CN1751705B - Traditional Chinese medicine preparation containing red-rooted salvia - Google Patents
Traditional Chinese medicine preparation containing red-rooted salvia Download PDFInfo
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- CN1751705B CN1751705B CN 200410072059 CN200410072059A CN1751705B CN 1751705 B CN1751705 B CN 1751705B CN 200410072059 CN200410072059 CN 200410072059 CN 200410072059 A CN200410072059 A CN 200410072059A CN 1751705 B CN1751705 B CN 1751705B
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- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
- 238000002562 urinalysis Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A Chinese medicine containing red sage root is prepared through extracting the liquid from the Chinese-medicinal materials including red sage root, clarifying, ultrafiltering and shaping. The details about said ultrafiltering are also disclosed.
Description
Technical field
The present invention relates to a kind of Chinese medicine preparation that contains Radix Salviae Miltiorrhizae, particularly use the Chinese medicine preparation that contains Radix Salviae Miltiorrhizae that the membrane ultrafiltration prepared forms.
Background technology
Radix Salviae Miltiorrhizae has stasis-dispelling and pain-killing, promoting blood circulation to restore menstrual flow, the effect of the relieving restlessness that clears away heart-fire, and is to treat one of coronary heart disease and anginal active drug clinically, and there are more than one hundred million tons in the annual whole nation of its use amount.The single preparations of ephedrine of Radix Salviae Miltiorrhizae has Radix Salviae Miltiorrhizae Injection, Radix Salviae Miltiorrhizae Tabellae etc., is that the compound Salviae Miltiorrhizae prescribed preparation of principal agent is just more with the Radix Salviae Miltiorrhizae, as FUFANG DANSHEN PIAN, FUFANG DANSHEN DIWAN, coronary disease granule, FUFANG DANSHEN ZHUSHEYE etc.But no matter be Radix Salviae Miltiorrhizae single preparations of ephedrine or red sage compound preparation, its traditional extraction process generally adopts pure water law or water alcohol method.Along with the employing of new technique, the extraction separation that extraction process for purification that some are new such as hyperfiltration technique are applied to Chinese medicine is to obtain better refining effect.Officina of Beijing Hospital of the Air Force of Chinese People's Liberation Army (Chinese herbal medicine, 1981,12 (12): 8-12) use cellulose acetate membrane CA
3, pressure is at 3kg/cm
2In time, prepare FUFANG DANSHEN ZHUSHEYE (Radix Salviae Miltiorrhizae, Lignum Dalbergiae Odoriferae), thinks that the FUFANG DANSHEN ZHUSHEYE with the ultrafiltration preparation is better than the FUFANG DANSHEN ZHUSHEYE of conventional preparation at aspects such as clarity, granularity, removal of impurity efficient.But the factor that influences ultrafiltration is a lot, and is not strong with above-mentioned simple ultrafiltration technology condition operability on commercial Application.For stablizing the process conditions of ultrafiltration, the people is also arranged when using pure water law, adopt ultrafiltration to make with extra care.Hao Li has carried out improving (Chinese herbal medicine with ultrafiltration (ultrafilter membrane of molecular cut off 20000) to the preparation technology of Radix Salviae Miltiorrhizae Injection, 1996,27 (8): 471), the technology that adopts is: Radix Salviae Miltiorrhizae decocts, concentrates, the concentrated solution precipitate with ethanol gets semi-finished product, dosing then, ultrafiltration, embedding, sterilization, lamp inspection, pack finished product.Usefulness micelle ultrafiltrations such as wangdan prepare Radix Salviae Miltiorrhizae Injection (Chinese patent medicine, 2003,25 (6): 441-443), the technology that adopts is: Radix Salviae Miltiorrhizae water is carried, extracting solution concentrates (proportion 1.35), adds 3 times of amount ethanol precipitate with ethanol, and alcohol deposit fluid adds the water water precipitating, water precipitating liquid paper pulp coarse filtration, coarse filtration liquid adds tween 80 and forms micelle solution, the micelle solution ultrafiltration, the dosing of fine straining liquid, embedding, sterilize finished product.But the above-mentioned desk study that in laboratory red sage formulation is carried out ultrafiltration preparation does not provide more detailed process conditions, be difficult to be applied on the suitability for industrialized production, moreover before ultrafiltration, dispel impurity and also have more disadvantage with alcohol deposition method, for example, loss of effective components is bigger, and alcohol consumption is big, big energy-consuming, cycle is long, causes production cost high.In addition, the compound red sage root preparation complicated component, mostly single Radix Salviae Miltiorrhizae or simple compound red sage root preparation were carried out ultrafiltration in the past, and it is few with ultrafiltration complicated red sage compound preparation to be carried out purified discussion, prepare compound red sage root preparation with ultrafiltration technology and still have a lot of industrialized concrete technical barriers that is difficult to, thereby seek the target that the ultrafiltration technology operating condition that is fit to suitability for industrialized production becomes people's effort.
Summary of the invention
The purpose of this invention is to provide the Chinese medicine preparation that contains Radix Salviae Miltiorrhizae that a kind of impurity is few, effective ingredient is high, it is to use the membrane ultrafiltration method to be prepared from, and has solved the difficult problem of suitability for industrialized production ultrafiltration technology condition operability.
The Chinese medicine preparation that the present invention contains Radix Salviae Miltiorrhizae is to be prepared from by following technical step:
(1) the Chinese medicine medical material that will contain Radix Salviae Miltiorrhizae is made extracting solution;
(2) predefecation is handled;
(3) ultrafiltration;
(4) ultrafiltrate concentrates, and is prepared into various preparations.
In the technology of the present invention step (1), the Chinese medicine medical material that contains Radix Salviae Miltiorrhizae is meant that needs are the medical material of respectively distinguishing the flavor of of monarch drug or ministerial drug with the Radix Salviae Miltiorrhizae through what extract hyperfiltration treatment, through extracting the flavour of a drug of hyperfiltration treatment, is generally 1～15 flavor medicine in needs, be preferably 1～10 flavor medicine, the best is 1～5 flavor medicine.Described Chinese medicine medical material both can have been distinguished extraction separately, also can kinds of traditional Chinese medicines medical material united extraction.Describedly make extracting solution through extraction, available general water or organic solvent or both mix Chinese medicine extracted and make it and get liquid, wherein organic solvent can be used the general conventional organic solvent of using, preferred alcohol organic solvent, the best is methanol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol.Carrying out next step predefecation after extracting solution can not concentrate or suitably concentrate handles.
In the above-mentioned technical step (2), described predefecation is handled available general material such as gauze, tiffany etc. carry out coarse filtration, 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 0.25～0.5kPa.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 0.1～0.2MPa.
(2) the feed liquid flow velocity is 1.0～4.0 meter per seconds, is preferably 2.0～3.0 meter per seconds.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 1.0～2.0 meter per seconds.
(3) feed high-pressure inert gas such as nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour～2 hours once, each 1 minute.
(4) feed temperature is 15～50 ℃, is preferably 20～40 ℃.
(5) 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.
(6) pH value of feed liquid is controlled at 5～9, is preferably 6.0～7.5;
(7) backwash condition: backwashing pressure is 1.5～2.5MPa, and backwashing period is that 0.5～1.5 hour, backwashing time are 1 minute～10 minutes.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 10～20 minutes, recoils 30 seconds～3 minutes.
(8) the Chemical cleaning cycle is 0.5 month～February, the Chemical cleaning medicament is generally diluted acid, diluted alkaline, surfactant, be preferably diluted alkaline, 0.5%～4.0% sodium hydroxide for example, the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite etc., pH value is 11, 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.
When flavour of a drug more for a long time, also can adopt 2～3 grades of ultrafiltrations, the molecular cut off of its one-level ultrafilter membrane, two-stage ultrafiltering film, three grades of ultrafilter membranes reduces successively.
In the technology of the present invention step (4), after ultrafiltrate concentrated, be prepared into various preparations more according to a conventional method.Can with the various dosage forms that are mixed and made into such as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, glycine for example of adjuvant on any or more than one pharmaceuticss, for example, can be made into injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule, microgranule, oral liquid etc.
The present invention contains the Chinese medicine preparation of Radix Salviae Miltiorrhizae, has following advantage:
(1) can dispel impurity in the Chinese medicine largely;
(2) can keep effective ingredient dramatically, effective.
(3) on the membrane ultrafiltration process, has very strong operability;
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
Raw material: Radix Salviae Miltiorrhizae 500g
Radix Salviae Miltiorrhizae powder is broken into coarse powder, adds deionized water heating extraction 3 times under 100 ℃ of slight boiling conditions, and 5.5 times of water heated 1 hour for the first time; Second and third time respectively adds 3 times of water gagings and heated respectively 0.5 hour.After extracting solution is 2 with 10% hydrochloric acid adjust pH, filter polyamide column on the filtrate (dried resin amount make a living dose 2/3).With the washing of 5 times of amount deionizations, continue with 0.1% sodium bicarbonate aqueous solution eluting, consumption is 5 times of column volume.After the eluent adjust pH is 5.5, be that 6000 cellulose diacetate film carries out ultrafiltration with molecular cut off, ultrafiltrate concentrates, lyophilization, the Radix Salviae Miltiorrhizae total phenolic acids lyophilized powder.
Cross flow filter is adopted in ultrafiltration, and its operating condition 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 2.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation 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 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 0.5% sodium hydroxide, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Embodiment two
Raw material: Radix Salviae Miltiorrhizae 300g, Cortex Moutan 150g
Adjuvant: Polyethylene Glycol-6000 180g
Radix Salviae Miltiorrhizae and Cortex Moutan are ground into coarse powder, decoct with water secondary, and each 2 hours, collecting decoction filtered, and it is 1.15 that filtrate decompression is concentrated into relative density, adds ethanol and makes medicinal liquid contain determining alcohol 75%, leaves standstill 10 hours.Getting the supernatant of medicinal liquid behind the precipitate with ethanol, is that 50000 three cellulose acetate membrane carries out ultrafiltration with this liquid molecular cut off, 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 0.25kPa.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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 2 hours 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 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10, 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 ℃), add Polyethylene Glycol-6000, evenly mixed, be heated to 60 ℃ of temperature, change material after 60 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In medicine liquid droplet to the 8 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment three
Raw material: Radix Salviae Miltiorrhizae 410g, Radix Notoginseng 80g, Borneolum Syntheticum 4.6g
Adjuvant: Polyethylene Glycol-6000 180g
Learn from else's experience the Radix Salviae Miltiorrhizae, pseudo-ginseng of coarse pulverization to extraction pot, add 5 times of water gagings, decocted 2 hours, filter, filtering residue carries out second time and extracts, and adds 4 times of water gagings, decocted 1 hour, and filtration, filtering residue discards, merging filtrate.Filtrate decompression is concentrated into medicine liquid volume (L) and medical material weight (Kg) than being 1: 1, slowly adds 95% ethanol, makes medicinal liquid contain determining alcohol 70%, leaves standstill 12 hours.Getting the supernatant of medicinal liquid behind the precipitate with ethanol, is that 40000 polysulfone membrane is carried out ultrafiltration with this liquid molecular cut off, 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 0.4kPa.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 0.15MPa.The feed liquid flow velocity is 3.0 meter per seconds, 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 2.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 2 hours the ventilation once, each 1 minute.Feed temperature is 40 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 8.0.Backwashing pressure is 2.0MPa, and backwashing period is that 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10, 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 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 65 ℃ of temperature, change material after 60 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 is mixed.In medicine liquid droplet to the 8 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment four
Raw material: Radix Salviae Miltiorrhizae 350g, Rhizoma Chuanxiong 160g, Styrax 5.2g
Adjuvant: Polyethylene Glycol-6000 200g
Rhizoma Chuanxiong extracts volatile oil, adds 0.5% HP-aqueous solution in the Rhizoma Chuanxiong volatile oil, and stirring and dissolving filters, and makes inclusion complex in solution, and is standby; Residue and Radix Salviae Miltiorrhizae that Rhizoma Chuanxiong extracts behind the volatile oil add 5 times of water gagings, decoct 2 hours, filter, and 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 decompression is concentrated into medicine liquid volume (L) and medical material weight (Kg) than being 1: 1, slowly adds 95% ethanol, makes medicinal liquid contain determining alcohol 70%, leaves standstill the leaching supernatant 12 hours.Filtrate is that 20000 sulfonated polysulfone membrane 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 0.25MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.35kPa.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 1.0 meter per seconds, in the ultra-filtration process, adopts the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, and the flow speed wave moment is 1.0 meter per seconds.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/12, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 2.0% sodium hydroxide solution, and pH value is 11, 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 (55 ℃).Get extractum and Styrax, evenly be heated to 60 ℃ of temperature, change material after 70 minutes, move in the dropping-pill machine jar that jar temperature remains on 85 ℃ with Polyethylene Glycol-6000 is mixed.In medicine liquid droplet to the 7 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment five
Raw material: Radix Salviae Miltiorrhizae 350g, Rhizoma Chuanxiong 160g, Borneolum Syntheticum 4.6g
Adjuvant: Polyethylene Glycol-6000 210g
Rhizoma Chuanxiong extracts volatile oil, adds 0.5% HP-aqueous solution in the Rhizoma Chuanxiong volatile oil, and stirring and dissolving filters, and makes inclusion complex in solution, and is standby; Residue and Radix Salviae Miltiorrhizae that Rhizoma Chuanxiong extracts behind the volatile oil add 5 times of water gagings, decoct 2 hours, filter, and filtering residue carries out the second time and extracts, and adds 4 times of water gagings, decocts 1 hour, and merge extractive liquid, filters.Filtrate is that 30000 poly-mystery sulfone 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 0.4MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25kPa.The feed liquid flow velocity is 3.0 meter per seconds, 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 2.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 2 hours the ventilation once, each 1 minute.Feed temperature is 30 ℃, when feed liquid stock solution is concentrated 1/10, 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 1.5MPa, and backwashing period is that 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, 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 1.36 (55 ℃), get extractum and Borneolum Syntheticum, evenly mixed with Polyethylene Glycol-6000, be heated to 85 ℃ of temperature, change material after 50 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In medicine liquid droplet to the 8 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
The active constituent content of test example 1 different process method relatively
(1) process:
Among water extraction: the embodiment five without the method for ultrafiltration, the Radix Salviae Miltiorrhizae of the coarse pulverization of promptly learning from else's experience, Rhizoma Chuanxiong extract residue behind the volatile oil to extraction pot, add 5 times of water gagings, decoct 2 hours, filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, decocted 1 hour, merge extractive liquid, filters; Filtrate is concentrated into the extractum that relative density is 1.36 (55 ℃).
Among decoction and alcohol sedimentation technique: the embodiment four without the method for ultrafiltration, the Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong of coarse pulverization of promptly learning from else's experience extracts residue behind the volatile oil to 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; Filtrate decompression is concentrated into medicine liquid volume (L) and medical material weight (Kg) than being 1: 1, slowly adds 95% ethanol, makes medicinal liquid contain determining alcohol 70%, leaves standstill the leaching supernatant 12 hours; Filtrate is concentrated into the extractum that relative density is 1.36 (55 ℃).
3. water is put forward ultrafiltration: water is put forward the method for ultrafiltration among the embodiment five, and ultrafiltrate concentrates and obtains the extractum that relative density is 1.36 (55 ℃).
(2) comparison of the component content of different process method
1. danshensu assay method: referring to " content of danshensu, protocatechualdehyde and red intoxicated sour B in the rp-hplc determination Radix Salviae Miltiorrhizae extract " (pharmaceutical analysis magazine, 2003,23 (6): 457～458) such as Zhang Wenshengs
2. result: the extract weight of water extraction is bigger, and the loss of effective components of decoction and alcohol sedimentation technique is bigger; And ultrafiltration can effectively reduce the content of extract, again can be active constituent-enriched effectively, and be the little and good process method of active drug of preparation dosage.See Table 1.
Table 1
The clinical observation of experimental example 2 medicines of the present invention (medicine of embodiment five) treatment angina pectoris
1 data and method
1.1 case is selected among the 100 routine angina pectoris patients, male 65 examples, and women 35 examples, 35～55 years old 32 age example, 56～70 years old 68 example, 50.2 years old mean age, the course of disease 2.6 years, wherein with hyperpietic's 43 examples, type 2 diabetes mellitus 7 examples.All patients all meet name and the standard of WTO about the ischemic heart desease diagnosis, wherein stable angina pectoris 48 row, unstable angina 52 examples.Be divided into treatment group and matched group at random, every group 50 example, two groups of sexes, medical history, age no significant difference.
1.2 removing, knot prescription method is associated with protopathy (hypertension, the conventional depressor of using), diabetes (routine is kept on a diet and used antidiabetic drug).Other treatment medicaments for coronary disease in principle requires to stop using during all MethodsThe cases enrolled treatments.The treatment group gives oral medicine of the present invention, and each 10, every day 3 times, sublingual administration nitroglycerin in case of necessity.Matched group gives FUFANG DANSHEN PIAN, and each 3, every day 3 times, sublingual administration nitroglycerin in case of necessity.4 weeks of the course of treatment.
1.3 observed content is inquired clinical symptoms and untoward reaction before and after taking Radix Salviae Miltiorrhizae drop pill.Recording blood pressure is done conventional 12 lead electrocardiogram and blood, routine urinalysis, hepatic and renal function detection.
1.4 efficacy assessment standard is evaluated according to bureau of drug administration of Ministry of Health of the People's Republic of China specified " cardiovascular medicament clinical research guideline ".The symptom efficacy assessment standard: produce effects, equal work capacity do not cause that angina pectoris attacks or attack times reduce more than 70%, and general activity does not have symptom uncomfortable in chest; Effectively, angina pectoris attacks number of times, sx uncomfortable in chest 50% ~ 70%; Invalid, above situation does not have significant change after the medication.The ECG curative effect evaluation criteria: produce effects, the performance of resting electrocardiogram ischemia recovers normal; Effectively, the resting electrocardiogram ischemic ST descends, and more than the treatment back rise 1mm, but abnormal, lower wall and left chest lead negative T wave shoal and reach more than the 1mm; Invalid, resting electrocardiogram is preceding basic identical with treatment.
2 results
2.1 treatment group and matched group curative effect relatively see Table 2, table 3.
Table 2 Drug therapy angina pectoris symptom of the present invention curative effect and matched group are relatively
Table 3 Drug therapy angina pectoris of the present invention ECG curative effect and matched group are relatively
Embodiment six
Raw material: Radix Salviae Miltiorrhizae 500g, Radix Notoginseng 100g, Styrax 5g
Adjuvant Polyethylene Glycol-6000 200g
Learn from else's experience the Radix Salviae Miltiorrhizae, pseudo-ginseng of coarse pulverization to extraction pot, add the 0.75g sodium bicarbonate, add 4 times of water gagings, decocted 2 hours, filter, filtering residue carries out the extraction second time, adds 4 times of water gagings, decocts 1 hour; Add chitosan flocculant in the extracting solution, left standstill 12 hours, filter.Filtrate is that 20000 sulfonated polyether sulfone 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 0.3MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.3kPa.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 2.0 meter per seconds, in the ultra-filtration process, adopts the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, and the flow speed wave moment is 1.0 meter per seconds.Feed temperature is 45 ℃, when feed liquid stock solution is concentrated 1/11, 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 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is 1.5% sodium hydroxide solution, and pH value is 10, 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 (55 ℃), get extractum and Styrax, evenly mixed with Polyethylene Glycol-6000, be heated to 85 ℃ of temperature, change material after 40 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In medicine liquid droplet to the 7 ℃ methyl-silicone oil, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment seven
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Paeoniae Rubra 141g, Borneolum Syntheticum 8g.
Adjuvant: Polyethylene Glycol-6000 200g
With 60% ethanol heating extraction Radix Salviae Miltiorrhizae and Radix Paeoniae Rubra 2 times, each 2 hours, merge extractive liquid, divided behind the high speed centrifugation and gets supernatant.With the supernatant molecular cut off is that 30000 polysulfonamides film carries out ultrafiltration, and filter type adopts dead-end filtration.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.3MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.25kPa.The feed liquid flow velocity is 3.0 meter per seconds, 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 2.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 2 hours the ventilation once, each 1 minute.Feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/14, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 8.0.Backwashing pressure is 2.0MPa, and backwashing period is that 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 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 1.37 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 60 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 is mixed.In medicine liquid droplet to the 8 ℃ methyl-silicone oil, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment eight
Raw material: Radix Salviae Miltiorrhizae 200g, Radix Notoginseng 200g, Lignum Dalbergiae Odoriferae oil 1.75ml
Raw material: magnesium stearate, starch
Learn from else's experience Radix Salviae Miltiorrhizae, the pseudo-ginseng of coarse pulverization add 4 times of water gagings, decoct 2 hours, filter, and filtering residue carries out extraction second time, adds 4 times of water gagings, decocts 1 hour; Add the ZTC1+1 natural clarifying agent in the extracting solution, mixing leaves standstill 12 hours, and is centrifugal, gets supernatant.The supernatant molecular cut off is that 40000 polyacrylonitrile film carries out ultrafiltration, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, 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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, 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 1.32～1.40 (55 ℃),, be pressed into tablet this extractum and Lignum Dalbergiae Odoriferae oil and an amount of magnesium stearate and starch mix homogeneously.
Embodiment nine
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g, Flos Carthami 50g
Adjuvant: Macrogol 4000 80g, Polyethylene Glycol 8000 130g
Extract Radix Salviae Miltiorrhizae, Radix Notoginseng and Flos Carthami 2 times with 70% ethanol heating (90 ℃), each 2 hours, merge extractive liquid, carried out microfiltration with ceramic membrane, collected filtrate.Filtrate is that 10000 cyanoethyl cellulose film carries 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 4.0 meter per seconds, in the ultra-filtration process, adopts the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, and the flow speed wave moment is 2.0 meter per seconds.Feed temperature is 50 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 9.Backwashing pressure is 2.0MPa, and backwashing period is that 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is 1.5% sodium hydroxide solution, and pH value is 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 (55 ℃).Get extractum and Borneolum Syntheticum, evenly mixed with Macrogol 4000 and Polyethylene Glycol 8000, be heated to 85 ℃ of temperature, change material after 40 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In medicine liquid droplet to the 6 ℃ methyl-silicone oil, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment ten
Raw material: Radix Salviae Miltiorrhizae 110g, Radix Notoginseng 30g, Radix Astragali 430g, Lignum Dalbergiae Odoriferae 100g
Adjuvant: Polyethylene Glycol-6000 180g
Get Lignum Dalbergiae Odoriferae, add 5 times of water gagings, reflux, extract, 5 hours is collected volatile oil, and is standby; To decoct with water 2 times through the Radix Astragali, Radix Salviae Miltiorrhizae, the Radix Notoginseng of pulverizing, add 7 times of water gagings at every turn, each 2 hours, merge decoction liquor, filter, filtrate is concentrated into 900ml, adds 95% ethanol, makes determining alcohol reach 70%, leaves standstill 24 hours, filters.Filtrate is that 20000 polysulfone membrane is carried 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 0.35MPa, 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 4.0 meter per seconds, 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 2.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 2 hours the ventilation once, each 1 minute.Feed temperature is 50 ℃, 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 9.Backwashing pressure is 2.0MPa, and backwashing period is that 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, 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 (55 ℃), get extractum, evenly mixed with Polyethylene Glycol-6000, be heated to 60 ℃ of temperature, add volatile oil of Lignum Dalbergiae Odoriferae, change material after 70 minutes, move in the dropping-pill machine jar that jar temperature remains on 85 ℃.In medicine liquid droplet to the 5 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment 11
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g, Radix Codonopsis 100g
Adjuvant: Polyethylene Glycol-6000 200g
With 70% ethanol heating extraction Radix Salviae Miltiorrhizae, Radix Notoginseng, Radix Codonopsis 2 times, each 2 hours, merge extractive liquid, carried out microfiltration with ceramic membrane, collected filtrate.Filtrate is that 50000 polysulfonamides 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 0.35MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.30kPa.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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 2 hours 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 1.5 hours, backwashing time are 10 minutes.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, works 20 minutes, recoils 3 minutes.The Chemical cleaning cycle is 2 months, and the Chemical cleaning medicament is 2% sodium hydroxide solution, and pH value is 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 1.37 (55 ℃).Get extractum and Borneolum Syntheticum, evenly be heated to 60 ℃ of temperature, change material after 50 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃ with Polyethylene Glycol-6000 is mixed.In medicine liquid droplet to the 6 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment 12
Raw material: Semen Ziziphi Spinosae (stir-fry) 250g, Radix Salviae Miltiorrhizae 50g, Fructus Schisandrae Chinensis (processed with vinegar) 50g
Adjuvant: dextrin
Semen Ziziphi Spinosae (stir-fry), Radix Salviae Miltiorrhizae, Fructus Schisandrae Chinensis powder are broken into coarse powder, add water supersound extraction secondary, and each 40 minutes, merge extractive liquid, added 101 fruit juice clarifiers, left standstill 12 hours, got supernatant.The supernatant molecular cut off is that 10000 polyimide film carries out ultrafiltration, and filter type adopts cross flow filter.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 0.5kPa.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 0.2MPa.The feed liquid flow velocity is 2.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 4.0% sodium hydroxide solution, and pH value is 10, 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 1.1.15 (20 ℃).1 part of qinghuo reagent, 1 part in dextrin, mixing is sprayed into granule, drying, promptly.
Embodiment 13
Raw material: Radix Salviae Miltiorrhizae 500g, Rhizoma Chuanxiong 500g, Radix Puerariae 500g
Adjuvant: cane sugar powder is an amount of
Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, powder of Radix Puerariae are broken into coarse powder, decoct with water secondary, and 1.5 hours for the first time, 1 hour collecting decoction for the second time, extracting solution filters with gauze.Filtrate is that methyl methacrylate～acrylonitrile copolymer film of 9000 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 0.5MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.5kPa.The feed liquid flow velocity is 3.0 meter per seconds, 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 2.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/12, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.08 that described ultrafiltrate is concentrated into relative density, filters while hot, and it is 1.40 clear paste that filtrate is concentrated into relative density, and it is an amount of to add cane sugar powder, makes granule, and 1000g is made in cold drying, promptly.
Embodiment 14
Raw material: Radix Astragali 350g, Ramulus Cinnamomi 150g, Radix Salviae Miltiorrhizae 250g, Radix Puerariae 250g
Adjuvant: sodium benzoate 3g
The Ramulus Cinnamomi distillation extracts volatile oil, and the aqueous solution behind distillation device is in addition collected; The medicinal residues and the Radix Astragali, Radix Salviae Miltiorrhizae, Radix Puerariae decoct with water three times, and each 2 hours, collecting decoction filtered, and filtrate merges with above-mentioned aqueous solution, filter, and filtrate is that 10000 cellulose diacetate film carries out ultrafiltration, filter type employing cross flow filter with molecular cut off.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 0.25kPa.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 0.1MPa.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 0.5% sodium hydroxide solution, and pH value is 11, and cleaning pressure is 0.1MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is suitably concentrated, add sodium benzoate 3g, put coldly, add Ramulus Cinnamomi Volatile oil, add water to 1000ml, stir evenly, promptly.
Embodiment 15
Raw material: Fructus Crataegi 270g, Radix Salviae Miltiorrhizae 200g, Radix Puerariae 300g, Radix Notoginseng 90g, Radix Aucklandiae 50g
Raw material: lactose
Fructus Crataegi, Radix Salviae Miltiorrhizae, Radix Puerariae, Radix Notoginseng, Radix Aucklandiae powder are broken into coarse powder, decoct with water three times, and each 1.5 hours, collecting decoction added the Ovum Gallus domesticus album flocculating agent, and essence is put 12 hours, and is centrifugal, gets supernatant; The supernatant molecular cut off is that 20000 cellulose diacetate film carries out ultrafiltration, 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 0.25kPa.The feed liquid flow velocity is 2.0 meter per seconds, in the ultra-filtration process, adopts the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, and the flow speed wave moment is 1.0 meter per seconds.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.20 clear paste that described ultrafiltrate is concentrated into relative density, and with the lactose fluidisation, drying is made granule 1000g, promptly in the batch (-type) fluid bed.
Embodiment 16
Raw material: Radix Salviae Miltiorrhizae 300g, Radix Angelicae Sinensis 150g, Fructus Aurantii 150g, Radix Notoginseng 200g, Rhizoma Zingiberis Recens 300g
Adjuvant: magnesium stearate and xylitol are an amount of
Radix Salviae Miltiorrhizae, Radix Angelicae Sinensis, Fructus Aurantii, Radix Notoginseng powder are broken into coarse powder, and Rhizoma Zingiberis Recens is thinly sliced, and add 50% ethanol ultrasonic extraction 2 times, and each 60 minutes, merge extractive liquid, filtered.Filtrate is that 70000 three cellulose acetate membrane 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 0.3kPa.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/11, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 4.0% sodium hydroxide, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is concentrated, be dried to dry extract, be ground into fine powder, add magnesium stearate and xylitol, mixing is made granule, and drying is pressed into 1000, sugar coating, promptly.
Embodiment 17
Raw material: Radix Paeoniae Rubra 335.4g, Radix Salviae Miltiorrhizae 670.8g, Lignum Dalbergiae Odoriferae 223.6g, Flos Carthami 335.4g, Rhizoma Chuanxiong 335.4g
Adjuvant: Icing Sugar, dextrin
Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae decoct with water twice, and 2 hours for the first time, 1 hour for the second time, decocting liquid filtered, and merging filtrate is standby; Cataclasm Lignum Dalbergiae Odoriferae and Rhizoma Chuanxiong extract volatile oil, use dissolve with ethanol, and standby, residue decocts with water 2 hours, and decocting liquid filters, and is standby; Flos Carthami adds water temperature and soaks twice, and 2 hours for the first time, 1 hour for the second time, merge immersion, filter, standby; Above-mentioned each filtrate is merged, and is that 20000 sulfonated polysulfone membrane carries out ultrafiltration, filter type employing cross flow filter with molecular cut off.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.25MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.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 0.15MPa.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 20 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 10, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.30 thick paste that described ultrafiltrate is condensed into relative density, gets 1 part of thick paste, 2.1 parts of Icing Sugar, and 0.7 part in dextrin, mixing, alcohol granulation, drying sprays into volatile oil, and granulate is made 1000 bags, promptly.
Embodiment 18
Raw material: Radix Salviae Miltiorrhizae 200g, Radix Paeoniae Alba 2000g, Radix Et Caulis Acanthopanacis Senticosi 1000g, Radix Curcumae 300g, Fructus Crataegi 2000g
Adjuvant: microcrystalline Cellulose
Fructus Crataegi is extracted secondary with alcohol heating reflux, and each 2 hours, merge extractive liquid,, standby; Radix Salviae Miltiorrhizae, the Radix Paeoniae Alba, Radix Et Caulis Acanthopanacis Senticosi, Radix Curcumae decoct with water secondary, and each 2 hours, collecting decoction filtered, and filtrate is concentrated into relative density to 1.20, and add ethanol and make pure content reach 70%, standing over night, the leaching supernatant merges with above-mentioned hawthorn extract, filters.Filtrate is that 10000 polysulfonamides 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 0.3MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.The feed liquid flow velocity is 3.0 meter per seconds, in the ultra-filtration process, adopts the fluctuation of periodicity flow so that produce pulsating flow or non-stationary flow in membrane channels, and the flow speed wave moment is 1.0 meter per seconds.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/12, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is reclaimed ethanol, be condensed into thick paste, add an amount of microcrystalline Cellulose, granulate, be pressed into 1000, promptly.
Embodiment 19
Raw material: Radix Notoginseng 134g, Rhizoma Chuanxiong 335g, Flos Carthami 134g, Radix Salviae Miltiorrhizae 67g, Rhizoma Alismatis 67g, Radix Et Caulis Acanthopanacis Senticosi extractum powder 31g
Adjuvant: Pulvis Talci is an amount of
Rhizoma Chuanxiong extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Medicinal residues and Flos Carthami, Radix Salviae Miltiorrhizae, Rhizoma Alismatis, Radix Notoginseng decoct with water secondary, and 3 hours for the first time, 2 hours collecting decoctions filtered for the second time, and the aqueous solution after filtrate and the distillation merges.The amalgamation liquid molecular cut off is that 30000 poly (ether sulfone) film carries out ultrafiltration, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, 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 0.2MPa.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 3.0% sodium hydroxide solution, 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 is condensed into extractum, and drying is pulverized, and adds an amount of Pulvis Talci, with the Radix Et Caulis Acanthopanacis Senticosi extractum powder mixing, sprays into Rhizoma Chuanxiong volatile oil, mixing, and airtight 2 hours, incapsulate, make 500, promptly.
Embodiment 20
Raw material: Radix Salviae Miltiorrhizae 250g, Radix Notoginseng 200g, Borneolum Syntheticum 50g, TENGHEHUAN 1000g, Radix Aucklandiae 200g, Styrax 50g
Adjuvant: Polyethylene Glycol-6000
Radix Salviae Miltiorrhizae, Radix Notoginseng, TENGHEHUAN, Radix Aucklandiae powder are broken into coarse powder, decoct with water secondary, each 2 hours, filter merging filtrate.Filtrate is that 50000 polyvinylidene fluoride 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 0.35MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 45 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is concentrated into the extractum of relative density 1.30 (55 ℃), adds Borneolum Syntheticum and Styrax, evenly mixed with Polyethylene Glycol-6000, be heated to 60 ℃ of temperature, change material after 80 minutes, move in the dropping-pill machine jar that jar temperature remains on 90 ℃.In medicine liquid droplet to the 5 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment 21
Raw material: Radix Salviae Miltiorrhizae 500g, Rhizoma Chuanxiong 250g, Radix Paeoniae Rubra 250g, Flos Carthami 250g, Rhizoma Cyperi 125g, Radix Aucklandiae 125g, Fructus Crataegi 60g
Adjuvant: lactose is an amount of
More than seven flavors, decoct with water three times, each 1 hour, collecting decoction filtered.Filtrate is carried out two-stage ultrafiltering, and the first order is that molecular cut off is 80000 polyacrylonitrile film, and the second level is that molecular cut off is 10000 polyacrylonitrile film, and filter type adopts cross flow filter.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 0.4kPa.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.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 5.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 3.0% sodium hydroxide solution, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.20 clear paste that described ultrafiltrate is concentrated into relative density, and with the lactose fluidisation, drying is made granule 1000g, promptly in the batch (-type) fluid bed.
Embodiment 22
Raw material: Radix Ginseng 180g, Radix Ophiopogonis 180g, Fructus Schisandrae Chinensis (processed with vinegar) 60g, Radix Salviae Miltiorrhizae 300g, Radix Paeoniae Rubra 240g, Radix Curcumae 200g, Radix Notoginseng powder 60g
Adjuvant: lactose
More than seven flavors, decoct with water three times, each 1 hour, collecting decoction adds the flocculate with chitosan clarifier, leaves standstill 24 hours, and was centrifugal, gets supernatant.The supernatant molecular cut off is that 30000 sulfonated polyether sulfone film carries 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 0.3kPa.The feed liquid flow velocity is 2.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 45 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.20 clear paste that described ultrafiltrate is concentrated into relative density, and with the lactose fluidisation, drying is made granule 1000g, promptly in the batch (-type) fluid bed.
Embodiment 23
Raw material: Radix Salviae Miltiorrhizae 300g, Flos Sophorae 150g, Rhizoma Chuanxiong 150g, Radix Notoginseng 54g, Flos Carthami 150g, Lignum Dalbergiae Odoriferae 150g, Radix Paeoniae Rubra 150g
Adjuvant: hydroxypropyl methylcellulose
Rhizoma Chuanxiong, Flos Carthami, Lignum Dalbergiae Odoriferae extract volatile oil respectively, use dissolve with ethanol, and be standby; Its residue and Radix Salviae Miltiorrhizae, Flos Sophorae, Radix Notoginseng, Radix Paeoniae Rubra decoct with water three times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrate is that 50000 three cellulose acetate membrane 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 0.35MPa, 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 0.15MPa.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/10, 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 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 4.0% sodium hydroxide solution, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into cream, and drying is pulverized, and sieves, and it is an amount of to add hydroxypropyl methylcellulose, adds volatile oil such as Rhizoma Chuanxiong, Flos Carthami, Lignum Dalbergiae Odoriferae, and mixing is made granule, is pressed into 1000, sugar coating, promptly.
Embodiment 24
Raw material: Rhizoma Chuanxiong 400g, Radix Polygoni Multiflori Preparata 534g, Rhizoma Polygonati (system) 534g, Flos Carthami 400g, Herba Epimedii 400g, Oletum Trogopterori (vinegar system) 267g, Radix Salviae Miltiorrhizae 400g
Adjuvant: magnesium stearate is an amount of
More than seven flavors, decoct with water three times, 3 hours for the first time, second and third time each 1 hour, collecting decoction filters, filtrate is concentrated into relative density and is about 1.24, adds ethanol and makes and contain the alcohol amount and reach 50%, leaves standstill the leaching supernatant.The supernatant molecular cut off is that 30000 polyvinylidene fluoride film carries out ultrafiltration, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.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.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 3.0% sodium hydroxide solution, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into cream, and drying is pulverized, and sieves, and it is an amount of to add magnesium stearate, and mixing is made granule, and drying is pressed into 1000, sugar coating, promptly.
Embodiment 25
Raw material: Radix Et Caulis Acanthopanacis Senticosi 225g, Radix Polygoni Multiflori Preparata 195g, Rhizoma Alismatis 195g, Radix Astragali 175g, Radix Ginseng 35g, Rhizoma Acori Graminei 60g, Radix Salviae Miltiorrhizae 170g, Radix Notoginseng 60g
Adjuvant: magnesium stearate and micropowder silica gel are an amount of
More than eight flavors, add 70% ethanol ultrasonic extraction 2 times, each 1 hour, merge extractive liquid, filtered.Filtrate is carried out two-stage ultrafiltering, and the first order is that molecular cut off is 70000 polysulfone membrane, and the second level is that molecular cut off is 10000 cellulose diacetate film, and filter type adopts cross flow filter.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 0.35kPa.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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into cream, and drying is pulverized, and sieves, and adds magnesium stearate and micropowder silica gel is an amount of, and mixing is made granule, and drying is pressed into 1000, sugar coating, promptly.
Embodiment 26
Raw material: Radix Salviae Miltiorrhizae 732g, Radix Notoginseng 141.6g, Borneolum Syntheticum 1.22g, Pulvis Cornus Bubali Concentratus 47.2g, Venenum Bufonis 0.79g, Flos Carthami 48.4g, Calculus Bovis 6.3g, Leptoradix Ginseng 94.4g
Adjuvant: lactose is an amount of
Radix Salviae Miltiorrhizae, Leptoradix Ginseng, Radix Notoginseng, Flos Carthami add hot water extraction 2 times, and each 2 hours, merge extractive liquid, filtered.Filtrate is that 8000 sulfonated polysulfone membrane 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 0.5MPa, 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 1.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 15 ℃, when feed liquid stock solution is concentrated 1/13, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into cream, and drying is ground into fine powder, sieves, and is even with Calculus Bovis, Pulvis Cornus Bubali Concentratus, Venenum Bufonis, Borneolum Syntheticum, lactose mixed grinding again, incapsulates, and makes 1000, promptly.
Embodiment 27
Raw material: Fructus Crataegi 300g, Radix Polygoni Multiflori Preparata 430g, Radix Salviae Miltiorrhizae 430g, Radix Puerariae 177g, Fructus Trichosanthis 517g, Semen Cassiae 430g, aluminum clofibrate 50g, vitamin C 20g
Powder of Radix Puerariae is broken into coarse powder, adds 5 times of amount alcohol heating reflux and extracts twice, and each 4 hours, merge extractive liquid, filtered filtrate for later use; Fructus Crataegi, Radix Polygoni Multiflori, Radix Salviae Miltiorrhizae, Fructus Trichosanthis, Semen Cassiae decoct with water three times, and each 1.5 hours, collecting decoction filtered, the ratio that filtrate is concentrated into the crude drug amount is 1: 1, puts coldly, adds ethanol and makes it contain the alcohol amount to reach 70%, stir evenly, placed 48 hours, and filtered, filtrate and above-mentioned Radix Puerariae extracting solution merge.Filtrate is that 20000 polysulfone membrane is carried 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 0.3MPa, 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.Feed temperature is 35 ℃, 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 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is concentrated into the thick paste shape, drying under reduced pressure, gained dry extract and aluminum clofibrate pulverize separately sieve, and mixing is made granule, and drying adds vitamin C, and mixing is pressed into 1000, sugar coating, promptly.
Embodiment 28
Raw material: Rhizoma Chuanxiong 100g, Rhizoma Ligustici 60g, Herba Asari 30g, Radix Angelicae Dahuricae 100g, Pulvis Cornus Bubali Concentratus 10g, Radix Salviae Miltiorrhizae 100g, Radix Puerariae 100g, Rhizoma Gastrodiae (processed with Rhizoma Zingiberis Recens) 100g, Ramulus Uncariae Cum Uncis 100g
Rhizoma Chuanxiong, Herba Asari extract volatile oil, and its residue and Rhizoma Ligustici, the Radix Angelicae Dahuricae, Radix Salviae Miltiorrhizae, Radix Puerariae, Ramulus Uncariae Cum Uncis decoct with water three times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrate is that 20000 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 0.35MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.3kPa.The ultrafiltration initial stage is adopted lower pressure, slowly boosts then.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 2 times again, and the pH value of feed liquid is controlled at 6.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 11, 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 1.32～1.40 (55 ℃), mixes with Pulvis Cornus Bubali Concentratus, Rhizoma Gastrodiae fine powder, spray into Rhizoma Chuanxiong, Herba Asari extraction volatile oil, mixing incapsulates.
Embodiment 29
Raw material: Radix Angelicae Sinensis 185g, Semen Cassiae 185g, Ramulus Uncariae Cum Uncis 125g, Radix Achyranthis Bidentatae 125g, Radix Salviae Miltiorrhizae 100g, Radix Puerariae 100g, Flos Sophorae 100g, Radix Ilicis Pubescentis 100g, Spica Prunellae 100g, Radix Notoginseng 60g
Adjuvant: magnesium stearate and lactose are an amount of
Flos Sophorae decocts with water after boil, and transfers pH to 8.5 with lime cream, decocts secondary again, filters, and merging filtrate is transferred pH to 4.5～5.4 with hydrochloric acid, after the cooling, and the leaching precipitation, drying is ground into fine powder.All the other Radix Angelicae Sinensis etc. nine flavor decocts with water secondary, filters, and merging filtrate is concentrated in right amount, adds ethanol and makes that to contain the alcohol amount be 70%, leaves standstill 24 hours, filters.Filtrate is carried out two-stage ultrafiltering, and first order molecular cut off is 70000 cellulose diacetate film, and the second level is 10000 cellulose diacetate film with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, 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.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 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into thick paste, and thick paste and above-mentioned Flos Sophorae fine powder, magnesium stearate and lactose mixing are made granule, and drying is pressed into 1000, sugar coating, promptly.
Embodiment 30
Raw material: Radix Salviae Miltiorrhizae 100g, Rhizoma Chuanxiong 100g, Radix Paeoniae Rubra 200g, Flos Carthami 80g, Radix Angelicae Sinensis 80g, Radix Pseudostellariae 80g, Bulbus Allii Macrostemonis 80g, Pericarpium Trichosanthis 80g, Radix Polygalae (Radix Glycyrrhizae system) 60g, Lignum Dalbergiae Odoriferae 60g, Rhizoma Acori Graminei 60g, Radix Glycyrrhizae (processed with honey) 60g
Adjuvant: microcrystalline Cellulose is an amount of
Flos Carthami is with 75 ℃ of warm water immersion secondaries, and each 2 hours, merge immersion, immersion is standby; Lignum Dalbergiae Odoriferae and Rhizoma Chuanxiong extract volatile oil, and its residue and Radix Salviae Miltiorrhizae, Radix Paeoniae Rubra, Radix Angelicae Sinensis, Radix Pseudostellariae, Bulbus Allii Macrostemonis, Pericarpium Trichosanthis, Radix Polygalae, Rhizoma Acori Graminei, Radix Glycyrrhizae decoct with water secondary, and each 3 hours, merge with above-mentioned Flos Carthami immersion, filter.Filtrate is carried out two-stage ultrafiltering, and first order molecular cut off is 80000 polyvinylidene fluoride film, and the second level is 10000 cellulose diacetate film with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.3kPa.The feed liquid flow velocity is 2.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 3% sodium hydroxide solution, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
It is 1.40 thick paste that described ultrafiltrate is concentrated into relative density, mixing, and drying is pulverized, and sieves and makes granule, adds microcrystalline Cellulose, sprays into Lignum Dalbergiae Odoriferae and Rhizoma Chuanxiong volatile oil, and mixing is pressed into 1000, sugar coating, promptly.
The embodiment hentriaconta-
Raw material: Radix Astragali 150g, Radix Codonopsis 80g, Radix Ophiopogonis 80g, Radix Polygoni Multiflori 60g, Herba Epimedii 100g, Radix Puerariae 120g, Radix Angelicae Sinensis 80g, Radix Salviae Miltiorrhizae 100g, Spina Gleditsiae 60g, Sargassum 60g, Thallus Laminariae (Thallus Eckloniae) 60g, Concha Ostreae 60g, Fructus Aurantii Immaturus 50g
Adjuvant: simple syrup 150g
Get Radix Puerariae, Radix Salviae Miltiorrhizae, heating and refluxing extraction secondary in 70% ethanol each 1 hour, merges ethanol extract; The medicinal residues behind the ethanol extraction and the Radix Astragali etc. ten are decocted with water secondary simply, 2 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate is concentrated into 1500ml, merges ethanol extract and aqueous extract, add ethanol and make and contain alcohol amount and reach 65%, cold preservation 48 hours filters.Filtrate is carried out two-stage ultrafiltering, and first order molecular cut off is 70000 sulfonated polysulfone membrane, and the second level is 10000 cellulose diacetate film 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.Feed temperature is 30 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is concentrated into 1300ml, adds simple syrup, regulate pH value to 7.0, add water to 1500ml, stir evenly, filter with 10% sodium hydroxide solution, embedding, sterilization, promptly.
Embodiment 32
Raw material: Radix Salviae Miltiorrhizae 112.5g, Myrrha (stir-fry) 25.5g, Caulis Spatholobi 112.5g, Sanguis Draxonis 25.5g, Rhizoma Corydalis (vinegar system) 45g, Radix Angelicae Sinensis 45g, Radix Curcumae 45g, Radix Polygoni Multiflori Preparata 75g, Semen Persicae (stir-fry) 30g, Rhizoma Polygonati (steaming) 75g, Flos Carthami 30g, Radix Puerariae 112.5g, Olibanum (stir-fry) 25.5g, Borneolum Syntheticum 4.5g
Radix Puerariae, Rhizoma Corydalis, Flos Carthami add 70% ethanol heating extraction 2 times, and each 2 hours, extracting solution was standby; Radix Salviae Miltiorrhizae, Caulis Spatholobi, Radix Angelicae Sinensis, Radix Curcumae, Radix Polygoni Multiflori, Semen Persicae, Rhizoma Polygonati decoct with water secondary, and 3 hours for the first time, 2 hours for the second time, filter, filtrate adds ethanol to be made and adds ethanol and make and contain the alcohol amount and reach 65%, leaves standstill 24 hours, the leaching supernatant, extracting solution such as supernatant and Radix Puerariae merge.Amalgamation liquid carries out two-stage ultrafiltering, and first order molecular cut off is 70000 cellulose diacetate film, and the second level is 8000 sulfonated polysulfone membrane with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.The feed liquid flow velocity is 1.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 35 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into thick paste, mixes with Myrrha, Sanguis Draxonis, Olibanum fine powder, drying is ground into fine powder, sieves, and mixing is made granule, and drying adds Borneolum Syntheticum, and mixing is pressed into 1000, sugar coating, promptly.
Embodiment 33
Raw material: Radix Salviae Miltiorrhizae 80g, Radix Paeoniae Rubra 60g, Radix Polygoni Multiflori Preparata 60g, Fructus Lycii 60g, Radix Puerariae 60g, Rhizoma Chuanxiong 60g, Flos Carthami 40g, Rhizoma Alismatis 60g, Radix Achyranthis Bidentatae 60g, Pheretima 60g, Radix Curcumae 6g, Radix Polygalae (processed with honey) 60g, Rhizoma Anemones Altaicae 60g, Semen Ziziphi Spinosae (stir-fry) 40g, Radix Glycyrrhizae 40g
Adjuvant: magnesium stearate
Ten five tastes such as above Radix Salviae Miltiorrhizae decoct with water three times, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrate is carried out three grades of ultrafiltration, first order molecular cut off is 80000 cellulose diacetate film, the second level is 20000 cellulose diacetate film with molecular cut off, and the third level is 6000 sulfonated polysulfone membrane with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.35MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.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.Feed nitrogen in the ultrafiltration system discontinuous, form the gas-liquid stream of pulses, the cycle be ventilation in 0.5 hour once, each 1 minute.Feed temperature is 30 ℃, when feed liquid stock solution is concentrated 1/10, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is the mixed solution of 1.5% sodium hydroxide and 2% sodium hypochlorite, and pH value is 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is condensed into cream, and with this extractum and magnesium stearate mix homogeneously, drying is pulverized, and mixing incapsulates, promptly.
Embodiment 34
Raw material: Caulis Spatholobi 50g, Semen Persicae 10g, Radix Salviae Miltiorrhizae 50g, Radix Paeoniae Rubra 25g, Flos Carthami 20g, Lignum Dalbergiae Odoriferae 20g, Radix Curcumae 25g, Radix Notoginseng 50g, Rhizoma Chuanxiong 15g, Radix Aucklandiae 20g, Rhizoma Acori Graminei 25g, Fructus Lycii 50g, Rhizoma Polygonati (wine is processed) 100g, Radix Ginseng 25g, Radix Ophiopogonis 50g, Borneolum Syntheticum 5g
Adjuvant: microcrystalline Cellulose
Radix Salviae Miltiorrhizae, Radix Paeoniae Rubra, Rhizoma Acori Graminei, Radix Curcumae, Radix Ginseng, Radix Notoginseng, Caulis Spatholobi, Radix Ophiopogonis, Semen Persicae decoct with water secondary, and 3 hours for the first time, 1 hour for the second time, collecting decoction filtered filtrate for later use.Rhizoma Polygonati, Rhizoma Chuanxiong, Flos Carthami, Fructus Lycii are with 70% alcohol reflux secondary, 3 hours for the first time, 2 hours for the second time, merging filtrate, filtrate for later use.It is most to oil that the Radix Aucklandiae, Lignum Dalbergiae Odoriferae extract volatile oil, and the leaching medicinal liquid.Merge above each filtrate, filtrate is carried out three grades of ultrafiltration, and first order molecular cut off is 70000 cellulose diacetate film, and the second level is 20000 cellulose diacetate film with molecular cut off, the third level is 8000 polysulfonamides film with molecular cut off, and filter type adopts cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.4MPa, and the liquid outlet pressure ratio inlet pressure of ultrafiltration hangs down 0.4kPa.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 2.0 meter per seconds, 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 1.0 meter per seconds, feeds nitrogen in the ultrafiltration system discontinuous, forms the gas-liquid stream of pulses, cycle be 0.5 hour the ventilation once, each 1 minute.Feed temperature is 25 ℃, when feed liquid stock solution is concentrated 1/8, adds water or dilute alcohol solution ultrafiltration 1 time again, and the pH value of feed liquid is controlled at 7.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.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, works 10 minutes, recoils 30 seconds.The Chemical cleaning cycle is 0.5 month, and the Chemical cleaning medicament is 4.0% sodium hydroxide solution, and pH value is 11, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Described ultrafiltrate is evaporated to the thick paste that relative density is 1.40 (50 ℃), and drying is ground into fine powder, adds an amount of microcrystalline Cellulose, adds the Radix Aucklandiae and volatile oil of Lignum Dalbergiae Odoriferae and Borneolum Syntheticum fine powder again, and mixing is pressed into 550 or sugar coating.
Claims (17)
1. preparation method that contains the non-injection Chinese medicine preparation of Radix Salviae Miltiorrhizae, it is characterized in that may further comprise the steps: (1) will contain the Chinese medicine medical material of Radix Salviae Miltiorrhizae and make extracting solution; (2) predefecation is handled; (3) ultrafiltration; (4) ultrafiltrate concentrates, and is prepared into the various preparations except that injection;
Wherein, the operating condition of ultrafiltration is: 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 molecular cut off of ultrafilter membrane is 6000～80000; 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.
2. preparation method according to claim 1, the flavour of a drug that it is characterized in that containing in the described step (1) the Chinese medicine medical material of Radix Salviae Miltiorrhizae are 1～15 flavor medicine.
3. preparation method according to claim 2, the flavour of a drug that it is characterized in that containing in the described step (1) the Chinese medicine medical material of Radix Salviae Miltiorrhizae are 1～10 flavor medicine.
4. preparation method according to claim 1, it is characterized in that predefecation is handled the employing coarse filtration in the described step (2), perhaps adopt microfiltration, perhaps adopt centrifugal, perhaps adopt the flocculating agent adsorption clarification, it is assorted perhaps to adopt alcohol deposition method to dispel, and perhaps associating in twos or multinomial the associating are used above-mentioned defecation method.
5. preparation method according to claim 1, it is characterized in that the used ultrafilter membrane of described ultrafiltration 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.
6. preparation method according to claim 5, it is characterized in that the used ultrafilter membrane of described ultrafiltration 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 above-mentioned ultrafilter membrane is 10000～70000.
7. preparation method according to claim 1 is characterized in that described ultrafiltration is cross flow filter or dead-end filtration.
8. preparation method according to claim 7 is characterized in that described ultrafiltration is a cross flow filter.
9. preparation method according to claim 1 is characterized in that 2～3 grades of ultrafiltrations of described ultrafiltration employing.
10. according to the described preparation method of the arbitrary claim of claim 1～9, it is characterized in that the operating condition of described ultrafiltration is: the inlet pressure of ultrafiltration is 0.1～0.35MPa; Feed temperature is 20～40 ℃; The pH value of feed liquid is controlled at 6.0～7.5; When feed liquid stock solution is concentrated 1/12～1/8, add water or dilute alcohol solution ultrafiltration 1～2 time again.
11. preparation method according to claim 1 is characterized in that, in described ultra-filtration process, the ultrafiltration initial stage is adopted lower pressure, slowly boosts then; Adopt the periodic pressure fluctuation separately, the pressure wave moment is 0.1～0.2MPa.
12. preparation method according to claim 1 is characterized in that, in described ultra-filtration process, the feed liquid flow velocity is 1.0～4.0 meter per seconds; Adopt periodically flow fluctuation separately, the flow speed wave moment is 1.0～2.0 meter per seconds.
13. preparation method according to claim 1 is characterized in that, in described ultra-filtration process, feeds high-pressure inert gas off and on, ventilates once each 1 minute in 0.5 hour～2 hours.
14. preparation method according to claim 11 is characterized in that, in the process of described ultrafiltration, associating or three unite the following method that adopts in twos: the periodic pressure fluctuation, and the pressure wave moment is 0.1～0.2Mpa; Periodically flow fluctuation, the flow speed wave moment is 1.0～2.0 meter per seconds; Feed high-pressure inert gas off and on, ventilated once each 1 minute in 0.5 hour～2 hours.
15. according to the described preparation method of the arbitrary claim of claim 1～9, it is characterized in that, in the process of described ultrafiltration or after the ultrafiltration, carry out backwash, its backwash condition is: backwashing pressure is 1.5～2.5MPa, and backwashing period is that 0.5～1.5 hour, backwashing time are 1 minute～10 minutes.
16. according to the described preparation method of the arbitrary claim of claim 1～9, it is characterized in that, in the process of described ultrafiltration, with the ultrafiltration module parallel connection, replace 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, work 10～20 minutes, recoil 30 seconds～3 minutes.
17. according to the described preparation method of the arbitrary claim of claim 1-4, it is characterized in that,
The used ultrafilter membrane of described ultrafiltration 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 above-mentioned ultrafilter membrane is 20000～50000;
Described ultrafiltration is a cross flow filter;
The operating condition of described ultrafiltration is: the inlet pressure of ultrafiltration is 0.25～0.35MPa; Feed temperature is 20～40 ℃; The pH value of feed liquid is controlled at 6.0～7.5; When feed liquid stock solution is concentrated 1/12～1/8, add water or dilute alcohol solution ultrafiltration 1～2 time again;
In the process of described ultrafiltration, the ultrafiltration initial stage is adopted lower pressure, slowly boosts then; Adopt the periodic pressure fluctuation separately, the pressure wave moment is 0.1～0.2Mpa; Perhaps adopt periodically flow fluctuation separately, the flow speed wave moment is 1.0～2.0 meter per seconds; Perhaps employing feeds high-pressure inert gas off and on separately, ventilates once each 1 minute in 0.5 hour～2 hours; Perhaps periodic pressure fluctuation and periodically flow fluctuation associating use; Perhaps periodic pressure fluctuates and feeds high-pressure inert gas off and on and unites use; Perhaps the periodicity flow fluctuates and feeds high-pressure inert gas off and on and unites use; Perhaps periodic pressure fluctuation, periodicity flow fluctuate and feed the high-pressure inert gas three off and on and unite use.
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