removing in the medicinal liquid saccharide impurity, and molecular cut off is that 10000 ultrafilter membrane does not have obviously influence to meliatin (molecular weight is 384); but being 1000 film, molecular cut off makes meliatin loss about 50% (Guo Liwei; Peng Guoping, Pan Yang etc. " the refining comparative study that contains the Fructus Corni Chinese medicine preparation of water alcohol method and membrane separation process ", Chinese patent medicine; 1999; 21 (2): 59). Wang Chengzhang etc. adopt ultrafiltration (polysulfone membrane, molecular cut off 30000) to separate with the ethanol extract of polyamide absorb-elute method to Folium Ginkgo; purification detects through high performance liquid chromatography (HPLC); the ginkgetin salidroside content is about 45%; yield is 0.5%～0.7%, more conventional steam distillation; the organic solvent extraction method is excellent, and can reduce discharge of wastewater in ultrafiltration technology; the protection environment; reduce production costs increase economic efficiency (Wang Chengzhang etc. " application of ultrafiltration in purification Folium Ginkgo flavone glycoside ", forestry science and technology communication; 1997, (2): 21).
Though hyperfiltration technique is applied to the production of Chinese medicine preparation its unique advantage is arranged, its degree of applying is still very limited, traces it to its cause, and remains in following problem:
(1) medicinal herb components complexity, particularly many compound preparations, effective ingredient are also unclear fully, therefore need to carry out very deep research before hyperfiltration technique is applied to Chinese herbal and crude drugs preparations.For example because the complexity of composition, do not carry out a large amount of pharmacology and clinical research test fully estimate ultrafiltration to Chinese medicine preparation in before the drug effect influence degree of each composition, ultrafiltration can not be applied to the production of most of Chinese medicine preparation.
(2) kind of membrane material is few, and membrane aperture distributes wide, and performance is understable.Used ultrafilter membrane material has cellulose acetate, polyacrylonitrile, polysulfones, SPSF, polysulfonamides etc. in Chinese medicine preparation production.By its affinity classification, be broadly divided into two classes: hydrophobic film material and hydrophilic film material to water.Hydrophilic film such as cellulose acetate, SPSF material is few to solute absorption, and molecular cut off is less, but poor heat stability, mechanical strength, chemical proof, antibacterium erosiveness are not high usually; Hydrophobic film materials such as polysulfones, the mechanical strength height, high temperature resistant, anti-solvent, anti-biodegradation, but because of containing a large amount of hydrophobicity genes or chain link in the strand, and have more electrostatic charge, thereby the permeable speed of film is low, contamination resistance is lower.
(3) pollution problem of film is to hinder hyperfiltration technique is moved towards the commercial Application stage by laboratory research biggest obstacle.In the ultra-filtration process of Chinese medicine preparation, when not good as if the medicinal liquid pretreating effect, face easily pollutes, and fenestra stops up, and making permeation flux is that productivity ratio descends, even cisco unity malfunction, and production efficiency reduces, and cost rises, and causes the shortening in service life of film.
(4) system of selection of membrane module is not set up as yet, the optimization of still needing of ultrafiltration parameter.The factor that influences the ultrafiltration effect is a lot, comprises the selection of membrane module, the cleaning method after the definite and ultrafilter of technological parameter uses etc.Therefore be applicable to ultrafiltration apparatus and the operating procedure that the ultrafiltration of Chinese medicine system is used, remain further to be studied.
The inventor by a large amount of experimental datas are analyzed, has determined suitable process condition, for the suitability for industrialized production of utilizing ultrafiltration to carry out medicine of the present invention provides concrete solution through the effort of long-term and unremitting ground.
Summary of the invention
The object of the present invention is to provide a kind of treatment treating coronary heart disease and angina pectoris drop pill.
The present invention is implemented by following scheme:
The present invention realizes by following technical step: with Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Ginseng and Borneolum Syntheticum is crude drug, is prepared according to following steps:
(1) Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Ginseng are mixed or make water extract or alcohol extract separately;
(2) described extracting solution being carried out predefecation handles;
(3) further described extracting solution is carried out hyperfiltration treatment;
(4) ultrafiltrate is condensed into extractum; With gained extractum and Borneolum Syntheticum and adjuvant mixed evenly after, make dropping pill formulation.
The proportioning of above-mentioned raw materials medicine is counted by weight: Radix Salviae Miltiorrhizae 20～97, Radix Notoginseng 2～79, Borneolum Syntheticum 0.2～3, Radix Ginseng 10～40; Be preferably: Radix Salviae Miltiorrhizae 63.0～94.0, Radix Notoginseng 4.0～35.0, Borneolum Syntheticum 0.5～2.0, Radix Ginseng 15～30; More preferably: Radix Salviae Miltiorrhizae 75.2～90, Radix Notoginseng 9～23.5, Borneolum Syntheticum 0.5～1.3, Radix Ginseng 20～25.
Above-mentioned raw materials medicine Radix Ginseng can be replaced with Radix Codonopsis, and promptly the above-mentioned raw materials medicine can be Radix Salviae Miltiorrhizae 20～97, Radix Notoginseng 2～79, Borneolum Syntheticum 0.2～3, Radix Codonopsis 10～40; Be preferably: Radix Salviae Miltiorrhizae 63.0～94.0, Radix Notoginseng 4.0～35.0, Borneolum Syntheticum 0.5～2.0, Radix Codonopsis 15～30; More preferably: Radix Salviae Miltiorrhizae 75.2～90, Radix Notoginseng 9～23.5, Borneolum Syntheticum 0.5～1.3, Radix Codonopsis 20～25.
In the technology of the present invention step (1), alcohol extract can be the extracting solution of the lower alcohol of variable concentrations such as methanol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol etc. or the extracting solution of its mixture.Carrying out next step predefecation after alcohol extract can not concentrate or suitably concentrate handles.
In the technology of the present invention step (2), preliminary clarifying treatment can be carried out coarse filtration with general material such as gauze, tiffany etc., the also available material such as the ceramic membrane of specialty carry out microfiltration, also can behind high speed centrifugation, divide and get supernatant, adsorption clarifications such as also available flocculating agent such as flocculate with chitosan clarifier, 101 fruit juice clarifiers, ZTC1+1 natural clarifying agent, Ovum Gallus domesticus album flocculating agent and remove particle bigger in the medicinal liquid, also available alcohol deposition method is removed most impurity.Both can singly use above-mentioned defecation method, but also use in conjunction, coarse filtration-adsorption clarification for example, adsorption clarification-high speed centrifugation, coarse filtration-microfiltration, coarse filtration-precipitate with ethanol etc.After can not concentrating or suitably concentrate, the solution that predefecation is handled carries out next step ultrafiltration; Preferably do not concentrate the ultrafiltration of promptly carrying out next step.
In the technology of the present invention step (3), the used ultrafilter membrane of ultrafiltration can be cellulose diacetate film (CA), three cellulose acetate membrane (CTA), cyanoethyl cellulose film (CN-CA), polysulfone membrane (PS), sulfonated polysulfone membrane (SPS), poly (ether sulfone) film (PES), sulfonated polyether sulfone film (SPES), polysulfonamides film (PSA), phenolphthalein side group polyarylsulfone (PAS) film (PDS), polyvinylidene fluoride film (PVDF), polyacrylonitrile film (PAN), polyimide film (N), cellulose membrane, methyl methacrylate-acrylonitrile copolymer film (MMA-AN), polyacrylonitrile/cellulose diacetate (PAN/CA) blend film, the dynamically ultrafilter membrane that forms, and the Modified Membrane of above-mentioned film.Be preferably cellulose diacetate film (CA), three cellulose acetate membrane (CTA), polysulfone membrane (PS), sulfonated polysulfone membrane (SPS), poly (ether sulfone) film (PES), sulfonated polyether sulfone film (SPES), polysulfonamides film (PSA), polyvinylidene fluoride film (PVDF), polyacrylonitrile film (PAN).
The molecular cut off of above-mentioned ultrafilter membrane is generally 6000～80000, is preferably 10000～70000, and the best is 20000～50000.
Ultrafiltration both can be adopted cross flow filter, also can adopt dead-end filtration, but preferred cross flow filter.
The operating condition of ultrafiltration technology is as follows:
(1) the inlet pressure of ultrafiltration is 0.1～0.5MPa, is preferably 0.1～0.35Mpa, and the best is 0.25～0.35Mpa; The liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.5～0.25kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1～0.2Mpa.
(2) the feed liquid flow velocity is 1.0～4.0m/s, is preferably 2.0～3.0m/s.In the ultra-filtration process, adopt the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 1.0～2.0m/s.
(3) feed high-pressure inert gas such as nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle is that 0.5h～2h ventilates once, each 1 minute.
(3) feed temperature is 15～50 ℃, is preferably 20～40 ℃.
(4) when feed liquid stock solution is concentrated 1/15～1/5, add water or dilute alcohol solution ultrafiltration 1～2 time again; Be preferably when feed liquid stock solution is concentrated 1/12～1/8, add water or dilute alcohol solution ultrafiltration 1～2 time again.
(5) pH value of feed liquid is controlled at 5～9, is preferably 6.0～7.5;
(6) backwash condition: backwashing pressure is 0.15～2.5MPa, and backwashing period is that 0.5～1.5h, backwashing time are 1min～10min.When ultrafiltration module use in parallel is replaced the method for recoil, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, exchange is carried out behind the certain interval of time, generally is work 10～20min, recoil 30sec～3min.
(7) the Chemical cleaning cycle is 0.5 month～2 months, the Chemical cleaning medicament is generally diluted acid, diluted alkaline, surfactant, be preferably for example 0.5%～4.0% sodium hydroxide of diluted alkaline, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite etc., pH value is 10～12, and cleaning pressure is 0.05～1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
In ultra-filtration process, both periodic pressure oscillation or the fluctuation of periodicity flow or periodicity fed noble gas separately, also can unite use, be periodic pressure fluctuation and periodically flow fluctuation associating use, perhaps the periodic pressure fluctuation is with periodically feeding noble gas unites use, perhaps periodically the flow fluctuation is with periodically feeding noble gas unites use, and perhaps the three unites use together.
In the technology of the present invention step (4), ultrafiltrate is condensed into extractum after, with Borneolum Syntheticum and adjuvant mixed evenly after, add the transconversion into heat material, move into dripping jar of drop pill machine, medicine liquid droplet is removed liquid paraffin to cryogenic liquid paraffin, select ball.
Wherein: adjuvant is a Polyethylene Glycol-6000, and 53～58 ℃ of its condensation points, addition are extractum and Borneolum Syntheticum weight 2～6 times; Changing the material temperature is 60～100 ℃; The temperature of liquid paraffin is 0～10 ℃ (the best is 5～10 ℃); Ball heavily is 5～50mg/ grain, diameter 1.95～4.29mm.
Experimental example Drug therapy angina pectoris of the present invention clinical observation on the therapeutic effect
1 clinical data
Ischemic heart desease, the anginal clinical diagnosis standard of WHO regulation pressed in diagnostic criteria, is divided into two groups at random, A group: 100 examples, 52～70 years old age, average 59.4 years old; B group: 100 examples, 50～68 years old, average 57 years old.
2 medicines and method
Two groups of patients carry out the general physical inspection, and the treatment group is thrown to medicine 250mg of the present invention behind Electrocardioscopy and the lab testing, and every day 3 times is oral, 3 months courses of treatment, matched group is thrown to FUFANG DANSHEN PIAN each 4, and every day 3 times is oral, and matched group angina pectoris type and treatment group are approximate.Observational technique: two groups of patients inactive all microcirculation improvement in the phase of receiving treatment, reduce the medicine of heart oxygen consumption, to the frequent patient of angina pectoris attacks, the sublingual administration nitroglycerine tablets are with relief of symptoms during outbreak, two groups of every two weeks of patient are had an electro-cardiogram once, the tight analgesic effect of observing two groups of medicines during the treatment, remission situation, electrocardiogram variation and heart rate, blood pressure, hepatic and renal function change, and heart rate, blood pressure and hepatic and renal function change two groups of controlled observations.
3 efficacy assessment standards and result
Produce effects: uncomfortable in chest, precordialgia symptom complete obiteration, it is normal that ECG ST-T changes recovery; Effectively: uncomfortable in chest, precordialgia sx, attack times reduces, and electrocardio diagram S-T changes the recovery that has to a certain degree; Invalid: symptom does not have improvement, the electrocardiogram no change.
4 results
Angina degree and electrocardiogram change sees attached list.
Two groups of case angina pectoriss of subordinate list and electrocardiogram improve situation (n=100)
Heart rate, blood pressure and two groups of patients of hepatic and renal function do not have significant change.
The specific embodiment
The invention will be further elaborated below in conjunction with embodiment.These embodiment only are used to the purpose that exemplifies, rather than limit the present invention by any way.
Embodiment one
Crude drug adopts Radix Salviae Miltiorrhizae 37.5g, Radix Notoginseng 11.8g, Borneolum Syntheticum 0.8g, Radix Ginseng 10.0g.
With ethanol extraction Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Ginseng, get the ethanol extract that it mixes medical material, with this extracting liquid filtering, collect filtrate with gauze.Filtrate is that 6000 cellulose diacetate film carries out ultrafiltration with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.5kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1Mpa.The feed liquid flow velocity is 1.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 1.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 0.5h ventilates once each 1 minute.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/15, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 0.15MPa, and backwashing period is that 0.5h, backwashing time are 1min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 10min, recoil 30sec.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃ with Polyethylene Glycol-6000 18g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment two
Crude drug adopts Radix Salviae Miltiorrhizae 46.5g, Radix Notoginseng 3.0g, Borneolum Syntheticum 0.8g, Radix Ginseng 8.5g.
Radix Salviae Miltiorrhizae, the people of coarse pulverization are participated in 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, fries in shallow oil 1 hour, filters, and filtering residue discards, and merging filtrate gets the Radix Salviae Miltiorrhizae Radix Ginseng extractive solution.With 70% ethanol extraction Radix Notoginseng, get the Radix Notoginseng extracting solution.Above-mentioned Radix Salviae Miltiorrhizae Radix Ginseng extractive solution and Radix Notoginseng extracting solution are merged, leave standstill, filter.Filtrate is that 80000 polysulfone membrane is carried out ultrafiltration with molecular cut off, and filter type adopts dead-end filtration.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.5Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.2Mpa.The feed liquid flow velocity is 4.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 2.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 2h ventilates once each 1 minute.Feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/5, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 9.Backwashing pressure is 2.5MPa, and backwashing period is that 1.5h, backwashing time are 10min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 20min, recoil 3min.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃ with Polyethylene Glycol-6000 20g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment three
Crude drug adopts Radix Salviae Miltiorrhizae 26.0g, Radix Notoginseng 16.5g, Borneolum Syntheticum 0.7g, Radix Ginseng 17.0g.
Obtain blended ethanol extract with ethanol extraction Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Ginseng, get supernatant dividing behind this extracting solution high speed centrifugation.With this liquid molecular cut off is that 50000 polysulfone membrane is carried out ultrafiltration, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.20kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.2Mpa.The feed liquid flow velocity is 3.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 2.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 2h ventilates once each 1 minute.Feed temperature is 40 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 7.5.Backwashing pressure is 2.5MPa, and backwashing period is that 1.5h, backwashing time are 10min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 20min, recoil 3min.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 20g is mixed.In ℃ methyl-silicone oil of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment four
Crude drug adopts Radix Salviae Miltiorrhizae 49.0 grams, Radix Notoginseng 8.4 grams, Borneolum Syntheticum 0.6 gram, Radix Ginseng 6.0g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the ginseng crude drug of coarse pulverization are added in the extraction pot, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, fries in shallow oil 1 hour, filters, and filtering residue discards, merging filtrate.Filtrate is that 6000 cellulose diacetate film carries out ultrafiltration with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.5kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1Mpa.The feed liquid flow velocity is 1.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 1.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 0.5h ventilates once each 1 minute.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/15, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 0.15MPa, and backwashing period is that 0.5h, backwashing time are 1min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 10min, recoil 30sec.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 21g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment five
Crude drug adopts Radix Salviae Miltiorrhizae 24.2 grams, Radix Notoginseng 25.5 grams, Borneolum Syntheticum 0.4 gram, Radix Ginseng 10.0g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the ginseng crude drug of coarse pulverization are added in the extraction pot, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, fries in shallow oil 1 hour, filters, and filtering residue discards, merging filtrate.Filtrate is that 80000 polysulfone membrane is carried out ultrafiltration with molecular cut off, and filter type adopts dead-end filtration.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.5Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.2Mpa.The feed liquid flow velocity is 4.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 2.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 2h ventilates once each 1 minute.Feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/5, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 9.Backwashing pressure is 2.5MPa, and backwashing period is that 1.5h, backwashing time are 10min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 20min, recoil 3min.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.32～1.40 (55 ℃), get extractum and Borneolum Syntheticum, evenly mixed with Polyethylene Glycol-6000 20g, be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment six
Crude drug adopts Radix Salviae Miltiorrhizae 16.2 grams, Radix Notoginseng 29.5 grams, Borneolum Syntheticum 0.4 gram, Radix Ginseng 13.8g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the ginseng crude drug of coarse pulverization are added in the extraction pot, add the 0.89g sodium bicarbonate, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, add 4 times of water gagings, fried in shallow oil 1 hour, and filtered, filtering residue discards, merging filtrate. filtrate is that 50000 polysulfone membrane is carried out ultrafiltration with molecular cut off, filter type adopts cross flow filter. and the operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35Mpa, and the low 0.20kPa. ultrafiltration initial stage of the liquid outlet pressure ratio inlet pressure of ultrafiltration is adopted lower pressure, slowly boosts then; In ultra-filtration process, the fluctuation of employing periodic pressure, the pressure wave moment is that 0.2Mpa. feed liquid flow velocity is 3.0m/s, in the ultra-filtration process, adopt periodically flow fluctuation so that in membrane channels, produce pulsating flow or non-stationary flow, the flow speed wave moment is 2.0m/s, feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, cycle is that 2h ventilates once, each 1 minute. feed temperature is 40 ℃, when feed liquid stock solution is concentrated 1/8, add water or dilute alcohol solution ultrafiltration 2 times again, it is 2.5MPa that the pH value of feed liquid is controlled at the 7.5. backwashing pressure, backwashing period is 1.5h, backwashing time is that 10min. is when replacing the method for recoil with ultrafiltration module use in parallel, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, exchange is carried out behind the certain interval of time, work 20min, the recoil 3min. Chemical cleaning cycle is 2 months, the Chemical cleaning medicament is 0.5%～4.0% sodium hydroxide, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, pH value is 10～12, and cleaning pressure is 1.0MPa. after cleaning with chemical, and the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.32～1.40 (55 ℃), get extractum and Borneolum Syntheticum, evenly mixed with Polyethylene Glycol-6000 18g, be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment seven
Crude drug adopts Radix Salviae Miltiorrhizae 37.5g, Radix Notoginseng 11.8g, Borneolum Syntheticum 0.8g, Radix Codonopsis 10.0g.
With ethanol extraction Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Codonopsis, get the ethanol extract that it mixes medical material, with this extracting liquid filtering, collect filtrate with gauze.Filtrate is that 6000 cellulose diacetate film carries out ultrafiltration with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.5kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1Mpa.The feed liquid flow velocity is 1.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 1.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 0.5h ventilates once each 1 minute.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/15, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 0.15MPa, and backwashing period is that 0.5h, backwashing time are 1min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 10min, recoil 30sec.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃ with Polyethylene Glycol-6000 18g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment eight
Crude drug adopts Radix Salviae Miltiorrhizae 46.5g, Radix Notoginseng 3.0g, Borneolum Syntheticum 0.8g, Radix Codonopsis 8.5g.
Radix Salviae Miltiorrhizae with coarse pulverization, Radix Codonopsis adds 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, add 4 times of water gagings, fried in shallow oil 1 hour, and filtered, filtering residue discards, merging filtrate, get Radix Salviae Miltiorrhizae Radix Codonopsis extracting solution. with 70% ethanol extraction Radix Notoginseng, get the Radix Notoginseng extracting solution. above-mentioned Radix Salviae Miltiorrhizae Radix Codonopsis extracting solution and Radix Notoginseng extracting solution are merged, leave standstill, filtering. filtrate is that 80000 polysulfone membrane is carried out ultrafiltration with molecular cut off, filter type adopts dead-end filtration. and the operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.5Mpa, and the low 0.25kPa. ultrafiltration initial stage of the liquid outlet pressure ratio inlet pressure of ultrafiltration is adopted lower pressure, slowly boosts then; In ultra-filtration process, the fluctuation of employing periodic pressure, the pressure wave moment is that 0.2Mpa. feed liquid flow velocity is 4.0m/s, in the ultra-filtration process, adopt periodically flow fluctuation so that in membrane channels, produce pulsating flow or non-stationary flow, the flow speed wave moment is 2.0m/s, feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, cycle is that 2h ventilates once, each 1 minute. feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/5, add water or dilute alcohol solution ultrafiltration 2 times again, it is 2.5MPa that the pH value of feed liquid is controlled at 9. backwashing pressures, backwashing period is 1.5h, backwashing time is that 10min. is when replacing the method for recoil with ultrafiltration module use in parallel, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, exchange is carried out behind the certain interval of time, work 20min, the recoil 3min. Chemical cleaning cycle is 2 months, the Chemical cleaning medicament is 0.5%～4.0% sodium hydroxide, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, pH value is 10～12, and cleaning pressure is 1.0MPa. after cleaning with chemical, and the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃ with Polyethylene Glycol-6000 20g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment nine
Crude drug adopts Radix Salviae Miltiorrhizae 26.0g, Radix Notoginseng 16.5g, Borneolum Syntheticum 0.7g, Radix Codonopsis 17.0g.
Obtain blended ethanol extract with ethanol extraction Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Codonopsis, get supernatant dividing behind this extracting solution high speed centrifugation.With this liquid molecular cut off is that 50000 polysulfone membrane is carried out ultrafiltration, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.20kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.2Mpa.The feed liquid flow velocity is 3.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 2.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 2h ventilates once each 1 minute.Feed temperature is 40 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 7.5.Backwashing pressure is 2.5MPa, and backwashing period is that 1.5h, backwashing time are 10min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 20min, recoil 3min.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 20g is mixed.In ℃ methyl-silicone oil of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment ten
Crude drug adopts Radix Salviae Miltiorrhizae 49.0 grams, Radix Notoginseng 8.4 grams, Borneolum Syntheticum 0.6 gram, Radix Codonopsis 6.0g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the codonopsis pilosula of coarse pulverization are added in the extraction pot, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, add 4 times of water gagings, fried in shallow oil 1 hour, filter, filtering residue discards, merging filtrate. and filtrate is that 6000 cellulose diacetate film carries out ultrafiltration with molecular cut off, and filter type adopts cross flow filter. and the operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1Mpa, the low 0.5kPa. ultrafiltration initial stage of the liquid outlet pressure ratio inlet pressure of ultrafiltration is adopted lower pressure, slowly boosts then; In ultra-filtration process, the fluctuation of employing periodic pressure, the pressure wave moment is that 0.1Mpa. feed liquid flow velocity is 1.0m/s, in the ultra-filtration process, adopt periodically flow fluctuation so that in membrane channels, produce pulsating flow or non-stationary flow, the flow speed wave moment is 1.0m/s, feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, cycle is that 0.5h ventilates once, each 1 minute. feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/15, add water or dilute alcohol solution ultrafiltration 1 time again, it is 0.15MPa that the pH value of feed liquid is controlled at 5. backwashing pressures, backwashing period is 0.5h, backwashing time is that 1min. is when replacing the method for recoil with ultrafiltration module use in parallel, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, exchange is carried out behind the certain interval of time, work 10min, the recoil 30sec. Chemical cleaning cycle is 0.5 month, the Chemical cleaning medicament is 0.5%～4.0% sodium hydroxide, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, pH value is 10～12, and cleaning pressure is 0.05MPa. after cleaning with chemical, and the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.35～1.39 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 21g is mixed.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment 11
Crude drug adopts Radix Salviae Miltiorrhizae 24.2 grams, Radix Notoginseng 25.5 grams, Borneolum Syntheticum 0.4 gram, Radix Codonopsis 10.0g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the codonopsis pilosula of coarse pulverization are added in the extraction pot, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, fries in shallow oil 1 hour, filters, and filtering residue discards, merging filtrate.Filtrate is that 80000 polysulfone membrane is carried out ultrafiltration with molecular cut off, and filter type adopts dead-end filtration.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.5Mpa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then; In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.2Mpa.The feed liquid flow velocity is 4.0m/s, in the ultra-filtration process, adopts periodically flow fluctuation so that produce pulsating flow or non-stationary flow in membrane channels, the flow speed wave moment is 2.0m/s, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle is that 2h ventilates once each 1 minute.Feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/5, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 9.Backwashing pressure is 2.5MPa, and backwashing period is that 1.5h, backwashing time are 10min.When with the in parallel method of using alternately recoil of ultrafiltration module, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, and exchange is carried out behind the certain interval of time, work 20min, recoil 3min.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 0.5%～4.0% sodium hydroxide, 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10～12, and cleaning pressure is 1.0MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.32～1.40 (55 ℃), get extractum and Borneolum Syntheticum, evenly mixed with Polyethylene Glycol-6000 20g, be heated to 60 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Embodiment 12
Crude drug adopts Radix Salviae Miltiorrhizae 16.2 grams, Radix Notoginseng 29.5 grams, Borneolum Syntheticum 0.4 gram, Radix Codonopsis 13.8g.
Radix Salviae Miltiorrhizae, Radix Notoginseng and the codonopsis pilosula of coarse pulverization are added in the extraction pot, add the 0.89g sodium bicarbonate, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out the second time and extracts, add 4 times of water gagings, fried in shallow oil 1 hour, and filtered, filtering residue discards, merging filtrate. filtrate is that 50000 polysulfone membrane is carried out ultrafiltration with molecular cut off, filter type adopts cross flow filter. and the operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35Mpa, and the low 0.20kPa. ultrafiltration initial stage of the liquid outlet pressure ratio inlet pressure of ultrafiltration is adopted lower pressure, slowly boosts then; In ultra-filtration process, the fluctuation of employing periodic pressure, the pressure wave moment is that 0.2Mpa. feed liquid flow velocity is 3.0m/s, in the ultra-filtration process, adopt periodically flow fluctuation so that in membrane channels, produce pulsating flow or non-stationary flow, the flow speed wave moment is 2.0m/s, feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, cycle is that 2h ventilates once, each 1 minute. feed temperature is 40 ℃, when feed liquid stock solution is concentrated 1/8, add water or dilute alcohol solution ultrafiltration 2 times again, it is 2.5MPa that the pH value of feed liquid is controlled at the 7.5. backwashing pressure, backwashing period is 1.5h, backwashing time is that 10min. is when replacing the method for recoil with ultrafiltration module use in parallel, wherein a cover or a few cover carry out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of a part of filtrate, exchange is carried out behind the certain interval of time, work 20min, the recoil 3min. Chemical cleaning cycle is 2 months, the Chemical cleaning medicament is 0.5%～4.0% sodium hydroxide, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, pH value is 10～12, and cleaning pressure is 1.0MPa. after cleaning with chemical, and the flushing of reuse water is near neutral.
Described ultrafiltrate concentrated obtain the extractum that relative density is 1.32～1.40 (55 ℃), get extractum and Borneolum Syntheticum, evenly mixed with Polyethylene Glycol-6000 18g, be heated to 85 ℃ of temperature, change material after 20～120 minutes, move in the dropping-pill machine jar that jar temperature remains on 85～90 ℃.In ℃ liquid paraffin of medicine liquid droplet to 7～8, take out drop pill, oil removing, screen cloth selects ball, makes 1000 drop pill, promptly.
Claims (12)
1. treat the treating coronary heart disease and angina pectoris drop pill for one kind, it is that crude drug is made with Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Codonopsis and Borneolum Syntheticum perhaps with Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Ginseng and Borneolum Syntheticum, it is characterized in that the processing step of its preparation is:
(1) Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Ginseng or Radix Codonopsis are mixed or make water extract or alcohol extract separately;
(2) described extracting solution being carried out predefecation handles;
(3) further described extracting solution is carried out hyperfiltration treatment;
(4) ultrafiltrate is concentrated, with gained extractum and Borneolum Syntheticum and adjuvant mixed even after, make drop pill;
The operating procedure condition of described hyperfiltration treatment is as follows:
The inlet pressure of ultrafiltration is 0.1～0.5MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25～0.5kPa; Feed temperature is 15～50 ℃; The pH value of feed liquid is controlled at 5～9; When feed liquid stock solution is concentrated 1/15～1/5, add water or dilute alcohol solution ultrafiltration 1～2 time again;
The weight proportion of described crude drug is: Radix Salviae Miltiorrhizae 20～97, Radix Notoginseng 2～79, Borneolum Syntheticum 0.2～3, Radix Ginseng or Radix Codonopsis 10～40.
2. medicinal dropping ball according to claim 1 is characterized in that the weight proportion of described crude drug is:
Radix Salviae Miltiorrhizae 63.0～94.0,
Radix Notoginseng 4.0～35.0,
Borneolum Syntheticum 0.5～2.0,
Radix Ginseng or Radix Codonopsis 15～30.
3. medicinal dropping ball according to claim 2 is characterized in that the weight proportion of described crude drug is:
Radix Salviae Miltiorrhizae 75.2～90,
Radix Notoginseng 9～23.5,
Borneolum Syntheticum 0.5～1.3,
Radix Ginseng or Radix Codonopsis 20～25.
4. medicinal dropping ball according to claim 1 is characterized in that described alcohol extract is to be selected from the following lower alcohol or the extracting solution of its mixture: methanol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol.
5. medicinal dropping ball according to claim 4, its feature is an ethanol extract at described alcohol extract.
6. what medicinal dropping ball according to claim 1, its feature obtained in described step (1) is the ethanol extract that Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Ginseng or Radix Codonopsis are mixed and made into.
7. what medicinal dropping ball according to claim 1, its feature obtained in described step (1) is the aqueous extract that Radix Salviae Miltiorrhizae, Radix Notoginseng and Radix Ginseng or Radix Codonopsis are mixed and made into.
8. medicinal dropping ball according to claim 1, its feature in described step (1) is: the Radix Salviae Miltiorrhizae of the coarse pulverization of learning from else's experience, Radix Notoginseng and Radix Ginseng or codonopsis pilosula add an amount of sodium bicarbonate to extraction pot, decoct with water secondary, filter, filtering residue discards, merging filtrate gets extracting solution.
9. medicinal dropping ball according to claim 1 is characterized in that described predefecation is treated to coarse filtration-adsorption clarification, adsorption clarification-high speed centrifugation, coarse filtration-microfiltration or coarse filtration-precipitate with ethanol.
10. medicinal dropping ball according to claim 1, it is characterized in that the used ultrafilter membrane of described hyperfiltration treatment is selected from: cellulose diacetate film, three cellulose acetate membrane, cyanoethyl cellulose film, polysulfone membrane, sulfonated polysulfone membrane, poly (ether sulfone) film, sulfonated polyether sulfone film, polysulfonamides film, phenolphthalein side group polyarylsulfone (PAS) film, polyvinylidene fluoride film, polyacrylonitrile film, polyimide film, cellulose membrane, methyl methacrylate-acrylonitrile copolymer film, polyacrylonitrile/cellulose diacetate blend film, the dynamically ultrafilter membrane that forms, and the Modified Membrane of above-mentioned film; The molecular cut off of its ultrafilter membrane is 6000～80000.
11. medicinal dropping ball according to claim 10, it is characterized in that described ultrafilter membrane is selected from: cellulose diacetate film, three cellulose acetate membrane, polysulfone membrane, sulfonated polysulfone membrane, poly (ether sulfone) film, sulfonated polyether sulfone film, polysulfonamides film, polyvinylidene fluoride film, polyacrylonitrile film; The molecular cut off of its ultrafilter membrane is 10000～70000.
12. medicinal dropping ball according to claim 1 is characterized in that, in the process of described ultrafiltration separately or unite the following method that adopts: periodic pressure fluctuation, periodically flow fluctuation, feed noble gas off and on; Wherein the pressure wave moment of periodic pressure fluctuation is 0.1～0.2Mpa, and periodically the flow speed wave moment of flow fluctuation is 1.0～2.0 meter per seconds, feeds noble gas off and on and be ventilation in 0.5 hour～2 hours once, each 1 minute.
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| CN1348815A (en) * | 2001-11-09 | 2002-05-15 | 天津天士力制药股份有限公司 | Medicine for preventing and treating coronary heart disease and angina pectoris and its prepn and other use |
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| CN1348815A (en) * | 2001-11-09 | 2002-05-15 | 天津天士力制药股份有限公司 | Medicine for preventing and treating coronary heart disease and angina pectoris and its prepn and other use |
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